Fracture Mechanics

of Ceramics
Volume 9
Composites, R-Curve Behavior,
and Fatigue
Volume 1 Concepts, Flaws, and Fractography
Volume 2 Microstructure, Materials, and Applications
Volume 3 Flaws and Testing
Volume 4 Crack Growth and Microstructure
Volume 5 Surface Flaws, Statistics, and Microcracking
Volume 6 Measurements, Transformations, and
High-Temperature Fracture
Volume 7 Composites, Impact, Statistics, and High-Temperature
Phenomena
Volume 8 Microstructure, Methods, Design, and Fatigue
Volume 9 Composites, R-Curve Behavior, and Fatigue
Volume 10 Fracture Fundamentals, High-Temperature
Deformation, Damage, and Design
Fracture Mechanics
of Ceramics
Volume 9
Composites, R-Curve Behavior,
and Fatigue

Edited by R. C. Bradt
University of Nevada-Reno
Reno, Nevada

D. P. H. Hasselman
Virginia Polytechnic Institute and State University
Blacksburg, Virginia

D. Munz
University of Karlsruhe
Karlsruhe, Germany

M. Sakai
Toyohashi University of Technology
Toyohashi, Japan

and V. Ya. Shevchenko

High Tech Ceramics Scientific Research Centre
Moscow, Russia, CIS

SPRINGER SCIENCE+BUSINESS MEDIA, LLC

ISBN 978-1-4613-6477-1 ISBN 978-1-4615-3350-4 (eBook)
DOI 10.1007/978-1-4615-3350-4
Library of Congress Catalog Card Number 83-641076

First part of the proceedings of the Fifth International Symposium

on the Fracture Mechanics of Ceramics, held July 15-17, 1991,
in Nagoya, Japan

© 1992 Springer Science+Business Media New York

Originally published by Plenum Press, New York in 1992

Aii rights reserved

No part of this book may be reproduced, stored in a retrieval system, or transmitted
in any form or by any means, electronic, mechanical, photocopying, microfiIming,
recording, or otherwise, without written permission from the Publisher
 DEDICATION

JUNN NAKAYAMA
1930-1991

Junn Nakayama was a pioneer of the quantitative study of the fracture of ceramics. A
physics graduate of Gakushuin University, he joined the research laboratory of the Asahi
Glass Co., Ltd. in 1953. Within a decade he had developed the now-famous work-of-fracture
test (Japan Journal of Applied Physics, 3[7]442(1964)). He had already applied it to the
quantitative analysis of the thermal shock damage of fireclay refractories (Bulletin of the
American Ceramic Society, 45[7]666(1966)) when others were just becoming cognizant of
this simple, yet elegant technique. Those two studies were landmark efforts in establishing
the framework for the microstructural design of improved thermal shock damage resistant
refractories. The principles were subsequently extended to structural ceramics, as well as
to the confirmation of the energy balance theories for thermal shock damage advanced by
Hasselman.

Junn Nakayama spent his entire career with the Asahi Glass Co., becoming Director of
the Research Center in Yokohama and subsequently Managing Director of the Asahi Glass
Foundation in Tokyo. At this Fifth Fracture Mechanics of Ceramics Symposium in July of
1991, Junn Nakayama attended the opening ceremonies at the Japan Fine Ceramics Center
in Nagoya, but was not able to participate in the meeting. When introduced to the attendees,
he received a standing ovation. It is with deep regret to report to you that Junn Nakayama
passed away on December 14, 1991. He will always be missed, but will never be forgotten.

v
PREFACE

These volumes, 9 and 10, of Fracture Mechanics of Ceramics constitute the proceedings
of an international symposium on the fracture mechanics of ceramic materials held at the
Japan Fine Ceramics Center, Nagoya, Japan on July 15, 16, 17, 1991. These proceedings
constitute the fifth pair of volumes of a continuing series of conferences. Volumes 1 and 2
were from the 1973 symposium, volumes 3 and 4 from a 1977 symposium, and volumes 5
and 6 from a 1981 symposium all of which were held at The Pennsylvania State University.
Volumes 7 and 8 are from the 1985 symposium which was held at the Virginia Polytechnic
Institute and State University.

The theme of this conference, as for the previous four, focused on the mechanical behavior
of ceramic materials in terms of the characteristics of cracks, particularly the roles which they
assume in the fracture processes and mechanisms. The 82 contributed papers by over 150
authors and co-authors represent the current state of that field. They address many of the
theoretical and practical problems of interest to those scientists and engineers concerned with
brittle fract ure.

The program chairmen gratefully acknowledge the financial assistance for the Symposium
which was provided by the Japan Society for the Promotion of Science, the Inoue Foundation
for Science, The Asahi Glass Foundation, the Nippon Sheet Glass Foundation for Materials
Science, The Daiko Foundation, the Japan Fine Ceramics Center, and the Nagoya Convention
& Visitors Bureau. Without their support, the magnitude and quality of this conference
simply would not have been possible.

Unfortunately, the numerous individ uals who contributed to the success of the conference
cannot all be listed here. However, the program chairmen would especially like to recognize
the contributions of Prof. N. Soga (President of the Conference, Kyoto University), Dr. O.
Kamigaito (President of the Conference, Toyota C. R. D. Labs.), Dr. H. Awaji (JFCC), and
Dr. H. Takahashi (Toyota C. R. D. Labs.) in planning and organization of the conference;
Ms. E. Deguchi for her conscientious and efficient organization of the registration; Mr. N.
Nakagomi for his patience and help in finally bringing these proceedings to press.

R.C. Bradt D.P.H. Hasselman D. Munz

Reno, USA Blacksburg, USA Karlsruhe, Germany

M. Sakai V.Y. Shevchenko

Toyohashi, Japan Moscow, USSR

July, 1991

vii
CONTENTS

Fracture Mechanics and Mechanism of Ceramic Composites

T. Kishi

Effects of Residual Stress and Frictional Sliding on

R-Curve Behavior in Fiber-Reinforced Ceramics 19
K. Sekine and Y. Kagawa

A Crack Growth Resistance Model for

Fiber-Reinforced Ceramic Materials 29
l. Zhou, Y-W. Mai and Y-c. Gao

On The Size Effect in Fracture of Ceramic-Ceramic Composite Materials 53

J. L10rca and M. Elices

Matrix Cracking and Fiber Bridging of

Carbon Fiber Reinforced Carbon Matrix Composites . • . . . . . 69
M. Sakai and T. Miyajima

Fiber Pullout and Fracture Energy of C-fiber/C-matrix Composites 83

T. Miyajima and M. Sakai

The Crack Growth Resistance of SiC-SiC Ceramic Composite Materials 97

M. Gomina and M-H. Rouillon

Effects of Temperature and Oxidation of The Mechanical Behavior of

Uncoated SiC-SiC Composite Materials . . • • • • 111
M. Gomina, J-l. (hermant and P. Fourvel

Fracture Toughness of Carbon Fiber Reinforced Ceramic Composites 123

K. Nakano, A. Kamiya, SYamauchi and T. Kobayashi

Dynamic Fracture Responses of Ab03, ShN 4 and SiCw / Al 20 3 133

Y. Takagi and A.S. Kobayashi

Fracture Toughening Mechanisms in The SiCw/ Al 20 3 Composite System 147

l. Guazzone and K.W. White

Microstructures and Fracture Behaviors at High Temperatures for

Ab03-SiC Nanocomposites .•... . • • . . • . . . . 165
A. Nakahira and K. Niihara

Fracture Toughness of SiC-Whisker/Zr02/Al 20 3 Triple Phase Composites 179

Y. Kogo, H. Hatta and Y. Kagawa

IX
 R-Curve Behavior of Ceramics • • • • • • • • • • • • • • • • • • 187
R.w. Steinbrech

Universal R-Curve of Crack Propagation Resistance in Ceramic Composites 209

S.M. Barinov and V.Ya. Shevchenko

Subcritical Crack Growth of Macro- and Microcracks in Ceramics 219

T. Fett and D. Munz

R-Curve and Fatigue Behavior of Gas Pressure Sintered Silicon Nitride 235
K. Urashima, Y. Tajima and M. Watanabe

Investigation of R-Curve Behavior and

Its Effect on Strength for Advanced Ceramics • • . • • • • • . 251
H. Tsuruta and Y. Furuse

Crack Face Bridging Tractions in Monolithic Spinel • • . • . . . • • 265

J.c. Hay and KW. White

R-Curve Properties of Alumina Measured by Stable Fracture Test in Bending 277

T. Nishida and I. Kameyama

Evaluation of Critical Defect Size of Ceramics Based on R-Curve Method 289

K. Tanaka, K. Suzuki and H. Tanaka

Crack Wake Effects on MgO Fracture Resistance • • • • • . . • • • 305

J. L10rca and T. Ogawa

Interrelation Between Flaw Resistance, KR-Curve Behavior, and

Thermal Shock Strength Degradation in Ceramics . . . • • 319
E.H. Lutz and M.V. Swain

Microcrack Toughening Mechanism in Brittle Matrix Composites .••• 339

N. Miyata, S. Akada, H. Omura and H. Jinno

R-Curve Behavior of Alumina and PSZ at Ambient and High Temperatures 357
M. Saadaoui, C. Olagnon and G. Fantozzi

R-Curve Behavior of PZT Ceramics Near Morphotropic Phase Boundary 371

S. Baik, S.M. Lee and B.S. Min

Crack-Resistance Curve and Cyclic Fatigue in Ceramic Materials .••• 387

Y-W. Mai, X. Hu, K. Duan and B. Cotterell

Effects of Crack Size on Crack Propagation Behavior and

Experimental Verification of Cyclic Fatigue Mechanism of
Sintered Silicon Nitride ••..••.•.•••••.. 423
A. Ueno, H. Kishimoto and H. Kawamoto

Fatigue Crack Propagation and Failure Prediction for

Toughened Ceramics under Cyclic Loads 439
A. Okada and T. Ogasawara

Tensile Fatigue Crack Growth of Polycrystalline Magnesia . • • • . • . 455

T. Ogawa

x
Fatigue Behavior of Structural Ceramics • • • . . . 465
Y. Yamauchi, 1. Ohji, W. Kanematsu, S. Ito and K. Kubo

Fatigue Behavior of Non-Oxide Ceramics at Elevated Temperature 481

M. Masuda, 1. Makino, Y. Nakasuji and M. Matsui

Cyclic Fatigue of Electrically Poled Piezoelectric Ceramics 493

T. Nishikawa, J. Takahashi, A. Hattori and M. Takatsu

Crack Growth Behavior of Sintered Silicon Nitride Su bjecied to Cyclic Loading 501
L.X. Zeng and Z.D. Guan

Crack Growth in Zirconia Bearing Ceramics under Cyclic Loading 507

K. Duan, B. Cotterell and Y-W. Mai

Fatigue Behavior of Sintered ShN 4 under Rotary Bending and Static Fatigue 517
H.N. Ko

An Approach on Lifetime Prediction for Ceramics under

Elevated Temperature with Static Fatigue 535
L.X. Zeng, Z.D. Guan and X.F. Zhao

Lifetime of HIPed Silicon Nitrides at Elevated Temperatures • . • . 543

I. Tanaka, G. Pezzotti and K. Niihara

An Indirect Method for The Determination of dajdN - ~K-Curves for

Ceramic Materials ........••.•. 559
1. Fett and D. Munz

Effect of Residual Stress Due to Knoop Indentation on

Subcritical Crack Growth Behavior in Ceramics 569
J.H. Gong and Z.D. Guan

Effect of Surface Charge on Subcritical Crack Growth in Glass 575

S. Takeda and I. Tari

International Editorial Board, Organizing

Committee, and Session Chairs 589

Authors 593

Index 603

xi
FRACTURE MECHANICS AND MECHANISM OF CERAMIC COMPOSITES

Teruo Kishi

Research Center for Advanced Science and Technology

The University of Tokyo
4-6-1 Komaba, Meguro-ku, Tokyo 153, Japan

ABSTRACT

Interfacial behavior of SiC fiber reinforced glass matrix composites was

analyzed by a single fiber pull-out testing. The interfacial properties of this
composite were calculated by using the shear-lag analysis during the fiber
pull-out tests in terms of interfacial shear strength, coefficient of friction and
residual clamping stress. Experimental difference of load-time curves
between materials can be explained by the analysis of shear stress
distribution of fiber. Fracture resistance with crack extension due to the fiber
bridging mechanism was also estimated by the interfacial mechanical
parameters in this composite on the basis of the stress distribution by the
above shear-lag analysis. Acoustic Emission (AE) waveforms during the
single fiber pull-out testing were recorded by using the advanced AE
measuring system with multi-channels. Locations of debonding were
estimated with good accuracy and debonding length was also evaluated by
this source model of debonding and the deconvolution method.

INTRODUCTION

Many ceramic matrix composites have been investigated to enhance

fracture toughness of ceramics. Especially in continuous fiber reinforced
ceramics remarkable increase of toughness has been reported [1, 2, 3]. In
such composites it is very important that the mechanism of stress shielding
can enhance fracture toughness, due to crack bridging and sliding at
interface between matrix and fiber. Thus interfacial shear stress or strength
determines the increasing of fracture toughness with crack extension, which
is called as R-curve behavior. The purpose of this paper is 1) to estimate
quantitatively the interfacial mechanical properties by a single fiber pull out
testing, 2) to evaluate the increase in fracture toughness by using the above
mechanical parameters, and 3) to analyze the discontinuous microfracture
process of interface by inverse Acoustic Emission (AE) source
characterization method.

Fraclure Mechanics of Ceramics, Vol. 9

Edited by R.C. Bradt el al., Plenum Press, New York. 1992
 The interfacial mechanical properties are quantitatively estimated by a
single fiber pull-out testing. The SiC fiber reinforced glass composite was
used as a model material where friction between matrix and fiber provides
stress transfer. The interfacial shear strength of this composite was
calculated by using Hsueh's shear-lag analysis [4]. Also the debonding
behavior at the interface was observed by the video microscope system with
high magnification. The debonding process in this composite is discussed in
the consideration of the stress distribution of a fiber which is estimated by this
model.

In the continuous fiber reinforced composites, the 'phenomenon of

multiple fracture in the case that fibers sustain stress mainly has been
analyzed based on the energy-balance analysis by Aveston et al. (ACK) [1].
Such a multiple fracture has been observed in the continuous fiber reinforced
composites when matrix is brittle and fibers have larger failure strain than
that of matrix, and it has been reported that the theoretical results were in
good agreement with experimental ones. On the other hand, Marshall et
al.[2] have evaluated the stress for matrix cracking in fiber reinforced brittle-
matrix composites using a stress intensity approach, in which the influence
of the fibers that bridge the matrix crack has been represented by closure
tractions at the crack surfaces. McCartney [3] has also modified ACK theory
for plane-strain conditions and analyzed the same problem that Marshall et
al. treated. In the continuous fiber reinforced composites assuming the state
that fibers sustain stress and close crack surfaces by sliding at interfaces
between fiber and matrix, the increase in fracture toughness by crack
bridging can be evaluated by the the interfacial shear stress in sliding at the
interfaces and the sliding length measured from cracked matrix. In this
paper, we consider the crack bridging problem on the basis of the stress
distribution by the above shear-lag analysis. Experimental value in fracture
toughness of this SiC fiber reinforced glass composites is compared with the
calculated one by this theoretical prediction.

The faulting source in an elastic medium such as a microcracking can

be modeled as generation of a moment tensor [5, 6]. However, a model of
debonding source at the interface in such a fiber reinforced composite was not
clear. We propose a model of AE source of debonding at the interface, which
is considered as very important in the interfacial shear strength tests, by
using the theory of faulting source in an elastic medium. AE waveforms
during this test were recorded by using the advanced AE measuring system
with multi-channels [7]. The debonding process in this composite is also
discussed from the results of both observation and analysis of AE
characteristics.

EVALUATION OF INTERFACIAL PROPERTIES

Theory of Interfacial Parameters

Analysis of interfacial shear stress in the single fiber pull-out test was
carried out by Hsueh [4] by using the configuration of the single fiber pull-out
test (see Figure 1) and .the stress vs. displacement curve (see Figure 2). Here
the frictional debonding process is assumed, that is, stress is always
transferred by the friction at interface. The interfacial shear strength, 'ts, is
used as a criterion for debonding, which can be represented as

2
 ttt

Figure 1. Configuration of the single pull-out test.

Partial debonding
Complete
\ debonding
Fiber
pull-out

Displacement
Figure 2. Stress vs. displacement curve fiber during the single fiber pull-out
test.

3
 (b2/a2-1)(EmlEf)coth(at)+21{exp(at)-exp(-at)} }
'ts =-crd (21a)[(1+Vm){1+(b2/a2-1)(EmlEf)}{b2In(b/a)-(b2-a2)/2}]1I2 ,
{ (1)

where a is the radius of fiber, b is the radius of specimen, t is the embedded

length of fiber, Em and Ef are Young's modulus of matrix and fiber, Vm and
Vf are volume fraction, Vm and Vf are Poisson's ratio and crd is the initial
stress of partial debonding. Also the coefficient of friction, Il, and residual
clamping stress, crc, can be obtained from the following equations,

{~N~[ 1-~]-1}[eXP(m1t)-eXP(m2t)]
+~ 1-~] {m1[1-exp(m2t)]-m2[1-exp(m1t)]}
21lvmL a

= -;Il[m1[1-eXP(m2t)]-m2[1-eXP(m1t)]+(m1-m2){~N:11-~]-1}] ::' (2)

(m1-m2)exp{(m1+m2)t}crd
exp(m1t)-exp(m2t)
A3 m2exp(m2t)-m1exp(m1t)+(m1-m2)exp{(m1+m2)t}
=A2 exp(m1t)-exp(m2t)
21l *{m1eXp(mlt)-m2eXp(m2t) 21lEmVf}
+a-crc+crd exp(m1t)-exp(m2t) +aD Ef ' (3)

where

1[ a 2Ef+(b2-a2)E m ]112 b2+a2 E m (1-nf)

a= a Ef(l+nm){b2In(b/a)-(b2-a2)/2} , D = b2_a2+nm+ Ef
a(l-b 2/a 2 )D
Al =2Ilvm(I+vm){b2 In(b/a)-(b 2-a 2)/2} ,
(1-b 2/a 2 )(Emvv'EfVm)-1
A2 =(1+vm){b2 In(b/a)-(b 2-a2 )/2} ,
crd*+(crdvm)(1-b 2/a 2)D
A3 =- (1+nm){b2In(b/a)-(b 2-a2 )/2} ,
m1 ={-A1-(A12-4A2)1I2J/2, m2 ={-A1-(A1 2-4A2)1/2}/2 , (4)

where crd* is the stress of complete debonding and crt is the stress of fiber pull-
out.

Frictional and Frictionless Debonding

The radial stress of interface at the position of surface, cr p , which is

induced by applied stress, crh, can be represented as

(5)

4
 fiber

notch

embedded
fiber length

t =4
Figure 3. Geometry of specimen.

Table 1. Interfacial mechanical parameters of the SiC fiber glass

matrix composites.

Material type A typeB

at 1023K at 1023K
Fabricated conditions in vacuum in An~on
Interfacial shear
strength, 'ts (MPa) 100.3 175.0
Coefficient of friction, m
0.41 0.41
Residual clamping
stress, crc (MPa) 34.1 34.1
Induced radial stress by
initial debonding, crp -23.1 -40.1
(MPa)
Induced radial stress by
complete debonding, crp -31.3 -
(MPa)

Debondinl'! behavior Frictional debondinl'! Frictionless debondinl'!

5
The interfacial frictional stress at the surface, 'ti, can be represented as

(6)

The partial debonding process can be valid for the frictional debonding
condition, <rc + <rp > o. If the length of fiber is long or the interfacial shear
strength is strong relatively, the condition, <r c + <rp ;5; 0, that is called as
frictionless debonding, is satisfied. Here stress is not transferred effectively,
and debonding would occur catastrophically.

Material

The composite, which was used in the experiment, consists of SiC fiber
(TEXTRON, SCS-6) and Pyrex glass (Corning, #7740). The fibers with an
average diameter of 150 /.lm were aligned in a layer at equal spacing and were
covered with two glass sheets. The samples were hot-pressed at 1023 K and a
pressure of 10 MPa in both vacuum (type A) and Ar gas (type B). The
specimens were cut from these sheets and polished. Figure 3 shows an
example of the geometry of specimen used in single fiber pull-out testing.

Single Fiber Pull-out Test

Notch was induced to crack matrix. A specimen was pulled out

vertically by Instron type tensile machine and the load to fiber was measured.
The observation from side view of specimen during pull-out test was employed
by the video microscope system (Scholar, VMS-lOOO).

An example of time-load curves of type A composite during pull-out test

are shown in Figure 4. Load increased linearly and then dropped suddenly
because of matrix cracking. Load increased again and compliance changed
accompanying partial debonding at interface. Step-like debonding occurred
before complete debonding, and then fiber pull-out started. It was clear from
the observation of interface that debonding at the interface propagated
gradually and finally fiber pull-out occurred. Figure 5 shows the time-load
curves of type B composite during pull-out test. In this material, partial
debonding of interface was not observed.

Results of Interfacial Parameters

Parameters that describe the interfacial characteristics such as

interfacial shear strength, coefficient of friction, residual clamping stress
and interfacial frictional stress at the surface were calculated from equations
(1), (2), (3), (5) and (6). The estimated values of these materials are listed in
Table 1.

In the type B composite, the coefficient of friction was calculated by using

the same value of the residual clamping stress as the type A composite since
the specimen of the type B composite showed the frictionless debonding
behavior and the temperature of fabrication was the same as that of the type
A. The result of interfacial frictional stress demonstrates that the present
model for debonding can explain the experimental difference of the load-time
curves of two materials.

6
 Matrix: CGW - 0.7740
Fabricated at 1023K in vacuum
Loading rate = 100j.lm/min
30 complete debonding
matrix
z
-020 / fiber pull-out
<':
o
...:l
./
10
initial debonding

O..............:::.......................~~~....L..-~~-'--'~~~--'
o 50 100 150 200
Time, S

Figure 4. Time-load curves of type A composite during pull-out test.

Matrix: GW· 0.7740

Fabricaled at 1023K in Ar
Loading rate = 100j.lm/min
30
frictionless debonding
z
] 20
o
...:l

OL-..~~~"""""'~~~..I..-~~~...J...-~~~....l

o 50 100 150 200

Time, S

Figure 5. Time-load curves of type B composite during pull-out test.

7
FRACTURE RESISTANCE

Mechanics of Crack Bridging

Fracture resistance due to fiber bridging is estimated using the

toughening mechanism by the force equilibrium which is shown
schematically in Figure 6. In this treatment, crack closure stress P is given
by

where Vf is a volume fraction of fiber. Crack opening displacement 0 is given

by

2E h h
2
0= Ef [crh(h)h + aE ~
m m 0
J J
dz ti(z,h)dz l.
z
(8)

J-integral associated with the closure stress, ~G, is

0* h*
~G = J P(o) do =
o
~: [ Jcrh2(h)dh + crh2(h*)h* l .
0
(9)

As a result, the increase of fracture resistance can be formulated by

~G E c 2 lJ2
M(={ +Ko} -Ko. (10)
( 1- vc 2 )

where ti(z, h) is the interfacial shear stress at z when the variable debonding
length is h, and h* is the maximum debonding length. By using the equation
(10), the fracture resistance can be calculated as a function of crack extension.

Fracture Toughness Test

Evaluation of fracture toughness is carried out by using a compact-

tension type specimen with unidirectional fiber along the loading direction
which is shown in Figure 7. Fracture toughness test was carried out by an
Instron type testing machine at constant cross head speed of 1 mm/min, at
room temperature in air. Debonding behaviors and debonding length were
observed by video microscope. Figure 8 shows an applied load-time curve of
this fracture toughness testing. At the point of sudden decrease in stress
crack initiation occurs and crack propagates with increasing applied load.

Optical Observation

Figures 9 shows the side views of specimen during fracture toughness

test. It was observed that a crack started to propagate from the tip of notch
and a white triangular area, which was due to debonding and sliding at the
interfaces between matrix and fiber, generated and increased in the region
between crack tip and notch. The length of sliding at the interface and the

8
 end of
debonding
matrix fiber /matrix

ad
l'
/ stress relaxed
position

....
z
'ri(') Jr 1l 'r i (z)

j
'1'
v iu
*'
~
J,

Figure 6. Schematic representation of fiber bridging.

=
m

t=4

Figure 7. Geometry of CT specimen.

9
 J()() .------~----"""T'"""----~---~

loading rate: I mm/min

specimen : at I023K in vacuum
for IOmin

Z
"'C 50
<':
'=!

propal:ation
extension
crack pause
OL-----~----.l-----~----l
o 10 20
Time, s

Figure 8. Load-time relation offracture toughness testing in glass matrix composite and
microfracture processes.

Figure 9. Side view of specimen during the fracture test.

10
length of propagating main crack can be measured from Figure 9, which
shows that no fiber was broken during the test.

Fracture Process

The fracture process in this material is schematically represented in

Figure 10. The interfaces between matrix and fiber were debonded. And then
matrix cracked when stress intensity factor of crack tip reached fracture
toughness of glass according to increasing load. Next, this crack of matrix
propagated at a relatively slow rate, that could be observed by eyes. This
propagated crack arrested in pause. And then as a crack propagated,
interfaces were debonded and slided in the back of crack tip, and a crack was
bridged by fibers. Figure 9 clearly shows that a crack propagated and a region
of debonding and sliding at interfaces extended in the form of triangle.
a
Finally, crack was bowed or branched and the end of slided interfaces was
fractured again when a crack was not able to propagate by the effect of
specimen geometry and applied load condition.

Resistance Curve

Figure 11 ( o-symbol ) shows the relation between the stress intensity

factor K and the increase of crack length ila, which is estimated from Figure
9 by the ASTM-E399. This material shows the resistance curve (R-curve), i.e.,
K value increases as ila increases. The closure pressure of the unbroken fiber
to crack surfaces P can be calculated from the sliding length at the interfaces
obtained in Figure 9. From the equations (9) and (10), ilK can be calculated
and the values of K are plotted in Figure 11 (il-symbol). A good correlation
exists between experimental and calculated results. Assuming that fibers
slide at interfaces to their break, the value of K in this material may be
enhanced to about ten times of Ko by the mechanism of crack bridging under
the condition that specimen is enough large and fibers can slide at interfaces
up to their break.

EVALUATION OF DEBONDING PROCESS BY AE

Displacement Field due to Faultin~ Source

It is well known that the faulting source in an elastic medium can be
modeled. Let L denote a fault surface contains two adjacent opposite internal
surface, labeled L+ and L-. Using the reciprocal theorem, the displacement
field at position x' and time t, u(x', t), for point source can be represented as
[5,6]

ui(x', t) "" Gij(x', x, t) * Tj{x, t) + Gij,k(x', x, t) * Djk(X, t), (11)

J
Tj(x, t) = L [tj{x, t)] dS, (12)

J
Djk(x, t) = L Cpqjk [up(x, t)] Vq dS, (13)

J
where * means a convolution integral with respect to time, L dS indicates a
surface integral and Gij{x', x, t) is the displacement field in the direction xi at
position x' at time t due to an impulsive force in the direction Xj at position x at
time 0, which is called as a Green's function. The displacement discontinuity

11
 (a) before test (b) debonding initiation
..... r-

> )1

'- '-

(c) crack initiation (d) crack propagation and

debonding extension
r- r- ,... r- r- r- r- r- r- .....

r
)I t-I f-
I

L.. '- '-

Figure 10. Schematic model offracture process.

15 ,....----r--,--.------,r----..--,-....------,r----.---,

loading rate : 1 mm/min

fabricated at l023K in vacuum

•
•
~
'"
=
Q,l

.c /).

-=
Of)
./).
<:> • Experiment
./).
/). Calculation fj./).

b. ~
fj.~
h
o L..----'---L._-'-_'------'-_--L._""'---_'----'-_....J

o 2 4 6 8 10
Crack extension, mm

Figure 11. Comparison between experimental and calculated results offracture

resistance with crack extension.

12
 v

/1£uJ

Figure 12. Model of AE source due to debonding.

Load

Probe tn, 'en,o, ...... ,HP216

Floppy Disc

Uideo
Microscope ~I>---I AE9620 ...... 1 HP310

Monitor --[)---1 AE9620 Hard Disc

Uideo Pre Amp

Recorder

Uideo
Printer

Figure 13. Experimental system with video microscope and AE equipments.

13
is denoted by [u(x, t)] for x on L, and the traction discontinuity is denoted by
[t(x, t»). The normal to L is v and Cpqjk is the elastic stiffness tensor. The
summation convention for the repeated indices is employed.

AE source of Debondin~

Suppose the debonding surface L shown in Figure 12. From the

equation (13), we can represent Djk(x, t) for an isotropic medium as

J
Djk = L (A [up] vp &,ik + 1l([Uj] Vk +[uk] Vj») dS, (14)

where A and Il are Lame's constants, and Ojk is Kronecker's delta. In the case
of debonding, [ul] = [u2] = n3 = 0 on L. We shall take cylindrical coordinates (r,
e, z) and state the relationship between Cartesian and cylindrical coordinates
as (uI, u2, u3) = (ur cose - ue sine, Ur cose + ue sine, uz). From the equation
(14), components of Djk can be calculated as

DU = D22 = D33 = D12 = D23 = D31 = 0, (15)

where the fault region on L is assumed to be homogeneous. Consequently, all

the components of Djk vanishes.

Similarly components of Tj can be calculated as, from the equation (12),

Tl =T2 =0,
T3 =21t R I [tz], (16)

where R is a radius of fiber and I is a length of debonding. Finally the

displacement field due to debonding can be represented as, from the equations
(11), (15) and (16),

ui(x', t) = Gi3(x', x, t) * T3(x, t). (17)

Thus AE source of debonding is equivalent to a monopole force.

AE Measurin~ System
AE measuring system with multi-channels is also shown in Figure 13.
Transducers were attached to the sample with a bond, of which positions are
shown in Figure 14. The AE transducer (Fuji Ceramics, M31) has a
resonance frequency of 200 kHz with about 2.5 mm diameter. AE waveforms
of 3 channels were recorded by the wave memory (NF, AE9620) with sampling
rate of 50 ns and 2 kwords each channel. Also conventional AE parameters
such as event and amplitude with the load to fiber were analyzed by AE
processor (NF, AE9600). Microcomputers (HP, model 216 and model 310) were
used to record the AE parameters and waveforms via GP-IB interface [7].

Load Curves and AE Characteristics

A specimen was pulled out vertically by Instron type tensile machine.
The time-load curve and time-AE amplitude plot during pull-out test are
shown in Figure 15. This figure shows that firstly AE with amplitude of less

14
 +-
w

Load

Figure 14. Geometry of specimen and positions of transducers.

50 0 100
0

40 00
0 co
"0
30 ai
Z "0
-0 50 .~
ctl a.
0
....J 20 E
<:

10

0 o
0 100 200 300 400 500
Time, s

Figure 15. Time-load curve and time-AE amplitude plots during interfacial shear
strength test.

15
than 65 dB was generated from the beginning of test and secondly AE with
amplitude of about 100 dB appeared at point of matrix cracking. Again AE
with high amplitude was generated from the point of step-like debonding.

Location

Accurate source location is required in order to understand fracture

processes. The location of each source event is determined by measuring the
differences in the wave arrival time between two transducers. Suppose that
~tij is the difference in the wave arrival time between i-th and j-th
transducers. Let ri denote the transducer positions (l S; i S; Q) and r denote the
location of the source, where Q is the total number of channels. We can
represent the general equation for source location as

VL ~tiQ = I r - ri I - I r - rQ I , lS;is;Q-l, (18)

where VL is the longitudinal velocity of material. A nonlinear least-square

method can be used to solve the equation (18) for source location r.

AE waveforms during tensile test can be classified into two groups. One
group, denoted as type (a), has the different phase of the first rising part of
wave in three channels. These AE were generated from the beginning of test
and had relatively small amplitude. The other group, denoted as type (b), has
the same phase. These AE were generated from the point of step-like
debonding. AE of type (a) had locations outside the specimen. It indicates that
AE of type (a) were due to mechanical noises such as friction between
specimen and pin. AE of type (b) were located around a fiber as shown in
Figure 16. It demonstrates that error of location can be estimated within about
0.5 rom and debonding propagates with the increasing of load.

Evaluation of Debonding Length

As mentioned previously, AE source of debonding can be represented as

a monopole force. The deconvolution method with one channel is sufficient to
determine a monopole source if Green's function of specimen and transfer
function of transducer are available. Combined response function of both
Green's function and transfer function was calibrated by the pencil lead
breaking on the surface of specimen. Source function of debonding was
calculated using one of the waveform due to debonding by the deconvolution
method. An exampl~ of source function of debonding is shown in Figure 17.
Debonding is generated with a rise time of about 5 IlS and debonding length is
estimated as 0.6 mm by using equation (16) from the values of [tzl = 200 MPa,
R = 75 Ilm and T3 = 4.2 N.

SUMMARY

1. The interfacial parameters of the SiC fiber reinforced glass matrix

composite have been measured by the single fiber pull-out test. The debonding
behavior at the interface was observed by the video microscope system with
high magnification. By using modified shear-lag model interfacial
mechanical parameters such as interfacial shear strength, frictional
coefficient and residual clamping stress, were successfully obtained from
experimental results of initial debonding stress, complete debonding stress

16
 End of specimen Notch
4

3
E 0
E 0
>. 2

o L-_~_-L __ ~_--L. _ _~ _ - J

o 5 10 15
x,mm

Figure 16. Results ofAE location.

Z 4
<Ii
~
0
LL 2 a T3

0
a I

-2
0 5 10
Time, micro second
Figure 17. Example of source function of debonding.

17
and fiber pull-out stress in a single fiber pull-out test. It could be concluded
that the present analysis demonstrates the experimental difference between
frictional debonding and frictionless debonding.

2. Fracture resistance with crack extension due to the fiber bridging

mechanism was estimated by the interfacial mechanical parameters in SiC
fiber reinforced glass matrix composite. From the interfacial mechanical
parameters which were obtained in a single fiber pull-out test, partial
debonding stress was estimated as a function of debonding length. The
resultant partial debonding stress and fracture resistance with crack
propagation due to fiber bridging were estimated. These results correlated
fairly well with the experimental results.

3. Acoustic emission waveform analysis was employed to evaluate the

microfracture process in this composite. A model of AE source of debonding
at the interface was proposed. AE waveforms during this test were recorded
by using the advanced AE measuring system with multi-channels. Locations
of debonding were estimated with good accuracy and debonding length was
also evaluated by this source model of debonding and the deconvolution
method. Discontinuous debonding -0.6 mm in a single fiber pull-out testing
due to shear deformation was quantitatively estimated by acoustic emission
inverse analysis.

REFERENCES
1. J. Aveston, G. A. Cooper and A. Kelly: Conference on The Properties of
Fibre Composites, (1971) 15.
2. D. B. Marshall, B. N. Cox and A. G. Evans: Acta Metall., 33, 2013 (1985).
3. L. N. McCartney: Proc. R. Soc. London, A 409, 329 (1987).
4. C. H. Hsueh: Mater. Sci. Eng., A123, 1 (1990).
5. K. Aki and P. G. Richards: in "Quantitative Seismology: Theory and
Methods", W. H. Freeman and Company, San Francisco, (1980).
6. M. Enoki and T. Kishi: Int. J. Fracture, 38, (1988), 295-310.
7. M. Enoki and T. Kishi: in "Acoustic Emission: Current Practice and
Future Directions", ASTM STP 1077, (1990), 47-66.

18
EFFECTS OF RESIDUAL STRESS AND FRICTIONAL SLIDING ON
R-CURVE BEHAVIOR IN FIBER-REINFORCED CERAMICS

Kenichiro Sekine and Yutaka Kagawa

Institute of Industrial Science, The University of Tokyo
7-22-1, Roppongi, Minato-ku, Tokyo 106, Japan

INTRODUCfION

Fiber-reinforcement in a ceramic matrix can improve mechanical properties such as

tensile strength, fracture toughness, and work of fracture. These mechanical properties of
the composites reinforced by continuous ceramics fibers are achieved by controlling the
failure process upon being subjected to loading condition. Recent progress in theoretical
analyses have shown various toughening concepts.These enable us to meet the requirements
of toughening mechanisms in the continues fiber-reinforced ceramic matrix composites [1-8].
The toughening process of the continuous fiber-reinforced ceramics is affected by the
properties of fiber, matrix, and their interfaces. Both theoretical and experiment reports
show that the toughening process of the composites can be achieved by fiber bridging behind
the tip of advancing crack, as shown in Fig.1 (a). The process is well represented by R-
curve behavior, as shown in Fig.1 (b).
The total fracture resistance GC(~a) is evaluated by the summation of crack starting
toughness, Gjc, and crack bridging toughening term, ~GC(~a), as

<>
~,.......
~ ~ ~Gc
~t?
~
c: GCI - - - - - - - - - - - - - - - - -

W Stan of crack

\4-----~ I Fiber
~a
o
(~a =0) Crack length (M)
Matrix
(a) (b)

Fig. I Schematic drawing of a toughening model by fiber bridging (a),

and R-curve caused by bridging fibers (b).

Fracture Mechanics ofCeranUcs. Vol. 9

Edited by R.C. Bradt et al.• Plenum Press. New York, 1992 19
 (1)

The outline of the analytical solution for, Gic, is shown in APPENDIX A. The toughening
tenn, ~Gc, of the ceramics by crack bridging is represented in tenns of the J-integral [9].
This toughening increment, ~G(=J), is

(2)

I~
,--------,
2 rc-'II
bonded interface
under residual I
compression
debond front
frictional sHding z
across debonded t---+-~
1-...I......Jr--..... z=O
interface
=/!<00-.10,)
'ts

Fig. 2 Axisymmetric shear lag model and defmition of parameters.

where f is the volume fraction of fiber, 0r(o) is the stress or as a function of displacement 0
for a single fiber bridging. From the equation (2), it can be seen that the force-displacement
relation of the bridging fiber is an important factor for the control of toughening of
composite. However, details of the effects of interfacial mechanical properties, which
depend on coefficient of friction at the interface and thennally-induced stresses during
processing, on the crack closure force are not clearly understood.
In this paper, major attention has been focused on the effect of the interfacial
mechanical properties on the force-displacement relation for the bridging fiber, especially just
after the cracking of a matrix, i.e., small crack opening displacement stage because of
engineering importance. The effect of crack closure force on the toughening (equation (2)) is
also discussed based on the theoretically-obtained force-displacement relation. SiC(CVD)
fiber-reinforced glass matrix composite are used as a model for the calculation because the
properties of the composite are relatively well known [10].

20
THEORETICAL ANALYSIS
Let us consider a single continuous fiber with a radius rfembedded in an
axisymmetric cylindrical matrix of a radius R. This is schematically illustrated in Fig. 2. The
volume fraction of the fiber, f, in the composite is defmed as

(3)

In this analysis, the crack closure stress is obtained as a function of crack opening
displacement using shear-lag analysis in which only normal axial stresses exist within a fiber
and the shear stress is concentrated at the interface between the fiber and the matrix.
The interfacial shear sliding strength, 't s, at the sliding area, O:5z<ls, is defined as

(4)
with

(5)

2
where,a=En/Ef, 11=f/(1-f)=rf/(R -rf) 11 is the coefficient of friction at the interface, cro is
the thermally-induced stress in the radical direction of the fiber, ~crr is the stress due to
Poisson's effect upon tensile loading of the fiber. T is the traction (as defined in Fig. 2),V is
the Poisson's ratio, E is the Young's modulus, and subscripts f and m refer to fiber and
matrix, respectively. The debonding length, ~,of the interface between fiber and matrix is
assumed to be identical to the sliding length, Is.
Above the debonded area, fiber and matrix deforms with an equal strain,
Ef(ls~(ls)=Ec(ls). The strain in the composite, Ec(ls), at z~ls is given as

(6)

with

(7)

According to shear-lag analysis, the forces of the fiber, Tf, and the matrix, Tm , at any
section for 0:5z:51 s is given by

(8)

. aVf) (~c)(
Tm=( aVr+-llvm -T eAz-1 )
(9)
with

(10)

21
 (11)

The detailed derivation of equations (8) and (9) is described elsewhere [4]. In the region
(O~z<ls)' the tensile stress-strain relationships of fiber and matrix under plane strain
condition, respectively, are given as [11]:

(12)

(13)

where <Xf and CXm are the coefficient of thermal expansion of fiber and matrix, respectively.
The sliding length, Is, of the interface along the fiber axis is obtained by setting q(z)
and em(z) equal when z=ls(Cf(ls)=tm(ls)). Is is obtained from equations (12) and (13) as

(14)

The crack opening displacement, 28, of the bridged fiber as a function of crack
closure force, Te, and sliding length, Is, is obtained by integrating the difference of strains of
the fiber £r(z) and the matrix €m(z), as given by equations (12) and (13), respectively, over
the sliding length, Is (O<z<1s), such that

8=fI q(z)-€m(z) Idz

(15)

After obtaining crack closure stress of the fiber as a function of crack opening
displacement, the toughening due to fiber bridging, ~Ge, is calculated by the equation (2)
knowing aro relation and Is (equation (14)).

RESULTS AND CONCLUDING REMARKS

Figure. 3 (a), (b), respectively, shows effect of thermally-induced stress, ao, in the
radial direction on the relation between sliding length and tensile stress of the fiber Fig. 3 (a),
and crack opening displacement (COD=2o) and tensile stress of the fiber Fig. 3 (b) for the
unidirectionally-reinforced SiC(CVD) fiber-reinforced soda-borosilicate glass matrix
composite with f=O.3. For the computation, we use EF400GPa, Em=7OGPa, Vt9).15,
Vm=O.2 and rF71.51lm were used [12]. The tensile force of the fiber is strongly dependent
on both the parameters. Similarly, Fig. 4 (a) and (b) show the variation oOs and 28
respectively with tensile stress af for the same composite. With increasing ao the tensile
force at the same sliding length increases. The same tendency is obtained by changing
coefficient of friction instead of ao and the typical result is shown in Fig. 4.

22
 g 0.0008
00= JOMPa
3 5 to
-7

-oS
-7
M 3 10

5
~ -7
0.0006
2510
-7
I>/) l¢ Z. 10
o
C 0004
o 1510·'
j
I>/) o.oooz
oU I. 10
-7
-8
.5 • 10
:2 -I-~~~----;:--;--
Ci5 a a 8 a a e IS a a "
I. 10 Z. 10 3 10 1. 10 S. 10 1 10 2 10 J. 10 1 10 5. to

Tensile Stress Or (Fa) Tensile Stress Or (Pa)

a b

Fig. 3 (a)Sliding length ls(m) versus fiber tensile stress o~Pa) and (b) crack opening
displacement oem) versus 0t<Pa) as a function of interfacial thermal stresses 00' (SiC
(CYD) fiber-reinforced soda-borosilicate glass composite, f=O.3 and ).1=0.2.)

g 0.00'
~=O.l O.OOOOOZ

oS 0.003
g 0.0000015

I>/)
0.000001
jC 0.002
l¢
Q
I>/) o -7
C; 0.001 U S. 10
:§
Ci5 a e
8 8 8 8 a
1 10
I
z. 10
•
3. 10 • 10
I
6. 10
1. ~ z. W 3. ~ •. ~ s. ~

Tensile Stress Or (Pa) Tensile Stress Or (Fa)

a b

Fig. 4 (a)Sliding length ls(m) versus fiber tensile stress 0t<Pa) and (b) crack opening
displacement Oem) versus 0t<Pa) as a function of interfacial friction coefficients ).I.
(SiC (CVD) fiber-reinforced soda-borosilicate glass composite, f=O.3 and 0o=1OMPa.)

Both the figures show that within the small range of crack opening displacement, the
toughening is not so significant. When 0o=50MPa and Il=O.5, values of which are assumed
to be maximum in the SiC(CYD)-glass systems, the fiber stress is not so high and the fiber
fracture could not occur in the laboratory level specimens because the large sliding
length(order of '" 10 cm) is required to increase fiber stress to its fracture stress ("'3.9 GPa).
The effect of longitudinal thermally-induced stress on the sliding length and crack
opening displacement is shown in Fig. 5. Here, we assume that ar<am , and therefore,
matrix is under the compressive force. Under the existence of the thermally-induced stress,
the sliding and crack opening near the origin of the curves are zero although tensile force of
the fiber exists. Therefore, it is suggested that the thermally-induced stress in the
longitudinal direction affects Is, especially, in the early stage of the toughening process.
Within this analysis, the effect of thermally-induced stress in the longitudinal direction on the
crack bridging appears only to a small amount of the whole stress-displacement relation of
the bridging fiber when 8 is small.

23
 -10
5. 10

:§: O.OOOOZ
-10
1, 10'
-10
.s ..--1t--ftijiM
-

I
63, 10
~ 0,00001 .......... -10
<-0 Z, 10
o
C
..!:! -10
oJ) 01. 10

:§ -0.00001
U
v.;
-O.OOOOZ
-1. 10
-10
t-----
Tensile Stress Or (Pa)

Fig. 5 Effect of therrnally-induced longitudinal stress on the relation between sliding

length Is and fiber tensile stress, and crack opening displacement and fiber tensile
stress for SiC (CVD) fiber-reinforced soda-borosilicate glass composite (f=O.3,
O'O=lOMPa, pO.2, and ~T=500K, ar2.53xlO-6/K, u m=3.6xlO-6/K).

Typical crack bridging toughening, versus crack opening displacement relations for
the different volume fraction of the fiber in SiC(CVD) fiber-reinforced glass matrix
composite is shown in Fig. 6. As clearly shown in this figure, when the 0'0 and 11. are the
same, ~OC increases with increasing volume fraction of the fiber. However the maximum
3 2
value of ~Gc in Fig. 6 is "'5xlO- J/m and is only 0.06% of the un-reinforced monolithic
2
glass materials ("'8J/m ). This result also suggests that the fiber closure force could not
approach tensile fracture strength of the fiber unless there exists some enhanced mechanism
of closure force. It is possible that the closure force is enhanced due to reaction between
fiber and matrix at a bonded part.

5r------o----------,

B
'"...
~ 2
'"o
~
>. 1
::.0
OJ
c
Ul 0 Ifte.:::::..-~----'----~----'
o 10 20
COD (!JID)

Fig. 6. Effect of fiber volume fraction on the R-curve behavior in SiC (CVD) fiber-
reinforced soda-borosilicate glass matrix composite (O'o=10MPa, 11.=0.2).

24
 The toughening of continuous fiber-reinforced ceramic matrix composites has been
analyzed based on the shear-lag analysis. The effect of thermally-induced stresses and
interfacial frictional coefficient on the crack bridging process is discussed based on the
calculated results for the SiC(CVD) fiber-reinforced soda-borosilicate glass matrix
composite. The results show the strong dependence of the crack closure force on the above
parameters. To use full potential of the bridging fibers, some interfacial reaction seems
necessary to generate high level of the closure force with a small cracking length ~a of the
matrix. However,-the maximum level of the interfacial bonding strength is limited by the
requirements of crack bridging condition.
It is concluded that the optimization of both the thermally-induced stresses and
interfacial mechanical debonding condition will decide the optimization of the R-curve
behavior. Further work needs to be done to optimize the R-curve behavior in the continuous
fiber-reinforced ceramics matrix composites and clarify the effect of interfacial debonding
condition on the crack closure force.

REFERENCES
[1] D. B. Marshall, B. N. Cox, and A. G. Evans: The mechanics of matrix cracking in
brittle-matrix fiber composites, Acta Metall, Vol. 33, No. 11,2013-2021, (1985)

[2] B. Budiansky, J. W. Hutchinson and A. G. Evans, Matrix fracture in fiber-reinforced

ceramics, 1. Mech. Phys. Solids, Vol. 34, No.2, pp. 167-189, (1986)

[3] L. N. McCartney, Mechanics of matrix cracking in brittle-matrix fibre-reinforced

composites, Proc. R. Soc. Lond. A 409,329-350, (1987)

[4] Y. C. Gao, Y. W. Mai and B. Cotterell, Fracture of fiber-reinforced materials, 1. of

Appl. Mathe. and Phys., Vol. 39,550, (1988)

[5] B. Budiansky and J. C. Amazigo, Toughening by aligned, frictionally constrained

fibers, J. Mech. Phys. Solids, Vol. 37, No.1, pp. 93-109, (1989)

[6] L. S. Sigl and A. G. Evans, Effects of residual stress and frictional sliding on cracking
and pull-out in brittle matrix composites, Mech. of Mater. 8, 1-12, (1989)

[7] M. D. Thouless, A re-examination of the analysis of toughening in brittle-matrix

composites, Acta Metall. Vol. 37, No.9, pp. 2297-2304, (1989)

[8] J. W. Hutchinson and H. M. Jensen, Models of fiber debonding and pullout in brittle
composites with friction, Report of the Division of Applied Sciences, Harvard Univ. MECH-
157, (1990)

[9] B. Budiansky, Micromechanics II, in Proc. Tenth U.S. National Congr. Appl. Mech.,
Austin, Texas, (1986)

[to] Y. Kagawa and H. Hatta, Effect of thermally-induced stress on the fracture toughness
of the SiC(CVD) fiber-reinforced glass matrix composites, 1. Mater. Sci., (in contribution)

[11] S. Timoshenko and 1. N. Goodier, "Theory of Elasitisity", McGraw Hill, (1950)

[12] Y. Kagawa and H. Hatta, "Ceramic Matrix Composites; Tailoring Ceramic

Composites", Agune-shoufuusha, Tokyo, (1990), (in Japanese)

25
APPENDIX A: CRACK STARTING TOUGHNESS

The crack starting toughness of the unidirectionally-reinforced composite is obtained

simply from the average values of the fracture energy required for crack growth of a unit
surface area. This energy 'f is given as

(A-I)

where X is a constant ('"1), yo is the surface energy of the matrix, 1- the surface energy of the
interface, ld is half the debonded length when 8 '" o. Then, the crack starting toughness, Gf
is given as

(A-2)

where G~ is the critical energy release rate of the matrix.

APPENDIX B: FIBER BRIDGING CONDITION

(c-l)
Interfacial Fracture
Tc
2rf mG~
L..--'t""t----I ~ ~G~
Tc Crack Propagation
(c-2) Fiber Fracture
Fig. B-1 Cylindrical crack propagation.

The requirements for crack bridging interfacial mechanical condition (Ghc: Mode II
critical energy release rate of interface) for a crack bridging is obtained using axisymmetric
model shown in Fig. B-1. After on set of matrix fracture, we assume a cylindrical crack
(Fig. B-1 (b)). In this case, the tensile force T~ of the composite required for debonding
along the interface between fiber and matrix (Fig. B-1 (c-1)) is

r fEr<Et+~Em)Ghc
T~=21tr
~Em (B-1)

26
where ~=1/f-1. On the other hand, tensile force ~ required for fracture of the fiber at the
plane of matrix cracking (Fig. B-1 (c-2» is

(B-2)

with shape factor

Y(o.)=~o.ll2( 1+~o.+~o.2_0.363o.3 +0.7310.4 )

where o.=rr/R=..J'f and Gfc

is the mode I critical energy release rate of fiber. Then, the crack
bridging condition, is given by

(B-3)

Substituting equations (B-1) and (B-2) in (B-3), we obtain requirements of interfacial mode
IT critical stress intensity factor Ghc for crack bridging condition. The final form of the
equation is

(B-4)

where ~= 1/0.-1.

The details of APPENDIXES will be published in Materials Transactions, JIM.

27
A CRACK GROWTH RESISTANCE MODEL FOR FIBRE-REINFORCED
CERAMIC MATERIALS

Limin Zhou, Yiu-Wing Mai and Yu-Chen Gao

Centre for Advanced Materials Technology

University of Sydney
N.S.W.2006
Australia

INTRODUCTION
The concept of crack-resistance curve is now commonly used to describe the
increasing resistance, in terms of either the stress intensity factor K or the potential
R
energy release rate G , to crack growth for a wide range of engineering materials
R
including many fibre composites, ceramics and cementitious materials (Atkins and
Mai, 1985; Mai, 1988; Mai, 1991; Cotterell and Mai, 1988; Foote et al., 1986). Mai
(1988) has recently discussed the various types of toughening mechanisms associated
with these different materials that would give rise to crack-tip shielding so that their
fracture toughness is apparently increased. For convenience, these toughening
mechanisms can be broadly divided into two categories, i.e. frontal shielding (ahead of
the crack tip) and wake shielding (behind the crack tip). Examples of the former are
plasticity-induced toughening, frontal microcracking, crack front deflection and
twisting, etc. Examples of the latter are notably phase transformation toughening,
fibre and grain bridging. Crack-resistance curves due to wake shielding or
"crack-interface bridging" mechanisms have been reported for several materials such
as fibre composites (Mai and Hakeem, 1984; Huang and Hull, 1989; Hashemi et al.,
1990) and coarse-grained aluminas (Swain, 1986; Mai and Lawn, 1987).

Fibre reinforced ceramic composites possess both high fracture toughness and
high tensile strength. The toughening of these composites can be achieved via the
bridging of crack surfaces by strong intact fibres in a zone behind the crack tip and by
fibre debond and pullout. The influence of bridging fibres on the fracture behaviour
can be analysed by replacing the fibres with effective crack closure stresses which
depend on the fibre pullout length, and which in turn is determined by the mechanical

Fraclure Mechanics a/Ceramics, Vol. 9

Edited by R.C. Bradt el aI.• Plenum Press, New York, 1992 29
properties of the fibre-matrix interface and the applied traction on the fibre. The
steady-state cracking of fibre reinforced composites has been investigated (Marshall et
al., 1985; Marshall and Cox, 1987; Cox et al., 1989). A simple interfacial frictional
sliding model is used in the analysis in which the friction stress on the interface is
assumed constant and the effect of Poisson contraction of the fibre is ignored. Some of
these assumptions are approximate and in this paper a more complete analysis is
presented which addresses these problems.

For many ceramic composites in which both the fibres and matrix are brittle,
fracture processes involving interface debonding between fibre and matrix and
subsequent fibre pullout may make an important contribution to the total fracture
toughness. Good bonding between fibre and matrix is necessary to enable efficient
stress transfer from matrix to fibre but weak bonding is needed to promote high
fracture toughness. A compromise is hence often needed to obtain both high strength
and high toughness of ceramic composites. A comprehensive review on how the
interfacial properties affect the strength and toughness of polymer matrix-fibre
composites, including the various methods for improving the fracture toughness by
means of interface control, has recently been given by Kim and Mai (1991). Some of
these concepts and techniques may be readily used for ceramic matrix composites.

In the present study, we consider a fibre reinforced ceramic with a pre-existing

penny-shaped crack in the matrix and the fibres are unidirectional and perpendicular
to the crack surface. A remote uniaxial stress is applied to the composite as shown in
Fig. 1. When the applied stress reaches a critical value, which depends on the initial
interfacial debonding stress or frictional pullout stress, the crack starts to open up but
the fibres remain intact. Simultaneously, a series of microfailure processes occur near
the crack surfaces and these include fibre-matrix interface debonding, non-uniform
sliding between fibre and matrix and fibre pullout. When the applied load is increased
further the matrix crack begins to grow encompassing more bridging fibres. The
resultant process gives rise to the rising crack-resistance curve mentioned earlier. The
purpose of this paper is to present a crack-resistance curve model for ceramic matrix
composites by means of Hankel's transformation and a fibre pullout analysis which
includes all the microfailure processes of fibre-matrix debond and fibre pullout.

DEFORMATION OF INTERFACE DEBONDING REGION

Fibre Pullout Model

Gao, Mai and Cotterell (1988) considered a shear lag model where a fibre with a radius
rf is embedded in a cylindrical shell of matrix with an outer radius, b = rf/.;cf (C f is
the volume fraction of fibre), as shown in Fig. 2. z is the direction parallel to the fibre

30
axis. The composite is fixed at one end (z = L) of the fibre and a tensile stress is
applied at the other end (z = 0). An initially debonded region is treated as a
pre-<:rack. On the assumption of plane strain deformation, Gao et al. (1988) have
derived the relationships between the debonding stress O'p partial debonding length l,

fibre stress at the debonding crack tip O'fl and fibre pullout length om' i.e.

(1)

(2)

(3)

where

(4)

(1 - 2kvf )( av f + 'yvm )
K = vfla + ,- 2k( aVf + IV m)]'
(5)

a =EmlEf (Young's modulus ratio of matrix to fibre), ,= Cf/Cm (volume fraction

ratio of fibre to matrix) and vf and vm are fibre and matrix Poisson ratios. 0'0 is the

frictionless initial debonding stress, 0'* the asymptotic debonding stress, and ), the

reciprocal length giving the effective frictional stress transfer distance. The
experimentally determined parameters 0'0' 0'* and), are related to the interfacial
fracture toughness (, the residual clamping stress qo and the coefficient of friction at

the debonded interface J1. by

(6)

(7)

(8)

31
 (fro
t
z

__..=-. =- ~f-.=-_=- .
;

;[7
c::.~:-_:-
____ A. .• _:.:. •.••.• _ -. . -.
r
7
:0
debonding region

!
(fro
Uro
Fig. 1. A schematic of the penny crack which is bridged
by fibres and loaded by a .
III

2~

2
L-l

6 0
L..-.L-_~m,

•
~
Fig. 2. A schematic of the fibre pullout problem.

32
From Eqn. (1), the debonded length I corresponding to the debonding stress I1f can be

written as

(9)

Thus, the fibre pullout length 6 can be rewritten as

m

(10)

When the embedded fibre length L is very short the interface debonding process is
unstable (Kim et al., 1991). After complete debonding along the full embedded length
L the fibre is pulled out from the matrix and the relation between the frictional fibre
pullout stress and fibre pullout length can be obtained from Eqn. (2) by using the
boundary condition at the embedded end of the fibre (l1fl = 0) as

(11)

where the maximum frictional pullout stress (i.e. initial frictional pullout stress) is
given by

lW f 11 *( eAL - 1)
I1fmax = 'W + lWf)\L .
m

Relations (10) and (11) are plotted in Fig. 3 for an untreated SiC fibre-glass matrix
composite whose material properties including those of the interface are given later.

Effective Crack Opening Displacement

The opening displacement of a matrix crack which is bridged by uniaxially

aligned fibres can only be accommodated by a debonded region near the crack-surface
where non-uniform slipping of the fibre relative to the matrix takes place and by fibre
pullout across the surfaces of the matrix crack (Fig. 1). The restraining effect of the
fibres causes a reduction in both the matrix crack opening displacement and the
resultant stress intensity factor at the crack tip. The relationships between these
quantities and the remotely applied stress 11
lD
can be evaluated by assuming the whole

deformation process to be divided into two steps (Gao, 1989). The first step is to

33
introduce a crack which cuts across a plane containing the fibres and the matrix
material with associated stresses O"f and O"m distributed on the surface of the crack.

The total average stress can be written as

(12)

Under the action of (J and (J the crack opening displacement is 8 (Fig. 3a). The
m
second step is a fibre pullout and debonding process in which a self-equilibrated stress
system (O"f' O"m) is exerted on the surface of crack and the corresponding displacements

of fibre and matrix are represented by (8f, 8m) (Fig. 3b). The result of the two steps

must ensure that the bridging fibres are continuous and the matrix is traction free at
the crack surface. Thus,

(13)

(14)

(15)

The total fibre bridging stress is

(16)

and the matrix crack opening displacement is

(17)

(Jf and 8m are the same as the debonding or frictional pullout stress (Jf and fibre

pullout length 8m given by Eqns (10) and (11) respectively in the analysis of the single

fibre pullout model. However, it is noted that the total average crack opening
displacement 8 is always smaller than the fibre pullout length 8 , A simple relation
m
between 8 and 8 has been given by Gao (1989):
m

(18)

34
 0.2

0.8
0.15

C'O 0.6 C'O

a.. a..
(') (') 0.1

b- 0.4 b-
0.05
0.2

0 0
0 2 3 4 5 0 0.5 1 1.5 2 2.5

6m 6m mm
~m
(a) (b)

Fig. 3. Plots of the stress-displacement relation of untreated SiC fibre-glass

matrix composites (Kim et al., 1991). (a) partial debonding stress l1f
as a function of pullout length 8m ; (b) frictional pullout stress as a
function of pullout length 8 ,
m

". 6 1

~---'-

(J,
(a) (b)

Fig. 4. Schematics of stresses and deformations in debonded

region. (a) A cut-plane across fibres and matrix; and
(b) fibre pullout and debond process.

35
in which a = CfEf/CmEm . From Eqns. (12) and (14) to (16) we have

(19)

and combining with Eqns. (10) and (18) this gives

(20)

For short fibre reinforced ceramic composites it is difficult to determine the

fibre distribution along the surface of the crack. However, on average, we may assume
the distribution of fibres to be uniform and symmetrical about the crack surface. If the
fibre-matrix interface is very weak we only need to consider the frictional pullout of
fibres from the matrix. Under these conditions the relationship between 6 and (J can be
obtained by

(21)

in which L* is the fibre length.

AXISYMMETRIC PROBLEM OF TRANSVERSELY ISOTROPIC MATERIALS

Basic Equations

The relationship between the remotely applied load (J and the effective crack
til

opening displacement 6 can be derived exactly by regarding the fibre reinforced

composite as a transversely isotropic material. We now consider the basic equations of
an axisymmetric problem of a transversely isotropic elastic medium in which the
z-axis of the cylindrical polar coordinate system (r, 8, z) coincides with the axis of
material symmetry. Let (u, w) denote the displacements along the radial and axial
axes respectively, and ((Jr' (JO' (Jz' T
zr ' E
r, EO' E
z' 1zr ) represent the non-zero
components of stress and strain. The following basic equations can be obtained:

36
(a) equilibrium equations

aq
_r+_z +
aT r qr - qo =0
(22a)
ar (k r

(22b)

(b) geometric equations

(23a)

(23b)

(23c)

(23d)

(c) stress-strain relationships

(24a)

(24b)

(24c)

T
rz -- A44 'Yrz (24d)

in which Aij are elastic constants which can be obtained from theoretical analysis or
experimental measurements.

In terms of the displacement function ¢>(r,z) u and w can be defined as

u=-a (25a)

(25b)

37
so that the stress components become:

= -A a3<P - A r r + {3A [a3<P +!rr + W a3 <P] (26a)

q
r 11 ~ 12 Or oz 13 ~ r oz Or &3

= -A a3 <p A ! r r + {3A [a3 <p +! r r + w a3 <p] (26b)

&3
q _
o 12 ~ 11 r or oz 13 ~ r oz Or

=-A [a3<P +!rr] +{3A [a3<P +!rr+ w a3 <P]

q
z 13 ~ r 8zOr 33 ~ r oz Or &3 (26c)

where {3 = A11 /(A I3 + A44 ), w = A44 /A 11 · Substituting the above stress

components into the equilibrium equations show that Eqn. (22a) is automatically
satisfied and Eqn. (22b) becomes

(27)

in which

2 a2 10 1 a2
V. = ~ + - - +~~ (i = 1,2)
1 or r Or Si f)z

Hankel's Transformation
Eqn. (27) is the basic differential equation for axisymmetric problems of
transversely isotropic materials. Using Hankel's transformation of zero order

38
we can express Eqn. (27) as

whose solution is given by

-S ~z -S ~z S ~z S ~z
G(~,z) = Ae 1 + Be 2 + Ce 1 + De 2 (29)

where A, B, C, D, are only functions of ~ and can be determined by the boundary

conditions. Further, using Bessel functions J and J we have
O I

(30a)

(30b)

(30c)

Basic Integral Equation

We now consider the boundary conditions for the penny-.<;haped matrix crack.
Since (Jz and ware symmetric about z = 0 we can restrict the analysis to a single
half-.<;pace (z ~ 0). In the plane of the crack at z = 0 the following boundary
conditions apply:

(J
z
= (J-(J
w
o ~ r < a; (3Ia)

w=O r>- a', (3Ib)

T = 0 r ~ 0; (3Ic)
zr

where a is the radius of the penny crack. Since the stress should be bounded at infinity
we have C = D = O. Substituting Eqn. (29) into Eqns. (30) we derive

39
 (32a)

(32b)

(32c)

From boundary condition (31c) and Eqn. (32c) we obtain

f3 - (f3w - 1)8 2
A(e) =- ~ B(e) (33)
f3 - (f3w - 1)8 1

and from (32a), (32b), (33) and boundary conditions (31b), (31c) we obtain

(a ~ r) (34)

(35)

where

Eqns. (34) and (35) are dual integral equations which can be idealised as

1o f(1J}Jo(p1J)d1J = 0
lD

(1 < p) (36)

40
 1o 1]f(r])Jo(p1/)d1/ = g(p)
w
(0 ~ p ~ 1) (37)

by the non-dimensional quantities

[o{ap) - u la5
P =!..
a'
g(p) =_ w
H

The solution of dual integral equations (36), (37) is (Sneddon, 1951)

Therefore,

_ 2 1 1 Xg(X~)
A[!l.]a = 31
7r1/ 0
~ sin(~1/) 1
0 (1 - X )
2 172 dxd~

and combining with Eqn. (32a) we have

_ 2ra [
w(ap,O) -1ilr uw(l- p)
2 1/2
-
fl 2
~ (1
2 172 J~
xu(ax~) ]
2 172 dxdx; (38)
p (x; - p ) 0 (1 - X )

in which

2
2 2 (3-({3W-l)SI]
r={3(wS
[ 1 -l)-(wS 2 -1) 2·
{3 - ({3w - I)S2

Note that the displacement w here is exactly the same as 8 given in Eqns. (20) and
(21) and this harmonious relation gives

41
 (39)

for a crack bridged by continuous long fibres and

_ 2 1/2
- (JCD(1- p) - fp1 (K2 - KP2)172 ] i01 (1xu(aXK)
2 172 dxdK
- X )
]
(40)

for a crack bridged by discontinuous short fibres. Eqns. (39) and (40) are the basic
integral equations which determine the fibre bridging stress for both long and short
fibre reinforced composites.

STRESS INTENSITY FACTOR AND CRACK GROWTH RESISTANCE CURVE

Stress Intensity Factor

The mathematical analysis of the penny-shaped matrix crack bridged by the

fibres and loaded by the remotely applied stress is now reduced to the solution of the
integral equation (39) which determines the fibre bridging stress acted on the surface of
the matrix crack. Therefore, with the crack-surfaces subjected to a net pressure, (J -
CD
(J(r) , the stress intensity factor at the crack tip can be derived as follows. From Eqns.
(32b) and (33), we obtain the stress component in the z-direction as:

z 1r 0
i
2 1 {CD
(J (ap,O) = - - K
0
i
TJJo(TJP) sin(KTJ) dTJ i
1X[(J -(J(aXK)] }
CD
0 (1 - X )
2 1/2 dX dK (41)

Further, using the following integral (Sneddon, 1951):

Jm =
nOm
i
CD
pn-1 sin ()
p e-pz J (pp) dp

42
we have

(42)

Substituting Eqn. (42) into Eqn. (41) gives

(43)

and the stress intensity factor is defined by

~
= 2~--i {H
{
lim+ fP=l
1
i01 (p2 -I\;)
1\;2 372 i
2 1X[u -u(XI\;)]
lD 2 172 dxdl\;
0 (1 - X )
}
(44)

There are two contributions to K One is the stress intensity factor due to the applied
r
load u ,K ,and other Kf due to the fibre bridging stress u, i.e.
lD a

where

= 2~u
{i lD (45)

To calculate K we introduce a polynomial to represent the continuous fibre bridging

f
stress

43
in which an is a function of crack length and applied load and is dependent on (1.

Hence,

= - 2
a +
m l
i n=1
E a n_ l I(n) (46b)

where

[
~.1r (n = 2,4,6 )
I(n) = n.. ~
(n-H!! (n = 1,3,5 )
n ..

Hence the crack tip stress intensity factor is:

(47)

Crack Growth Resistance Curve

To model matrix crack growth we propose that at equilibrium fracture the net
stress intensity factor (K ) at the crack tip is numerically equal to the intrinsic
I
fracture toughness of the reinforced-matrix material (K ) (Mai, 1988; Mai, 1991;
IC
Cotterell and Mai, 1988; Foote et al., 1986):

(48)

in which K is a function of crack growth and is a negative increasing quantity.

f
Rearranging Eqn. (48), the crack growth condition becomes

44
At equilibrium crack growth K = K which is commonly referred to as the crack
a R
growth resistance, i.e.

This is the basic equation for the crack growth resistance curve and it can be rewritten
as

(49)

NUMERICAL RESULTS

To calculate the crack growth resistance curve we choose the examples of both
untreated and acid treated SiC fibre-glass matrix composite whose material constants,
fibre radius and interfacial properties are already published by Butler, Fuller and Chan
(1990), i.e. Ef= 400 GPa, Em = 70 GPa, vf = 0.15, vm = 0.2, rf = 71 J.I1I1, Cf = 0.2,
JL = 0.048, qo = 64.5 MPa, ( = 0.964 J/m 2 for untreated fibres; JL = 0.078, qo = 72.3

MPa, ( = 2.4 J/m 2 for acid treated fibres. The elastic constants A of the
ij
transversely isotropic elastic material have been derived by Whitney and Riley (1965)
and Hashin and Rosen (1964) using the composite cylinder model. The expressions of
A.. as a function of material constants of fibre and matrix are given in the Appendix.
IJ
The fracture toughness of the glass matrix, K = 0.8 MPa.jill, is used in the
IC
calculations. Eqns. (39) and (40) are solved numerically by an iterative method
beginning with a constant initial value of fibre bridging stress on the crack surface.
The integrals are evaluated after making the transformations X = sin t and y =
~ ,..2 _ p2. The iterative process is stopped when the condition 100i+l - O"i I $ 10-8 is
satisfied. After obtaining the numerical results of 0" as a function of the position r on
the crack surface the coefficients of the polynomial, an' are determined by solving the

linear algebraic equations. Then from Eqn. (47) the stress intensity factor is
computed. Further, based on the condition of equilibrium fracture (Eqn. 48) the crack
growth resistance curve is calculated from Eqn. (49).

The computed stress intensity factors, KI' as a function of applied load, 0"00' are

plotted in Fig. 5 for a crack bridged by long and short untreated fibres. The crack
length is taken as 2 mm in these calculations. From these numerical results it is

45
 0.8 , 0.8
,;

···
,,
,,,
IS 0.6 ,, IS 0.6
,, CO
·
···
CO
a.. ,, a..
~ 0.4 ,,, ~ 0.4

···
':Z ,, ':Z
, ,,
0.2 ,, 0.2

·
,
,,
0
40 50 60 70 80 90
·
40 50 60 70 80 90 100
(f(X) MPa (f(X) MPa
a b
Fig. 5. Plots of stress intensity factor K as a function 01 applied
I
stress (J with different coefficients offriction: (a) for a
w
crack bridged with long fibres, a = 2 mm, qo = 64.4 MPa,

(= 0.964 J/m 2, C = 0.2; --J.L = 0.048; - - - J.L = 0.12.

f
(b) for a bridged crack with short fibres, a = 2 mm, L* =
4 mm, ~ = 64.5 MPa, (= 0.964 J/m 2, C = 0.2; - - J.L =
f
0.048; - - - J.L = 0.096.

14

12

10
l£
CO 8
a..
~
6
~
~ 4
,,
2

0
0 2 4 6 8 10 12

a mm
Fig. 6. KR-eurves for long SiC fibre-glass matrix composites:
- - acid treated; - - - untreated.

46
 10 9
Cf =0.25 ,...
,... ,... 6
6 ,...
,... 7
,...
,...
E
6 ,...
,...
l§ 6
n. ,... n.

""
:::!: :::!: 5
ro4 r ~4
~ ~
3
2
2

0 1
0 2 4 6 6 10 12 0 2 3 4 5 6 7
amm amm
a b

Fig. 7. KR-{;urves for long SiC fibre-glass matrix composites:

(a) effects of fibre volume fraction C and residual clamping
f
stress qo: - - - qo = 32.25 MPa; - - qo = 64.5 MPa;
(b) effect of coefficient of friction: - - - JL = 0.12;
- - JL = 0.096; - - - JL = 0.048.

14.---------------------,

10

--- --- _.... - ..... -

2 ;::_------
5 10 15 20 25
a mm

Fig. 8. KR-<:urves of untreated short SiC fibre-glass matrix composites

with fibre volume fraction C = 0.2 and different fibre lengths:
f
- - L* = 8 mm; - - - L* = 4 mm; - - - L* = 2 mm.

47
apparent that threshold stresses are required to open the crack and that these are given
by the product of the initial interfacial debonding stress (To and the fibre volume

fraction C (i.e.
f
(Tw = 46.62 MPa) for a crack bridged with long fibres or the initial

frictional pullout stress (Tfmax and Cf (i.e. (Tw = 35.46 MPa when p, = 0.048; (Tw =
71.97 MPa when p, = 0.096) for a crack bridged with short fibres.

The crack growth resistance curves, KR(a), for long SiC fibre-glass matrix

composites (both untreated and acid treated fibres) are shown in Fig. 6. The initial
radius of the penny crack is taken as 0.2 mm. It is clear that the properties of the
interface between fibre and matrix play an important role on the crack-resistance
curve. High interfacial friction gives a higher crack-resistance curve. The effects of
residual clamping stress, fibre volume fraction and coefficient of friction on KR(a) are

shown in Fig. 7. These results indicate that C is a more effective method to vary the
f
toughness curve than qo' KR(a)-eurves for the short untreated SiC fibre-glass matrix

composites are also shown in Fig. 8 to illustrate the significance of the finite length of
the fibres.

CONCLUSIONS

A theoretical model for calculating the crack growth resistance curves of both
long and short fibre reinforced ceramic composites containing a penny crack has been
presented. The fibre bridging stresses can be determined by numerically solving the
integral equations (39) and (40). The KR-eurves of both long and short SiC
fibre-glass matrix composites have been calculated to demonstrate the relative
influence of fibre volume fraction, residual fibre clamping stresses, frictional coefficient
and length of fibres.

ACKNOWLEDGEMENTS

The authors wish to thank the Australian Research Council for partial support
of this work. One of us (L.Z.) is supported by a Sydney University Postgraduate
Research Award.

REFERENCES

Atkins, A.G. and Mai, Y-W., 1985, "Elastic and Plastic Fracture," Ellis Horwood/
John Wiley, Chichester/New York.

48
Butler, E.P., Fuller, E.R. and Chan, H.M., 1990, Interface properties for ceramic
composites from a single-fibre pullout test, in: "Mater. Res. Soc. Symp. Proc.
170, II Materials Research Society, Philadelphia.
Cotterell, B. and Mai, Y-W., 1988, Modelling crack growth in fibre-reinforced
cementitious materials, Materials Forum, 11:341.
Cox, B.N., Marshall, D.B. and Thouless, M.D., 1989, The mechanics of matrix
cracking in brittle-matrix fibre composites, Acta MetalI., 33:2013.
Foote, R.M.L., Mai, Y-W. and Cotterell, B., 1986, Crack growth resistance curves in
strain-softening materials, J. Mech. & Phys. Solids, 34:593.
Gao, Y.C., 1989, Damage modelling of fibre reinforced composites, Theoretical &
Appl. Fracture Mech., 11:147.
Gao, Y.C., Mai, Y-W. and Cotterell, B., 1988, Fracture of fibre-reinforced materials,
ZAMP, 39:550.
Hashemi, S., Kinloch, A.J. and Williams, J.G., 1990, Mechanisms of delamination in a
poly(ether sulphone)-fibre composite, Compo Sci. & Tech., 37:429.
Hashin, Z. and Rosen, B.W., 1964, The elastic moduli of fibre-reinforced materials, J..
Appi. Mech., 31:223.
Huang, X.N. and Hull, D., 1989, Effects of fibre bridging on G of a unidirectional
IC
glass/epoxy composite, Compo Sci. & Tech., 35:283.
Kim, J-K., Baillie, C. and Mai, Y-W., 1991, Instability of interfacial debonding
during fibre pullout, Scripta Metall. et Mater., 25:315.
Kim, J-K. and Mai, Y-W., 1991, Compo Sci. & Tech., in press.
Mai, Y-W., 1988, Fracture resistance and fracture mechanisms of engineering
materials, Materials Forum, 11:232.
Mai, Y-W., 1991, Failure characterisation of fibre-reinforced cement composites with
R-eurve characteristics, in: "Toughening Mechanisms in Quasi-Brittle
Materials, II S.P. Shah, ed., Kluwer Academic Publishers, Dordrecht, pp.
467-505.
Mai, Y-W. and Hakeem, M.L, 1984, Slow crack growth in cellulose fibre cements, J..
Mater. Sci., 19:501.
Mai, Y-W. and Lawn, B.R., 1987, Crack-interface grain bridging as a fracture
resistance mechanism in ceramics: II, theoretical fracture mechanics model, J..
Amer. Ceram. Soc., 70:289.
Marshall, D.B., Cox, B.N. and Evans, A.G., 1985, The mechanics of matrix cracking in
brittle-matrix fibre composites, Acta Metall., 33:2013.
Sneddon, I.N., 1951, "Fourier Transforms," McGraw-Hill, New York.
Swain, M.V., 1986, R-eurve behaviour in a polycrystalline alumina material, J. Mater.
Sci. Lett., 5:1313.

49
Whitney, J.M. and Riley, M.B., 1965, Elastic stress-strain properties of
fibre-reinforced composite materials, Air Force Materials Laboratory Report
AFML-TR~5-238.

APPENDIX
The elastic constants Aij in the stress-strain relationships can be expressed in

terms of the material properties of fibre and matrix (Ef, Em' IIm' II
f
) and the

respective volume fractions (C , C ) (Hashin and Rosen, 1964; Whitney and Riley,
f m
1965) as

where El' E 2, 1112 , 1123 and G12 are the engineering constants of the transversely

isotropic materials. (Subscript 1 refers to the fibre direction and subscripts 2 and 3
refer to the transversely isotropic plane.) Thus,

50
- Em
E = 2
m 2(1 - II - 211 )
m m

51
ON THE SIZE EFFECT IN FRACTURE
OF CERAMIC-CERAMIC COMPOSITE MATERIALS

J. LLorca and M. EEces

Department of Materials Science
Polytechnic University of Madrid
ETS de Ingenieros de Caminos. 28040 - Madrid, SPAIN

INTRODUCTION
It is well known that self-similar notched structural elements become more
brittle as their size increases. This size effect is predicted by fracture mechanics, as
opposed to the classical theory of plastic collapse, which is insensitive to the specimen
dimensions. For a single-edge notch tension specimen, such as the one depicted in
Figure la, the strength criterion predicts a nominal failure stress, aN, given by,

aN = at (1 - ao I d) (1)

where ao is the initial notch length, d is the specimen width, and at stands for the
tensile strength. On the other hand, linear elastic fracture mechanics (LEFM) leads
to a nominal failure stress expressed by

(2)

where ]{!c is the material fracture toughness, and Y(ao/d) is the stress intensity
factor shape function for this particular geometry and aid ratio. Both failure loci
have been plotted vs. the width d in bilogarithmic coordinates in Figure 1b for
self-similar specimens having the same ao/d ratio. Equations (1) and (2) are upper
bounds for the failure load, and experimental results lie on the thin line in Figure lb.
Very large specimens (over a critical size d LEFM ) behave in accordance with LEFM
predictions, whereas the maximum carrying capacity of smaller samples has to be
determined by using non-linear fracture mechanics (NLFM). On the other hand, very
small specimens follow the behaviour predicted by the maximum strength criterion.
The failure of LEFM to analyse the behaviour of specimens below d LEFM is due
to the breakdown of the LEFM hypotheses, mainly that the length of the fracture
process zone has to be small as compared with d, ao, and d - an, regardless of the
physical nature of fracture mechanism (either plastic deformation, microcracking, or
crack wake surfaces interaction). d LEFM is a function of both specimen geometry
(through Y(ao/d)) and material fracture toughness. As tough materials usually have

Froclure Mechanics of Ceramics, Vol. 9

Edited by R.C. Bradt el ai., Plenum Press, New York, 1992 53
large process zones, the minimum specimen size to apply LEFM (dLEFM) increases
with K 1c .
Ceramics have been considered brittle materials and their nominal failure load
has usually been calculated by using LEFM for both laboratory specimens and struc-
tural elements, because specimen sizes were well below dLEFM. However, the devel-
opment of new, tough ceramic materials, such as transformation toughened ceramics
and fiber and whisker reinforced composites, has changed the panorama. Failure load
and post-peak behaviour in these materials cannot be studied for practical interest
sizes through LEFM, and non-linear models have to be developed to ascertain the
size effect on their fracture behaviour (Bazant and Kazemi, 1990). In addition, it
is worth noting that geometry and loading conditions can also modify the fracture
behaviour (LLorca and Elices, 1991). Both size and geometry effects have to be
taken into account when fracture properties of two ceramic materials are compared
to find out which one exhibits better behaviour, or when fracture properties obtained
in the laboratory are employed in the design of structural elements. Furthermore,
the development of testing standards should take these results into consideration.

STRENGTH CRITERION
/
LEFM CRITERION
/
d

d LEFM logd
a b

Fig. 1. (a) Specimen considered (b) Maximum load size effect diagram.

In this paper, a non-linear model, previously developed by the authors (LLorca

and Elices, 1990a and 1990b), is employed to study the influence of specimen size (in
the range of 1 to 1000 mm) and geometry on the failure load and post-peak behaviour
of a lithium aluminosilicate (LAS) glass-ceramic matrix, biaxially reinforced with
SiC fibers. The composite was chosen because the properties of the fibers, matrix
and interface are well known. Two different geometries, a center-crack panel and a
notched three-point bend beam, were analysed because they stand respectively for
the two limiting loading conditions tension and bending.

54
FRACTURE MODEL FOR FIBER-REINFORCED CERAMICS
Fracture mechanisms in fiber-reinforced ceramics
Ceramic-fibers ceramic-matrix composites present various failure modes de-
pending on fiber arrangement, the presence of notches, and fiber-matrix bonding.
If the fibers are strongly bonded to the matrix, the crack breaks the fibers as it
propagates, and the composite fails catastrophically by the growth of a single mode I
crack. A completely different behaviour is found when a weak fiber-matrix interface
is provided. The crack propagates without breaking the fibers, and those in the crack
wake bridge the crack, contributing to the composite toughening. Moreover, fibers
break within the matrix when the crack propagates further. They are pulled out,
and the energy dissipated by friction enhances the fracture resistance (Hillig, 1987).

Fig. 2. Fracture modes in laminated com-

posites containing biaxially oriented fibers
(a) Notch front perpendicular to the lam-
inate (b) Notch front parallel to the lami-
nate.

The presence of a weak fiber-matrix interface leads to two competing failure

modes. The crack may either propagate perpendicularly to the fibers, as described
in the previous paragraph, or parallel to them, taking advantage of the weak inter-
face. The dominant mechanism is controlled by the fiber spatial distribution and the
presence of notches. In uniaxially reinforced composites with the fibers oriented per-
pendicularly to the crack plane, mode I crack propagation prevails if the specimen is
unnotched (LLorca and Singh, 1990; Singh, 1991). On the other hand, if the specimen
is notched, interfacial delamination from the notch tip is dominant, and mixed-mode
fracture takes place (Marshall and Evans, 1985). In laminated composites, containing
biaxially oriented fibers, the fracture process is influenced by the orientation of the
notch (Zok et at., 1991). Specifically, when the notch front is perpendicular to the
laminate (Figure 2a), delamination cannot take place and the crack propagates in
mode I. If the notch is parallel to the laminate, failure occurs by delamination along
the interface between the fiber layers (Figure 2b).
This paper deals with the size effect of either uniaxially or biaxially fiber-
reinforced composites with a weak interface which fail by the propagation of a mode

55
I crack. The main sources of composite toughening are fiber bridging and fiber pull-
out. The stress transferred through the crack due to crack bridging, 17b, can be
calculated by assuming that the fibers slip from the matrix at a constant stress T and
that fiber strength follows a Weibull distribution, characterized by the fiber strength
L; and its Weibull modulus m. If the fiber-matrix debond resistance is neglected, T
is well below E, and the effect of residual stresses is not considered, then an explicit
expression can be obtained between 17b and w, the crack opening displacement. This
relation is given by (Thouless and Evans, 1988; LLorca and Elices, 1990a):

--= 4>mh e -</>

17b
(3)
L;Vf

where

4>= [:J¥ (4)

L; 2 R
v= (5)
2TE f (1 + 0

e
where Vf is the volume fraction of fibers, R the fiber radius, = E f VI! E m (1 - Vf),
and Ef and Em are respectively the Young's moduli of the fibers and the matrix.
As the crack propagates, fibers begin to break. The fibers broken between the
crack surfaces do not contribute further to the fracture resistance. The fibers broken
within the matrix have to be pulled out. The stress transferred by these fibers, 17 p , is
obtained by following the same assumptions mentioned above, leading to (Thouless
and Evans, 1988; LLorca and Elices, 1990a):

17 p 1-e-</> '"Y _ L;(m + l)W] if w:S (6a)

EVf = (1+0(1+m) [ 2Ef v
We

.!!:L = 0 if W ~ We (6b)
L;Vf

where

(7)

and We is the critical crack opening displacement for which the interaction between
the crack surfaces vanishes. Then the total stress tranferred through the crack, 17, is
obtained by adding 17b and 17 p . The first term accounts for the elastic energy stored
in the non-broken fibers, whereas the second one stands for the energy dissipated
by friction during fiber pull-out. As both mechanisms can be modeled by stresses
acting on the crack wake, and the material outside the crack region can be considered
elastic, a cohesive crack model is used in the next section to determine the mechanical
behaviour of notched specimens.

56
Mechanical behaviour
As the crack propagates, bridging and pull-out stresses are applied in the crack
wake. At any given crack length, a, the crack will grow when the stress intensity
factor at the crack tip reaches the matrix fracture toughness, /{ M. Mathematically,

/{M = /{p(a) - /{u(a) (8)

where /{ p( a) is the stress intensity factor due to the applied external load, P, and
/ {u the stress intensity factor induced by the cohesive forces applied on the crack

surfaces. /{ p( a) is given by

/{p(a) = aNV1W' F(a/d) (9)

where aN is the nominal externally applied stress and F( a/ d) the stress intensity
factor shape function. For a center-crack panel (CCP) under uniaxial tension, such
as the one depicted in Figure 3a, aN = P /2bd, b being the specimen thickness. For
a three-point bend beam (TPB) (see Figure 3b), aN = 3PS/2bd2 , S being the beam
span between the supports.

p
.,
4d

~ I
~

ao ]
2d
t pn Pl2 t
P
I( s= 4d
.1
a r b

Fig. 3. Specimens considered (a) Center-crack panel

(CCP) (b) Three-point bend beam (TPB).

/{u( a) can be obtained by adding up the individual contributions of the cohesive

forces acting in the crack wake according to

/{u(a) = r 2a~)] . H(a/d, x/a) dx

lao 7l"a
(10)

where ao is one half of the initial notch length for the CCP (or the full initial notch
length in the beam), x is a dummy variable that stands for the distance from the
place where a cohesive force is applied to the center of the specimen (or to the notch

57
mouth in the beam), and H(a/d,x/a) is a shape function found in the literature
for either a CCP or a TPB of infinite length (Tada et al., 1985), which gives very
accurate values when the specimen length to width ratio is equal to, or greater than
two (Tsai and Ma, 1989).
Equation (10) is non-linear because the displacements in the crack wake w(x)
depend on both aN and a( w( x)), and it has to be solved numerically to obtain the
nominal stress that leads the crack to propagate. In order to simplify this task, it
is assumed that the crack opening displacements increase linearly with the distance
to the crack tip within the cohesive zone. This hypothesis was first introduced by
Foote et al. (1986) to study the fracture behaviour of cementitious composites, and
it has been succesfully applied to concrete (LLorca and Elices, 1990c) and ceramic
composites (LLorca and Elices, 1990a; LLorca and Singh, 1990). The details of the
procedure can be found elsewhere (LLorca and Elices, 1990c).
Once equation (10) is solved, the nominal stress a N and the cohesive stresses
acting on the crack surfaces are known. Then, the displacements at any given point of
the specimen can be calculated by using the appropiate compliance functions. They
have been previously calculated (LLorca and Elices, 1990c) for the displacement at
the notch mouth (crack mouth opening displacement, CMOD), and the displacement
of the loading point (15). In the case of the CCP, 15 is the average displacement between
the panel ends.

RESULTS AND DISCUSSION

Material properties and testing geometries
The material model chosen is a laminated lithium aluminosilicate (LAS) glass-
ceramic matrix biaxially reinforced with 50 vol. per cent of SiC fibers. Mechanical
properties of the matrix, fibers and interfaces in this material have been widely
studied in the past and the appropiate values have been picked from the references
and are listed in Table 1 (Prewo and Brennan, 1982; Marshall and Evans, 1985; Weihs
et al., 1991). The notch is assumed to be orientated as shown in Figure 2a in both
the CCP and the TPB specimens, to secure a mode I dominated failure mechanism.
The material is also assumed to be fully dense, and the Young's modulus, E, which
characterizes the elastic composite behaviour outside the crack region, is given by
the rule of mixtures,

(11 )

where Vf = 0.25 because of fiber orientation. Similarly, only the fibers perpendicular
to the crack plane contribute to the composite toughening.

Table 1. Matrix, fiber and interfacial properties for LAS

glass-ceramic reinforced with SiC fibers

Em ](M Ef ~ m R T

(GPa) (MPa m 1 / 2 ) (GPa) (GPa) (/lm) (MPa)

85 2.0 200 2.4 5 10 20

58
 Bridging and pull-out stresses calculated from equations (3) and (6) for this
particular composite are plotted in Figure 4, as a function the the crack opening dis-
placement w. Both mechanisms are almost independent. Crack bridging is dominant
for small crack opening displacements, whereas fiber pull-out controls the tail of the
(J - w curve. The area under the (J - w curve is the composite fracture energy, GF,

e.g. the energy per unit area which must be supplied to create two new, free surfaces.
G F can be divided into bridging energy, G FB, and the pull-out energy, G FP, whose
values are given in Table 2.

Table 2. Fracture energies for LAS

glass-ceramic reinforced with SiC fibers

3.59 1.42 2.17

400,--------r-----,------,------,
LAS Glass-Ceramic + 50% Vol. SiC

300

Bridging stresses
'iU
~ 200

100

Pull-out stresses
o Jr~----.:...:=-=-=~=_
o 20 40 60 80
w(l1m)

Fig. 4. Cohesive stresses, computed according to (3) and (6), as a

function of the crack opening displacement w.

The geometries studied are depicted in Figures 3a and 3b. All the dimensions
are scaled by the specimen width (2d in the CCP and d in the TPB), with d values
in the range of 1 to 1000 mm, which include the size of both laboratory specimens
and engineering components. The specimen thickness, b, is constant and equal to 10
mm in all cases. Two different initial notch lengths (ao/ d = 0.2 and 004) have been
studied. The CCP provides a remote stress state of uniaxial tension, whereas the
TPB leads to a bending moment, which are the two limiting loading conditions for a
crack under mode 1.
Nominal failure stress
The maximum nominal stresses, (J N, calculated for various sizes, are presented
in Figures 5a and 5b for the CCP and the TPB specimens respectively. In each plot,
results for two initial notch depths (0.2d and OAd) are included. Thicker lines stand
for the LEFM predictions, obtained through equation (2). In these equations, ]{[c

59
is the fracture toughness of an infinite size specimen. In this specimen, the cohesive
zone length is always small when compared with both ao and d, and under plane
stress conditions, K 1c can be calculated as

(12)

The size effect plots of Figures 5a and 5b indicate that LEFM can predict
accurately the maximum nominal stress if d is over 1 m. In other cohesive materials,

a
0.001 0.01 0.1 1
d (m)

b
0.001 0.01 0.1 1
d (m)

Fig. 5. The maximum nominal stress as a function of the specimen size

(a) CCP (b) TPB.

60
such as concrete, previous studies (Hillerborg et al., 1976) have shown that the critical
specimen size, dLEFM , below which LEFM cannot be applied, is controlled by the
material characteristic length, lck,

(13)

where at stands for the maximum stress transferred through the crack. In our ce-
ramic composite, at is 377 MPa, leading to a characteristic length of 2.87 mm. The
larger the characteristic length, the larger the critical specimen size needed to use
LEFM. In fiber-reinforced ceramics, lck is a function of the fiber, matrix and inter-
facial properties. Changes in properties which increase the fracture energy without
modifying at lead to larger lck, and thus bigger specimens are required for LEFM to
be applicable. This turns out to be the case when either the fiber radius increases or
the interfacial slipping stress decreases (LLorca and Elices, 1990a). Ar:other factor
that has an important influence on lck is the fiber Weibull modulus. When m is
large, all the fibers tend to fail in a very short range of stresses centered in I;. As the
maximum stress in the fibers which bridge the crack is attained between the crack
surfaces, the majority of them tend to break in this region, and they do not have to
be pulled out from the matrix, which limits the energy dissipation. Thus, large m
values give rise to brittle composites with short characteristic lengths. The opposite
is true when fibers have low Weibull modulus. Most of them fail within the matrix,
and the composite fracture energy increases, whereas (Jt drops. Finally, the fiber
strength also affects lck by enhancing both at and G F. As G F grows more rapidly
than a; (LLorca and Elices, 1990a) the overall effect is an increase in lck'
The size effect plots of Figure 5 clearly show that as the specimen size dimin-
ishes, the nominal failure stress aN differs from the LEFM predictions. However,
the predicted transition curve between the strength and the LEFM criteria is not a

5 00 ,-------r---....,-------,,----~--______,

400 d = 2 mm d = 100 mm

~ 300 d = 20 mm d = 50 mm
III
0.
::IE
~

I:' 200

100

2 4 6 8 10
M (mm)

Fig. 6. Cohesive stresses at the maximum load for different sizes (TPB
specimen).

61
 smooth one, and an inflexion point is found for both geometries for sizes in the range
of 2 to 5 mm. This result can be explained with the help of Figure 6, where the cohe-
sive stresses acting in the crack wake when the maximum load is reached are plotted
for various specimen sizes (2, 20, 50 and 100 mm). For very large sizes, both fiber
bridging near the crack tip and fiber pull-out far away from the crack tip have been
developed. Actually, the instability condition is attained in the case of d=l meter
(not shown in Figure 6) when both are completely developed and the crack opening
displacement at the initial notch root is We. As the specimen size decreases, the
amount of energy dissipated by fiber pull-out in the crack wake lessens, and the pull-
out energy does not influence at all the instability load beyond the inflection point
in the curves depicted in Figures 5a and 5b. These results indicate that specimen
size also influences the main toughening mechanism in these composites. For large
sizes, both G F B and G F P contribute to the composite high fracture strength. As the
specimen size decreases, GF B becomes preponderant, and the factors that affect this
magnitude to a greater extent (particularly the fiber strength ~) become dominant.
The relation between the instability condition (maximum load) and the development
of the cohesive zone is also worth noting. For very large specimens, the maximum
load is reached when the cohesive zone is fully developed, and the real crack (without
cohesive stresses) starts to propagate from the initial notch root. However, this is
not true in smaller specimens, the maximum load being attained well before the real
crack has begun to propagate.

~
bJ

0.001 0.01 0.1 1

d (m)

Fig. 7. Influence of the specimen geometry on the variation of the

maximum nominal stress with specimen size.

The influence of the geometry is shown in Figure 7, where the size effect curves
for the CCP and the TPB specimens are replotted together. The CCP curve is
over the TPB one when the initial notch length is 0.2d, whereas TPB specimens
exhibit a slightly larger maximum nominal stress when ao=O.4d. The cohesive stress
distributions in the crack wake when the maximum load is reached are shown in
Figure 8 for both geometries and initial notch lengths (d = 200 mm). The cohesive

62
zone is always longer for the CCP than for the TPB, and in the former more energy
has been dissipated up to this point. However, the crack growth resistance depends
on the energy dissipated and on the shape functions of the stress intensity factors
(see equation 10). The combined effect of both factors leads to the size effect plots
depicted in Figure 7.

400 , - - - - , - - - - - - , , - - - - - - , - - - - - - - , - - - - - ,
d = 200 mm CCP
320

...... 240
(II
aId = 0.2
-
Q. o
~

t:l 160

80

5 10 15 20 25
6a (mm)

Fig. 8. Cohesive stress at maximum load for CCP and TPB specimens,
when d=200 mm.

Post-peak behaviour
The main limitation for ceramics to be used in structural applications is not
the fracture stress (which can be improved up to reasonable values by reducing the
flaw size in the surface) but the extremely brittle behaviour after the maximum load
has been attained. Hence, the post-peak behaviour of CMC is also important and
should be examined carefully. In this section, attention is paid to the influence of the
size and geometry on the characteristics of the load-displacement curves.
P - 8 curves for various specimen sizes (5, 10, 20 and 100 mm) are shown in
Figures 9a and 9b for both geometries. The circles in the curves stand for the instant
when the cohesive zone is fully developed and the real crack starts to propagate. As
mentioned above, this occurs after the maximum load has been attained for typical
laboratory specimens. Whereas the differences in the maximum nominal stress do
not depend heavily on the loading conditions, the post-peak behaviour is extremely
different in the tension panel and in the bend beam. The former exhibits a snap-
back instability in the whole range of sizes studied, whereas the latter presents a
ductile behaviour. The implications of these results are twofold. First, monolithic
ceramics are reinforced with fibers to avoid brittle fracture and to increase fracture
strength. Whereas the latter goal can be attained, providing that sufficient crack
bridging and fiber pull-out take place in the crack wake, high strength CMCs may
still exhibit catastrophic failures depending on the specimen geometry. The two limit
situations presented in Figure 9a and 9b indicate that structures loaded in tension

63
are more prone to fail in a brittle fashion than those in bending. It is worth noting
that material properties are the same, and that the transition between brittle and
ductile failure is controlled in this case by geometry and loading conditions.

200

160
tV
CL
:::E
120
:s
.c d =5 mm
~
Q:
80
II
z
d = 10 mm
~
d = 20 mm
40

a
00 2 3 4 5 6 7
old ( • 1 O· 3)

200 . - - - - - - . - - - , . - - - - - - , - - - - - - - , - - - - - ,

tV 160
CL
:::E I
.....
'\, 120
.c

-
N

.....
~

en
no 80
CO)

d =5 mm
d = 10 mm

d = 100 mm b
0.02 0.04 0.06 0.08
old

Fig. 9. Load-displacement curves (<1) CCP (b) TPB.

The second consequence of this affects the experimental determination of the

fracture properties of CMCs. The fracture behaviour of these materials can be pre-
dicted if the properties of the fibers, matrix and fiber-matrix interface within the
composite are known. Several of these properties (such as T) can be measured by
using the appropriate testing techniques (Marshall, 1984; Weihs et al., 1991), but

64
others can only be estimated. For instance, fiber Weibull modulus (m) does change
during composite processing, because defects are induced on the fiber surface due to
the high temperatures and pressures employed, and to chemical reactions with the
matrix, and the actual values within the composite can be very different from those
obtained by testing fibers which have not been processed (LLorca and Singh, 1990).
An indirect method to infer the fiber properties is based upon the experimental mea-
surement of the fracture energy G F. If the only mechanisms of energy dissipation
are those acting in the crack wake, G F can be obtained as the area under the P - 8

200 I--,------r-----r--r-;::::==::::::!::===:!:~I

160
III
Q.
:E
_ 120
'0
D
C'>I
Ii:
~ 80
II
tJz

40

00 2 345 6 7
CMOD/d (. 1 O· 3)

200 r - - T - - - - r - - - - - , - - - - - - , - - - - - - ,

160
III
Q.
:E I
.;; 120
D

--
C'>I
(f)

~ 80

d = 5 mm
40 d = 10 mm
d=20mm
d = 100 mm b
0.02 0.04 0.06 0.08
CMOD/d

Fig. 10. Load-CMOD curves (a) CCP (b) TPB.

65
curve divided by the crack surface. Under load or stroke control, fracture tests on
the CCP would be unstable, the load showing a vertical drop to zero without any
possibility for the crack to arrest, and the whole P-O curve cannot be recorded. On
the other hand, TPB specimens exhibit a more ductile behaviour, and it is easier to
get stable, stroke controlled, fracture tests. Once G F is known, it can be used to
estimate the fiber Weibull modulus within the composite through equations (3) and
(6).
For a given structure and loading system, a snap-back instability develops when
the brittleness number, SE (Bache, 1986)

2
SE = _d = __
da t_
(14)
l ch EG F

is larger than a critical value, which in turn depends on the geometry and on the
constitutive equation for the cohesive crack. Our results (Figures 9a and 9b) clearly
show that the larger the specimen size (d), the more fragile the post-peak behaviour,
in accordance with equation (14). However, this expression does not provide any
information related to the effect of specimen geometry. The plots in Figures 9a and
9b show that this factor can lead to completely different behaviours and that it is
easier to get stable tests when bend beams are used.
Another technique to get stable fracture tests is to carry out the test under
CMOD control. Figures lOa and lOb show the P - CMOD curves for the specimens
in Figure 9. In this case, the CMOD increases monotonically during the test for all
sizes, even in the tension specimens, although the specimen becomes more brittle as
the size increases.

CONCLUSIONS
The effect of the specimen size and geometry on the maximum nominal failure
stress and the post-peak behaviour of a fiber-reinforced ceramic-matrix composite
was analysed by using a cohesive crack model. The results show that LEFM can
only be used to predict the nominal failure stress if specimens are very large, (d 2:
1m), for both tension and bending remote loading conditions. For smaller sizes,
LEFM tends to overestimate the failure stress.
Crack growth resistance in these composites is provided by the mechanisms of
fiber bridging and fiber pull-out. The relative influence of both mechanisms on the
maximum nominal stress depends on the specimen size. When d is below 5 mm, only
fiber-bridging has developed in this particular composite when the maximum load is
attained, and fiber pull-out does not contribute to an increase of the failure stress. As
the size increases, fiber pull-out begins in the crack wake. The effect of fiber pull-out
increases steadily with d. For d values over 1 meter, both fiber bridging and fiber
pull-out are completely developed, and have to be taken into account in calculating
the composite failure strength. The results also show that loading conditions have
a weak influence on the maximum nominal failure stress, as compared with the size
effect.
On the other hand, the post-peak behaviour is mainly controlled by specimen
geometry and loading conditions. Tension specimens are prone to exhibit a snap-
back instability in the P-O curve beyond the maximum load point, whereas bend
beams show a ductile behaviour, the displacement rising monotonously as the stress
decreases. The smaller the size, the more ductile the behaviour, but in the range of

66
sizes used in laboratory specimens (5 mm::; d::; 100 mm), CCP always presents snap-
back inestability as opposed to the TPB beam. Thus, the TPB has an advantage over
the CCP in measuring the composite fracture energy, which requires stable fracture
tests. Another approach to performing stable tests in CCP involves using CMOD
controlled tests. The CMOD increases continuously during the fracture tests in both
CCP and TPB specimens.

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Foote, R. M. L., Mai, Y. W. and Cotterell, B., 1986, Crack growth resistance
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mechanical properties of a continuous fiber-reinforced ceramic-matrix composite to

67
the sliding resistance of the fibers, J. Am. Ceram. Soc., 74: 535.
Zok, F., Sbaizero, 0., Horn, C. L. and Evans, A.G., 1991, Mode I fracture
resistance of a laminated fiber-reinforced ceramic, J. Am. Ceram. Soc.,74: 187.

68
MATRIX CRACKING AND FIBER BRIDGING OF
CARBON FIBER REINFORCED CARBON MATRIX COMPOSITES

Mototsugu Sakai and Tatsuya Miyajima*

Department of Materials Science

Toyohashi University of Technology
Tempaku-cho, Toyohashi 441, Japan

ABSTRACT
Among the numerous microfracture processes and mechanisms that occur in
carbon fiber reinforced carbon matrix composites, studied are both the first matrix
cracking and the fiber bridging as the most important microfracture processes for
toughening these unique composite materials. For the quantitative assessment of
the fracture of these composites, it is essential to independently characterize these
fundamental microfracture processes and mechanisms. In this paper, those individ-
ual processes and mechanisms are addressed, based not only on their theoretical
fundamentals, but also from the experimental studies.

INTRODUCTION
The requirement of composite processing to blend two or more distinct phases
together invariably means a more complicated fabrication processes with increased
costs. Consequently, composite approaches are unlikely to be made in preference to
monolithic ones unless there are appreciable advantages not only in the improved
material properties, but also in the potential pedormance.

Despite the attractiveness of fiber-reinforced composites as engineering compo-

nents, they are not currently being applied to the extent that they could be. Even
where they have been adopted, it is in low stress applications, or with such large safety
factors as to nullify much of their potential. The reason for this is the difficulty and
uncertainty that exist in defining and determining their failure strength, fracture
toughness, operating lifetime in service condition, etc., because of the very compli-
cated nature of their deformation and failure behavior. Accordingly, only limited
success of the use of linear elastic fracture mechanics (LEFM) has been reported for
fiber-reinforced composite materials, although related engineering techniques which
are based on LEFM have been very successful for assessing and predicting fracture
behavior of most monolithic ceramics and metals.

* Present address: Mechanical Engineering Department, Government Industrial

Research Institute-Nagoya, Hirate-cho, Kita-ku, Nagoya 462, Japan
Frcu;lure Mechanics a/Ceramics. Vol. 9
Edited by R.C. Bradt el aI.• Plenum Press, New York, 1992 69
 In the regime of the present LEFM, it is assumed that the crack will start propa-
gating when the stress intensity factor, K, achieves a "certain" critical value, K c (the
fracture toughness). The LEFM by no means addresses and provides the physical
basis of this critical value, that is to say, the fracture criterion of LEFM is merely
a hypothesis. 1 This non-physically based LEFM criterion introduces a serious diffi-
culty and considerable confusion to the extremely complex fracture of fiber-reinforced
composite materials. The apparent composite fracture toughness determined by the
LEFM-formalism is strongly dependent on the fracture mechanics test specimen ge-
ometry and the test configuration, and is never a characteristic material parameter.
There is no rational definitions of "strength" and "toughness" for these composite
materials. Inappropriate application of LEFM to composite fracture with little or
no modification never circumvents these serious difficulties. More theoretically valid
analytical models and the related experiments on the fundamental microfracture pro-
cesses and mechanisms of composite fracture, based on a microfracture physics are
needed. To emphasize these features, the aspects addressed in this paper are both
the theoretical and experimental considerations of fundamental fracture processes
and mechanisms of carbon fiber-reinforced carbon matrix composites.

In a like/like system, such as carbon-fiber/carbon-matrix system, i.e., a compos-

ite system composed of fibers and matrix with very similar values of the elastic moduli
and the fracture toughnesses, a propagating matrix crack is unlikely to "recognize"
the fiber at the interface, if the interface bonding is perfect. 2 The matrix crack ex-
tends into and through the fiber without bridging and pullout of intact fibers along
the fracture path. The composite failure is thus very brittle and catastrophic. There
would be little or no property enhancement in this form of composite failure.

The microfracture processes accompanied by the main crack extension of carbon

fiber reinforced carbon matrix composites with "weak" interface bonds are believed
to be as follows: 3 The first cracking occurs at the most critical flaw in the matrix
(first matrix cracking). The matrix crack then extends to the matrix/fiber-interface.
At some critical stress level, by increasing the applied load, the component of shear
stresses developed at the interface will exceed the interfacial shear strength to allow
local interfacial debonding. This debonding will move along the interface in both
directions from the crack plane as the applied load increases. After debonding, the
fiber and the matrix slip relatively to each other to form intact fiber bridging for
further crack extension. Accordingly, the fiber is subjected to a bridging stress over
the debonding length, where Weibull statistics will dictate the failure point along
the debonding length when the tensile stress reaches the critical value. 4 After fiber
fracture, the broken ends which are gripped by the "matrix socket" resist further crack
opening through the fiber pullout process, requiring considerable frictional energy.

Among the numerous microfracture processes as discussed above, the following

three fundamental processes may be the most critical for controlling the fracture
toughness and strength of carbon fiber-reinforced carbon matrix composites:
(1) first matrix cracking,
(2) intact fiber bridging which develops behind the propagating crack-tip, and
(3) fiber pullout processes.
These essential microfracture processes will all occur, often simultaneously dur-
ing the main crack extension. By far the most important task in the quantitative
study of composite fracture is to individually characterize these fundamental mi-
crofracture processes and mechanisms. In this paper, the first matrix cracking and
the intact fiber bridging of carbon fiber reinforced carbon matrix composites are

70
mainly discussed. The microfracture mechanics and mechanisms of the fiber pullout
processes of the same carbon composites will be reported elsewhere. s

EXPERIMENTAL
Test Samples
Two different types of commercial C-fiberjC-matrix composites, a unidirection-
ally reinforced composite (ID-CjC, Nippon Steel Co., Ltd.) and a satin weave lami-
nar composite (2D-CjC, Schunk Kohlenstofftechnik GmbH) were used for the present
study. In the former composite (lD-CjC), PAN-based carbon fiber (7fLm in diam-
eter, tensile strength of 3GPa for the gage length of 25mm, Young's modulus of
230GPa) with phenolic resin were heat-treated at 1000°C, followed by impregna-
tionjcarbonization processes for four times and finally baked at 2000°C. The fiber
content, bulk density, and the Young's modulus of the resultant composite were
56vol%, 1.63gjcm3 , and 200GPa, respectively. The lamina-composite (2D-CjC) was
manufactured to contain 60vol% of the woven fabric by first layering, molding, and
curing the preimpregnated fabric. After the initial carbonization, the composite was
subjected to reimpregnation and carbonization a number of times at 1700°C until
the desired density (1.63gjcm 3 ) was achieved. The thickness of each woven plane in
the composite was about 140fLm. The details ofthe material characteristic properties
have been reported elsewhere. 6

Fracture Tests
First matrix cracking: The unidirectionally reinforced CjC composite was
used for the study of first matrix cracking, since the rather simple microstructure
has an advantage for the experimental results to be more appropriate for the test
of validity of theoretical models for first matrix cracking. Three-point flexural test
specimens with different dimensions, B = 10, W = 2, S = 70, and B = 15, W = 4,
S = 70 (mm), were machined, as depicted in Fig. 1. The tensile (or compressive)
axis of the flexural specimen coincides with the reinforcing fiber axis. In order to
introduce a controlled semi-elliptical surface flaw on the surface at a right angle to
the tensile stress, a thin steel blade (q,5.5mm) with the tip radius less than 5fLm
was used. Since the conventional fracture mechanics test specimen geometry with
a straight-through notch, such as the compact tension or the single edge-notched
bend specimen, yields a plane stress- or plane strain-state at the notch-tip, the crack
does not extend across the unidirectionally reinforcing fibers, but instead propagates
along the fiber direction by delamination cracking. However, because of the triaxial
stress-strain state of the semi-elliptical surface flaw, the present flexural test specimen
avoids such undesirable delamination cracking at the crack-tip, and results in a crack
plane passing through the composite at a right angle to the reinforcing fibers. 1

A special type of displacement-controlled test apparatus was designed for the

present st udy. A precise determination of the onset load (critical load) for first
matrix cracking, which occurs at the bottom of the semi-elliptical surface flaw, is
easily conducted through the in-situ observation of cracking at the bottom of the
surface flaw. The details of the test apparatus have been reported in the literature. 1

Fiber bridging: The laminar CjC composite was used for the study of fiber
bridging. Fracture testing employed a standard fracture mechanics specimen ge-
ometry (the wedge opening loaded (WOL) specimen). The dimensions ofthe WOL-
specimen are shown in Fig. 2. The notch-plane of the composite was machined in an

71
 p

1
s ~
~~"
~
f'/2 P/2

Fig. 1. Three-point flexural specimen with a controlled semi-elliptical

surface flaw for the fracture test for first matrix cracking.

I I I
I I
:==t====J
i i~<jJ3

Fig. 2. WOL-specimen geometry for the test for crack bridging.

72
edge-wise direction. The notch was diamond-sawed in the specimen using a O.8mm
thickness blade, and then extended about 1mm with a very thin saw made from a
razor blade to yield a sharp notch with the resulting notch-tip radius of about lOJLm.
The initial notch depth (a o ) was changed from 33 to 56mm.

Fracture mechanics tests were conducted on a displacement-controlled testing

machine using a cross-head speed of O.05mm/min. The precise measurement of
crack length (a) during quasistatic crack extension is required to determine the crack
resistance curve, R curve, in the form of crack growth resistance, K R versus incremen-
tal crack extension, Aa. However, because of the formidably complicated fracture
processes occurring in the crack-tip region of this composite, visual technique was
inapplicable not only for identifying the crack-tip location but also for determining
the precise crack length, as well. This difficulty was overcome with a thick-through
drill-hole (3mm in diameter) which was introduced to the test specimens at different
millimeters (ad away from the initial notch-tip along the crack extension path, as
shown in Fig. 2. 6

The load versus displacement relationship shows a discrete change when the
crack-tip meets the hole. This discrete change was successfully used to monitor the
precise crack extension. However, this thick-through hole affects and disturbs sig-
nificantly the stress-strain state around the crack-tip. The experimental calibration
of this hole effect is very important for precise determination of the R-curve. The
detailed experimental procedures for calibrating the hole effect have been reported
in the literature. 6

RESULTS
The interrelationship of the fracture toughness for first matrix cracking (K c ) and
the initial notch length is plotted in Fig. 3. The fracture toughness is nearly constant
(7.0 ± 0.6M Pavm) over a wide range of notch sizes. 7 It should be noticed that the
fracture toughness of the composite is considerably improved by fiber reinforcement,
while the fracture toughness values of monolithic carbons, graphites, and carbon
fibers are less than 1.5M Pavm.

The R curve of the laminar composite is illustrated in Fig. 4, in the form of

K R versus Aa (a solid line connecting cirdes). It shows a prominent rising behavior
which may result mainly from the intact fiber bridging behind the propagating crack-
tip. The KR-value increases to 22M Pavm and higher by the crack extension of
10mm from its initial value (the fracture toughness for matrix cracking, K c ) of only
7M Pavm. The dotted extrapolation to Aa = 0 in Fig. 4 was made by the use of
the KR ver,sus VKa linear relationship (Dugdale approximation, see Eq. (18)).6

DISCUSSION
First Matrix Cracking
There have been two different theoretical models advanced to predict the fracture
toughness for first matrix cracking of fiber reinforced brittle matrix composites. One
is the stress intensity approach of Marshall, Cox, and Evans,S and the other is the
energy approach of McCartney.9 In the former model, the fracture toughness for

73
 Crack length (depth), a (Jtm)

00 100
~ 10 r'---=,.:--..:,--,.....----=-.;;..::---=~~:.:;:..:::.....

cd
p...,
~
'--" -8--------0
---------00------

o0.0 0.2
0.1 0.3
Dimensionless crack length, alc ( - )

Fig. 3. Dependence on the size of surface flaw of the fracture toughness

for first matrix cracking.

25
~cd
0..
~
'--" 20
ll::
~
~
u 15
@

l
....,
'"
.iii
...
CJ)

10
..c:
....,
a:0 !
...b.O
~ 5
u
...
cd
(,)

0
0 5 10
Crack extension, 6.a (mm)

Fig. 4. Rising R curve of a laminar C/C-composite. Dashed

line was calculated from the compliance analysis (Eq.
(13». The extrapolation (dotted line) represents the
y'X(i-approximation (see Fig. 7 and Eq. (18».

74
first matrix cracking is introduced after stating "intuitively" that the matrix and
composite stress intensities scale with stresses in the ratio, Eml Eej 8

(1)

where K e and K';' are the first matrix cracking toughness of the composite and the
fracture toughness of the matrix, while Ee and Em are the Young's moduli of the
composite and the matrix, respectively. In the McCartney model, an energy-balance
consideration of a continuum model for cracking in a fiber-reinforced composite has
confirmed that the Griffith-Irwin fracture criterion is applicable to matrix cracking
in composites. McCartney derived;9

(2)

where Vm is the volume fraction of the matrix. There is a distinct discrepancy be-
tween these two expression (Eqs. (1) and (2)), not only in the analytical formulae, but
also in the numerical results of K e versus Vm as illustrated in Fig. 5. The two theories
are completely different from one another except for Vm = 1.0. The dimensionless
toughness (Kel K';') ofthe Marshall's expression (Eq. (1)) changes linearly with Vm ,
while the McCartney expression yields a maximum (= (EJ 1Em )/(2J(EJ 1Em) - 1))
at Vm = (112)[1/(1 - Eml E J )], and then reduces to zero at Vm = O.

A general consideration for the first matrix cracking of brittle matrix composites
derives from the J-integral approach. 10 Under equilibrium conditions for cracking, the
crack driving force, J, equals the crack resistance, R e ;

J = Re (3)

where R e is the potential energy-derived toughness for the composite. The value of
Re , of course, depends upon whether or not fiber cracking occurs during the crack
propagation. If the reinforcing fiber failure occurs during the matrix cracking, then
the potential energy-derived toughness is given byll

(4)

where '1m and '1J are the fracture surface energies for the matrix and the fiber, and
Vm and VJ are their volume fractions, respectively. In the case that the reinforcing
fiber is too strong to fail, i.e., it keeps intact during matrix cracking:

(5)

When the Irwin's similarity relationships (2'1m = (K';')2 1Em and R e = (K e)21Ee)
are applied to Eq. (5), they yield the McCartney formula, Eq. (2). By contrast, Eq.
(1) with the intuitive assumption that the stress intensities scale with Ee/Em can be
recast into the form:
Re = 2 ,m 'V m + VJ •
KJ 2
E
J
(6)

where use has been made of Ee = Vm . Em + VJ • E J and the Irwin's similarity.

In Eq. (6), K J is the stress intensity factor (not resistance) of the intact fibers
at the critical condition for matrix cracking. Comparing Eqs. (5) and (6), i.e.,

75
the alternative expressions of Eqs. (2) and (1), respectively, the difference of the
theoretical predictions stems from the additional second term in the right-hand side of
Eq. (6). This additional term, Vf ·(Kf 2 / Ef ), is a kind of "phantom" energy, released
from a virtual cracking process of "intact" fibers. This physically unacceptable term
overestimates the fracture toughness for first matrix cracking. 1 It is further discussed
in the following section in reference to fracture test results.

The fracture toughness for first matrix cracking of the ID-C/C composite is
shown in Fig. 5 as the plot of K e / K': versus Vm along with the theoretical predic-
tions (hatched zones) of McCartney and Marshall, respectively.1 The hatched zones
cover the theoretical predictions for the possible variation of 230 < E f < 350GPa
and 5 < Em < lOG Pa for carbon materials. The fracture toughness of the monolithic
matrix carbon, K':, was assumed to be l.OM PaJffl after an extensive survey ofthe
literature for polycrystalIine carbons and graphites with a wide range of the density,
grain size distribution and the degree of graphitization,12-15 pyrolytic carbon,16 and
glassy carbons. 11 - 19 It is interesting to note that the observed toughness value falls
between the theoretically predicted zones. This discrepancy between the experimen-
tally observed and theoretically predicted fracture toughness values may result from
a lack of proper theoretical considerations as to the crack-tip stress shielding effect
which arises from the fiber/matrix interface debonding ahead of the crack front.

Numerous microfracture processes and mechanisms have been proposed to shield

the crack-tip from the applied stresses, and to toughen composite materials, as pre-
viously mentioned. The fracture toughness of a composite can be generally described
in terms of the matrix toughness, K':, and a stress shielding coefficient, SSC, as
follows;1
K e = (SSG)· K': (7)
where SSG is defined by the nominal and the local stress intensity factors(F(a) and
F(a)'oea') in the critical condition for matrix cracking,1

SSG = F(a) (8)

F(a)'oea'

The local value of the stress intensity, F(a)'oea', is given by F(a) - tiF, where
tiF is the reduction of the stress intensity through stress "shielding" processes. In
the Marshall's and McCartney's models for elastic stress shielding ((SSG)el), which
consider only the elastic partition of the applied stresses between the fibers and the
matrix, (SSG)el is expressed by Ee/ Em and J(E e/ Em) . Vm , respectively.

Accordingly, the fracture toughness of a composite with combined toughening

processes of the elastic stress partition and the crack front debonding can be expressed
with the following formula by modifying Eq. (7) in terms of the stress shielding
coefficient for interface debonding, (SSG)db;

K e = (SSG)db . (SSG)el . K': (9)

A plausible and consistent way to accommodate the important difference between

the theoretical predictions and the experimental result which is clearly illustrated in
Fig. 5, is to invoke the term of (SSG)db in Eq. (9), where the (SSG)db-values are
0.2 '" 0.5 for the Marshall and 1.7 '" 2.9 for the McCartney models, respectively,
depending on the possible variation of 23 < E f / Em < 50 for carbon materials. It

76
 l: "
::::::: 20
--......
:::::::"
en
[j)
<l)
.::
...c:
be
::l
15
....,
0
<l)

'"'
....,
::l
u
cd
..t:l
'"0
10
<l)
N

~
8 Q
'0"'
Z
5

1
o
o 0.5 1
Volume fraction of matrix, V m
Fig. 5. Normalized fracture toughness values (Ke / K e m) for the the-
oretical models and for the experiment of a unidirectionally
reinforced C/C-composite, plotted against the matrix volume
fraction, Vm . Each hatched area indicates the variation of the
Young's moduli of the carbon fibers and the carbon matrix.

77
must be emphasized that the modified Marshall model predicts embrittling by crack
front debonding, because (SSC)db < 1.0. This embrittling by crack front debonding
is unreal and unacceptable as is evident from the considerations of delamination
toughening of Cook and Gordon 20 , and Sakai, Takeuchi, Bradt, and Fischbach. 21
The physically ambiguous excess energy, Vf . (K f 2 / Ef), in Eq. (6) gives rise to this
unacceptable embrittling.

Fiber Bridging and Rising R-curve Behavior

If the strengths of the reinforcing fibers are sufficiently large, the matrix crack
extends completely through the matrix and remains bridged by intact fibers over
the entire area of the newly formed crack surface. It is the region of unbroken
fibers behind the crack tip which leads to substantial toughening. The classical
analysis which has been credited to Aveston, Cooper, and Kelly, and is referred to
as the ACK-theory, has provided a solution for the critical stress for steady-state
fully bridged matrix cracks in unidirectionally reinforced composites. 22 However, the
ACK-theory does not relate a failure criterion to the stress intensity concept (K-
concept) of cracks in the LEFM-regime. The attempt to achieve this has been made
by Marshall, et al.,s with further improvements by McCartney.9 These theoretical
considerations have demonstrated dramatic improvements in the fracture toughness
parameters through fiber bridging.

The stress intensity factor in the crack-tip region is reduced by ~Fb as a func-
tion of the crack extension, ~a, for a matrix crack with intact fiber bridging fully
developed over ~a through its stress shielding. The crack growth resistance, K R ( =
K e + ~Kb(~a)), as a function of ~a, i.e., the expression for R-curve behavior, is
then described byl
(10)
where the stress shielding coefficient, [SSC(~a)Jb, is defined in Eq. (8) by expressing
F(a)loe.l! = F(a) - ~Fb(~a), and Ke is the composite fracture toughness for matrix
cracking.

In fiber bridging system, the following three distinctive portions reflect respective
micromechanical processes: 6
(i) a linear elastic body which surrounds the crack, the crack bridging region, a
frontal process zone, and the crack wake region, the compliance, Ce(a), of the
elastic body being dependent on the crack length, a, and predictable from the
LEFM,
(ii) a linear elastic spring system which models the crack bridging along the frac-
ture surface, the compliance, Cb(~a) being a decreasing function of the crack
extension, ~a, and
(iii) an inelastic region including various irreversible deformation and microcracking
processes not only in the frontal process zone, but also in the following crack
wake region.

The composite compliance, Ce(a), with a finite crack bridging region can be
expressed in terms of the compliance reduction, ~Cb, introduced by crack bridging,6

(11)

where
(12)

78
This compliance reduction, ~Gb(~a), by the crack bridging process is quantitatively
related to the stress intensity reduction, ~Fb(~a), and thus to the enhanced tough-
ening.

The dependencies of the loadpoint compliance on the crack length for test spec-
imens with and without crack bridging, Gc and Ge , respectively, are illustrated in
Fig. 6. 6 The decrease of the compliance from Ge to Gc by fiber bridging reflects
the increased resistance to crack opening, and then toughens the composite by fiber
bridging. Applying Irwin's similarity relationship to Eqs. (10) to (12) yields the
crack growth resistance in terms of the compliance change with crack extension: 6

dGe/da . K
(13)
dGc/da c

The rising R-curve behavior (dashed line) in Fig. 4 was thus obtained by the com-
pliance changes in Fig. 6 and Eq. (13).

An energy-derived formulation of the procedure used to determine the toughness

increment, ~Rb, of composites toughened by fiber bridging can be made applying
the J-integral j 23
(14 - 1)

21
or
u·
~Rb = O'b(u)du (14 - 2)

where O'b( a:) is the bridging stress at the distance, a: behind the crack-tip, lb is the
bridging zone length, and u· is the crack half-opening at the trailing edge of the
zone. In order to complete the integration of Eq. (14-2), the constitutive equation
for crack bridging;
(15)
must be known. In Eq. (15), A and n are numerical constants, which are dependent
on the crack bridging model. In metal and polymer systems, perfect plastic springs
are usually adopted. These have uniform bridging traction (O'b) over the bridging
zone, referred to as the Dugdale model, and given by A = O'b and n = O. In frictionally
interface-constrained ceramic composites, A = 2(V';Vm)V( T/ R)(E f . E c2/ Em 2) and
n = 1/2, in terms of the interface frictional stress T, the radii of fibers R, and the
Poisson's ratio v. 9 Because of the integral nature (Eq. (14-1) or (14-2)) for crack
bridge-toughening, these two different forms of the constitutive equations result in
the same toughness increment;

(16)

in the energy-derived expression, and

(17)

in the stress intensity expression, 24 after substituting O'bo = (2/3)Vj'O'fSl u· = (1/4)·

(R/T).(Vm2 Em 2 / E f E c2)'O'f. 2, and lb = (3/32).( 7r R)·(O'f./T),(Vm2 Em 2 /VfEcE f ) (=

79
 ---
z
--... 6
6
l-
I
0
.....
........-

U"
"'0 4
:::
CIl
.,
U
Q)
()
'" - .. -
...- "--1-'
~
.~
0. 2 C c

EJ
60
U

;-6.a-
0
30 35 40 45 50
Crack length, a (mm)

Fig. 6. Dependence of loadpoint compliance (Ce and Cc ) on the crack (or

notch) length (a or da) ora lamina C/C-composite for test specimens
without (open circles and solid line) and with fiber bridging (closed
circles and dashed line), respectively.

80
(37r/8)(E,)Vf O"f.)u*) in the Dugdale model, where O"f. is the strength ofthe reinforc-
ing fibers. In the expression of Eq. (16), the toughness increment, aRb, includes the
strain energy change per unit area for the composite around the crack plane resulting
from the matrix cracking, interface debonding, and additional load being placed on
the fiber, as well as the work done per unit area of crack surface against friction at the
fiber/matrix interface. The above discussion of crack bridge-toughening implies that
the apparent difference in the constitutive equations is not essential, but that the
information on "how strong the 'averaged' crack bridging stress (O"b O ) is", and "how
large the bridging zone length (i b ) is ", are the most important in the considerations
of toughness improvement by crack bridging. 24 The modified Dugdale model, the
most primitive and the simplest model, has advantages in practical considerations
for microfracture processes of crack bridging. The frictionally constrained interface
model, that is apparently sophisticated, but yet insufficient to describe the fracture
of real composites, leads to solving an impractical integral equation.

If the Dugdale model of uniform fiber traction stress (O"b 0) is adequate for the
present GIG-composite, then aKb must be proportional to ~ as expected from
Eq. (17);
40"b °
aKb(aa) = tiC' ~ (18)
Y 27r
The plot of K R versus ~ is shown in Fig. 7. It exhibits an excellent linear rela-
tionship between K R and ~, the slope of which gives the averaged bridging stress,
O"bo = 130MPa. It can then be converted into the fiber strength O"f. = O"bo/(2VJ!3)
of about 600M Pa. This very crude estimate for the strength of reinforcing fibers in
the composite implies that the tensile strength of the reinforcing fibers is reduced
to 1/3 of the level of the virgin fibers (about 2GPa) by perhaps through damage
introduced during the composite processing.

....
........
.....................

o 1 2 3
Crack extension, viCla (mm 1 / 2 )

Fig. 7. K R versus ~ relationship of a laminar GIG-composite.

The slope of the linear line provides the averaged crack
bridging stress, O"b 0 •

81
CONCLUDING REMARKS
The two important microfracture processes and mechanisms of carbon fiber rein-
forced carbon matrix composites, first matrix cracking and fiber bridging have been
emphasized and have been separately characterized by studies of their toughening ef-
fects. Both the theoretical and experimental aspects of these individual microfracture
processes have been addressed. The stress shielding coefficients are: (i) the elastic
stress partitions, (SSC)el ~ 2, (ii) crack front debonding, (SSC)db ~ 2.5, and (iii)
the fiber bridging, (SSC)/w ~ 4.

ACKNOWLEDGMENTS
Discussions with Profs. R.C. Bradt and M. Inagaki are gratefully acknowledged.
A part of this work was supported by the Japan Ministry of Education under a
Grant-in-Aid for Scientific Research (No. 03453073).

REFERENCES
1. M. Sakai and R.C. Bradt, Int. Mater. Rev., to be published.
2. R.W. Davidge, Compo~ite~, 18:92 (1987).
3. B. Harris, Metal Sci., August-September:351 (1980).
4. M. Sutcu, Acta Metall., 37:651 (1989).
5. T. Miyajima and M. Sakai, this volume.
6. M. Sakai and T. Miyajima, Compo Sci. Tech., 40:231 (1991); T. Miyajima and
M. Sakai, J. Mater. Re~earch, 6:539 (1991).
7. T. Miyajima and M. Sakai, J. Mater. Re~earch, in press.
8. D.B. Marshall, B.N. Cox, and A.G. Evans, Acta Metall., 33:2013 (1985).
9. L.N. McCartney, Proc. Roy. Soc. Lond., A409:329 (1987).
10. D.B. Marshall and B.N. Cox, Acta Metall., 35:2607 (1987).
11. M.D. Thouless, Acta Metall., 37:2297 (1989).
12. S. Sato, K. Kawamata, H. Awaji, and M. Miyauchi, High Temp.-High Preu.,
12:23 (1980).
13. M. Sakai, J. Yoshimura, Y. Goto, and M. Inagaki, J. Am Ceram. Soc., 71:609
(1988).
14. P.H. Hodkinson and J.S. Nadeau, J. Mater. Sci., 10:846 (1975).
15. J.M. Corum, J. Nuclear Mater., 22:41 (1967).
16. M. Sakai, R.C. Bradt, and D.B. Fischbach, J. Mater. Sci., 21:1491 (1986).
17. J .S. Nadeau, J. Am. Ceram. Soc., 56:467 (1973).
18. M. Sakai, H. Hanyu, and M. Inagaki, Proc. Int. Sym. Carbon, 1990, p. 398,
Japan Carbon Society, Tsukuba (1990).
19. W.P. Minnear, T.M. Hollenbeck, R.C. Bradt, and P.L. Walker, Jr., J. Non-Cry~t.
Solid~, 21:107 (1976).
20. J. Cook and J.E. Gordon, Proc. Roy. Soc. Lond., A282:508 (1964).
21. M. Sakai, S. Takeuchi, D.B. Fischbach, and R.C. Bradt, p. 869 in Ceramic
Microstructure~ '80, J .A. Pask, ed. Plenum, New York (1988).
22. J. Aveston, G. Cooper, and A. Kelly, p. 15 in NPL-Conf. Proc., Science and
Technology Press, Guildford (1971).
23. R.A. Schapery, Int. J. Fract., 11:141 (1975).
24. M. Sakai, ISIJ Int., to be published.

82
FIBER PULLOUT AND FRACTURE ENERGY OF C-FIBER/C-MATRIX
COMPOSITES

Tatsuya Miyajima* and Mototsugu Sakai

Department of Materials Science
Toyohashi University of Technology
Tempaku-cho, Toyohashi 441, Japan

ABSTRACT

A brief review on microfracture processes and the respective energy absorption

mechanisms of fiber-reinforced composites is made, in which emphasized is that the
fiber pullout process is of the most important for fiber-reinforced composite materials
to become "tough". An experimental technique to determine the fiber pullout energy
is proposed using a novel 3-point bend specimen. Based on the measurements of fun-
damental fracture parameters, such as fiber strength in composite ((f' f), frictional shear
strength at fiber/matrix interface (T), as well as fiber pullout energy, microfracture
mechanisms for the fiber pullout processes of C/C-composites are addressed.

INTRODUCTION

Numbers of linear and nonlinear fracture mechanics parameters based on both

stress intensity- and energy-analyses have been applied to engineering materials in-
cluding metals, ceramics, and refractory materials. The conventional linear elastic
fracture mechanics (LEFM) techniques have been very successfully used for assess-
ing and predicting the failure strength, fracture toughness, and the operating lifetime
in service conditions of most monolithic ceramics and metals 1 ,2. However, it has
been pointed out that the failure strength as well as the apparent fracture tough-
ness of fiber-reinforced composite materials determined by the LEFM-formalism are
strongly dependent on the fracture mechanics test specimen geometry and the test
configuration 3 . These parameters are by no means characteristic materials parame-
ters. This difficulty arises from the very complicated natures of the deformation and
failure behavior of fiber reinforced composite materials 4 - 6 •

In fiber reinforced composites with brittle matrix carbon, first cracking occurs in
natural defect or flaw of the matrix 6 • When the crack extends through a composite
with strongly bonded fiber/matrix interfaces, the fibers do not resist to the crack

* Present address: Mechanical Engineering Department, Government Industrial

Research Institute, Nagoya. Hirate-cho, Kita-ku, Nagoya 462, Japan.

Fracture Mechanics of Ceramics. Vol. 9

Edited by R.C. Bradt et aI.• Plenum Press. New York, 1992 83
extension, giving fracture surfaces as smooth as monolithic carbon materials 6 . In
contrast, in weak interface bonding, various microfracture processes, such as interface
debonding, fiber bridging, and fiber pullout processes operate. These microfracture
processes generally make the composite tough and strong. The strength of interface
bonding, therefore, significantly affects the fracture behavior of composite materials.

The fundamental microfracture processes and mechanism of unidirectionally re-

inforced C-fiber/C-matrix composite are surmised as follows 6 : The first cracking
occurs at the most critical flaw in the matrix, when the elastic energy release rate
(~) of the composite reaches the fracture energy (2"Ym) of the matrix carbon 7,8. The
matrix crack extends to the fiber/matrix interface. At some critical stress level, the
component of shear stresses developed at the interface will exceed the interface shear
strength to allow local interface debonding and a cylindrical crack along the fiber.
The stress-strain redistribution associated with the local interface debonding around
the fiber causes a change in the local elastic strain energy. After debonding, the
fiber and the matrix slip relatively each other to form intact fiber bridging for further
crack extension9 •10 • Accordingly, the fiber is subjected to a bridging stress over the
debonding length. The strain energy change per unit area for the composite around
the crack plane resulting from the matrix cracking, interface debonding, additional
load being placed on the fiber, combined with the work done per unit area of crack
surface against friction at the fiber/matrix interface can be expressed by 7,

~. (VmEm) . (VjT)2 .ldb

3 VIE, Eo (1)

where T is the stress in the fiber at the crack plane, and ldb is the debonding fiber
length measured from the crack plane. V and E stand for volume fraction and
Young's modulus, respectively, and the subscripts m, f, and c indicate matrix, fiber
and composite, respectively. This energy change (~b?) is equivalent to the toughness
increment of the composite in the absence of any fiber failure.

The Weibull statistics will dictate the failure point along the debonded fiber
length when the tensile stress reaches the critical valuel l - 13 . The elastic energy
stored in the bridging fibers releases by the failure of the fibers and converts into
thermal energy or eventually into the fiber pullout energy. The broken ends of fibers
which are gripped by the "matrix socket" resist to further crack opening through the
fiber pullout process, requiring a considerable frictional energy h'po)13 j

v: T
-'-
l'
10
00

z2 . Rj(z) dz (2a)

where Rj (z) is the fraction of fiber failure over an infinitesimal distance dz at point z
measured from the matrix crack plane along the fiber. T and r represent the interface
shear stress and the radii of fibers. If we assume the distribution function, Rj(z)
is uniform, such that the fiber pullout length ranges uniformly from 0 to lma'" , the
integration in Eq.(2a) can be conducted analytically to yield 4 ,

=
Vj . ~ .l2 (2b)
"Ypo 6 l' ma",

In order to understand which microfracture processes and mechanisms mainly

contribute to the toughness of fiber reinforced composite materials, we have to examine
separately the following three energy dissipation systems.

84
[1] Fracture surface energies for matrix cracking h'm), fiber cracking hi)' and for
fiberjmatrix interface hd,

[2] Toughness increment for fiber bridging system (~b.), and

[3] Frictional energy by fiber pullout process h'po)'

In general, in fiber reinforced composites, ~b. and IPO dominate the total fracture en-
ergy. It is the work-of-fracture technique 14 that is the most useful and practical for
determination of the total fracture energy of materials exhibiting complicated nonlin-
ear fractures lS such as those of fiber reinforced composites 16 - 30 • The major intent of
this work is to develop a novel test method for the quantitative determination of the
fiber pullout energy, and to discuss the related toughening processes and mechanisms
of CjC-composite materials.

EXPERIMENTAL DETERMINATION OF THE WORK-OF-PULLOUT

Samples

Two types of C-fiberjC-matrix composite materials, a unidirectionally reinforced

composite (ID-CjC, Nippon Steel Co. Ltd.) and a satin weave laminar composite
(2D-CjC, CF222, Schunk Kohlenstofftechnik), were used for the study of fracture
mechanics and mechanisms of the fiber pullout. PAN-based carbon fibers (the ten-
sile strength of 3 GPa for the gage length of 25 mm, Young's modulus of 230 GPa)
with phenolic resin were heat-treated at 1000 °C, and then followed by impregna-
tionjcarbonization processes for 4 times and finally baked at 2000 °C to produce the
ID-CjC composite. The fiber content in the resultant ID-CjC composite was 56
vol.%. On the other hand, for the 2D-CjC, a satin laminar weave of PAN-based car-
bon fibers with phenolic resin was heat-treated for carbonization, and then subjected
to reimpregnation and recarbonization at 1700 °C a number of cycles until the de-
sired density (1.611 gjcm 3 and the fiber volume fraction of 0.6) was achieved. Those
two types of the composites exhibit different fiber pullout fracture modes, a dominant
bundle-pullout of fibers for the 2D-CjC composite and the pullout of individual fibers
for the ID-CjC composite, resulting in completely different fiber pullout energies.

Fracture Test for the Work-of-Pullout

There are various types of fracture mechanics methods and specimen geometries
used in laboratory works for the study of fracture behavior of monolithic metals and
ceramics. Of these conventional test methods, both the Compact Tension (CT) and
the Single Edge-Notched Bend (SENB) techniques are most prevailing because not
only of the easiness in machining and testing but also of the exact expressions for their
stress intensity factors (K r ).

However, some critical disadvantages and difficulties appear in these conventional

fracture mechanics specimen geometries when they apply to fiber reinforced compos-
ite materials with extreme anisotropy and macroscopic inhomogeneity in mechanical
properties 3 ,31. Because of predominant delamination cracking and buckling, the crack
in a unidirectionally reinforced composite by no means extends at a right angle to the
reinforcing fibers, but propagates along the fiber direction, in addition to compressive

85
damages and fiber failure by compressive buckling. Furthermore, shear fracture on
the neutral plane of bend specimens is common.

Accordingly, in order to precisely measure the fiber pullout energy (the work-
of-pullout), the energy consumption associated with these non-essential fracture pro-
cesses (delamination cracking, buckling, shear fracture, etc.) must be eliminated com-
pletely, since these undesirable cracking and damages consume appreciable amount of
energies, and strongly perturb the work-of-pullout. One can not use the work-of-
pullout parameter for the quantitative study of fiber pullout processes unless one can
design novel test geometries and techniques which prevent these undesirable fracture
modes.

small pin 2

]b ]10
.JW
~I
40
(mm)
Fig.1 Three-point flexural specimen geometry with a circumferen-
tial notch and a compressive stress supporting pin for fiber
pullout test.

The "work-of-fracture" technique was adopted in this work to determine the fiber
pullout energy(work-of-pullout; "'tpo). The work-of-fracture bwo!) is approximated
to be the sum of the elastic energy release bez) and the fiber pullout energy bpo):

"'two! = "'tel + "'tpo, (3)

since the contributions ofthe fracture surface energies, "'tm, and "'t!, ofthe matrix and
fibers to the work-of-fracture can be neglected in fiber reinforced composites. The "'tel
is an elastic energy release as the stresses in the fiber and the surrounding matrix relax
over a debonding distance when the fiber failure occurs. Furthermore, in a "com-
pletely" stable crack extension of the composite fracture, the released elastic energy
bel) is eventually converted and involved in the pullout energy bpo). Accordingly,
the work-of-fracture ("'two!) of fiber reinforced materials can be expressed for stable
crack extension by
"'two! = "'tpo (4)

86
 A novel test specimen geometry used in the present study, a flexural bar with a
deep circumferential notch perpendicular to the specimen length parallel to the fiber
orientation, is depicted in Fig.1. The most important feature of the test specimen is
that the specimen has a circumferential deep notch and a small pin (<pO.8 x 15mm).
This circumferential notch is most essential to prevent completely the undesirable
delamination cracking 16 ,17. The buckling fracture in the compressive zone of the
bending mode is eliminated by the small pin which is inserted in the slit of the rear
notch of the test specimen so that the pin supports all of the compressive load during
flexural deformation, resulting a pure tensile deformation and a pullout failure over
the unnotched remaining ligament length. Changing the ligament length, b, from
specimen to specimen is a key factor to control the pull-out fiber length; the larger
the ligament length is, the longer the length of pullout fibers results.

lOOJLm
Fig.2 SEM photographs of fractured surface for (a) ID-CjC and (b) 2D-CjC com-
posites. Crack planes are on the upper right of the pictures. A mixed pullout
mode of individual fibers and fiber bundles for the ID-CjC composite, and an
exclusive pullout of fiber bundles for the 2D-CjC composite.

RESULTS

The circumferential deep notch combined with the compressive stress supporting
pin worked satisfactorily to eliminate delamination cracking and buckling of the com-
posites. Both of the composites (ID-CjC and 2D-CjC composites) exhibit extensive
fiber pullout. However, an important difference was seen in the pullout mode, as
show~ in Fig.2. In the lD-CjC composite (Fig.2a), the pullout of individual fibers
dominate the fracture process, while the pullout of fiber bundles occurs exclusively in
the 2D-CjC composite (Fig.2b).

87
 600 (a)
ID-CjC

---
Z
400
llt

'"0
rd 200
0
Io..:l
1.0

0
0 0.2 0.4 0.6 0.8
Loadpoint Displacement, u (mm)

800 (b)
b = 5.0
2D-CjC

---
Z 600
llt
400
-d'
rd
0
Io..:l 200

o
o 0.2 0.4 0.6 0.8
Loadpoint Displacement, u (mm)
Fig.3 Load-Ioadpoint displacement relationships for (a) ID-CjC and (b) 2D-CjC
composites with different unnotched remaining ligament length, b.

88
 The load(P)-loadpoint displacement( u) relationships of test specimens with differ-
ent unnotched remaining ligament length, b, are illustrated in Fig.3a for the ID-CjC
composite and in Fig.3b for the 2D-CjC composite, which show fractures in a com-
pletely controlled manner. The smooth change and some rapid load drops in the P-u
relationships of Fig.3a correspond presumably to the pullout processes of individual
fibers and fiber bundles, respectively. As a matter of fact, a postmortem observation
of the extruding fibers on the fracture surface (see Fig.2a) confirms this mixed mode
fracture. This difference in the pullout modes, i.e., individual fibers pullout and fiber
bundle pullout, yields a significant influence to the resultant work-of-pullout, IPo, as
will be addressed in the later section.

The experimentally determined values of the work-of-pullout, IPO' are shown in

FigsAa and 4b as a function of the maximum length of pullout fibers (lma",)' The
IPo-value increases with lma"" as easily expected from the theoretical consideration
(Eq.(2b)). The comparison of FigAa and 4b emphasizes easily an important difference
in the absolute values of the work-of-pullout. The IPo-value ofthe ID-CjC composite
is about 10 times larger than that of the 2D-CjC composite. In addition, it should be
noted that the IPo-values of both ID- and 2D-composites are extremely large, about
10 2 to 103 times larger than the fracture energies of monolithic carbons and graphites.

DISCUSSION

Microfracture Parameters for Fiber Pullout Process

It has been pointed out in the preceding section that the most dominant mi-
cromechanics contribution to the fracture energy of fiber reinforced composite mate-
rials arises from the fiber pullout process. As readily expected from the theoretical
considerations of Eqs.(2a) and (2b), the fundamental parameters which control the
pullout energy, IPo, are the interface shear strength( T), the radii of fibers(r), the vol-
ume fraction of fibers(Vf ), and the pullout length of fibers(lpo)' It is theoretically
derived from the Weibull statistics that the mean pullout fiber length, < lpo >, can
be approximated by13;

Vm l' Em
--·-·-·5 (5)
m+ 1 2T E c
where m is a parameter known as the Weibull modulus and S is the fiber strength
in the composite, respectively. The more precise considerations of the mean pullout
fiber length « lpo » and the mean square pullout fiber length « l;o » are given
in the literature 13 . The most fundamental micromechanics parameters which control
the fiber pullout process in composite materials are, therefore, the parameters T, 5, r,
m, E f , Em' and Vf . In other words, once we obtain the experimental value of these
parameters, we can easily predict the pullout behavior and the pullout energy (IPO)
of the composite.

In order to make the experimental determination of these micromechanics param-

eters, in particular T and S, a new type of tensile fracture test was also conducted in
this work only for the ID-CjC composite, because of the more complicated microstruc-
ture of the satin weave 2D-CjC composite which may yield additional difficulties to
the analysis 32 • The test specimen geometry is very similar to that of the present
IPo-test (see Fig.I).

89
 .-.- 250 ...---"T""T""--...-----.,---..,.-----,--...,
'"8 (a)
.........

I
~ 200
'-'
c o
-f:
150
....::l I
o
::a
llt
100
I o
o

50/ 0

0lL-_-I-_---l_ _...1..-_---1..._ _' - - _

o 2 4 6 8 10 12
Maximum Pullout Fiber Length, {max (mm)
.-.-
'"8 10 (b)
..,..:.::
.........

'-' 8
...c
(-
o
....::l 6

-....
....... ..........
~

0
::l 4
llt
0
..:.:: 2
~

~ 0
0 1 2 3 4 5 6

Maximum Pullout Fiber Length, (max (mm)

FigA Dependence of the work-of-pullout on the maximum pullout fiber length of (a)
ID-CjC and (b) 2D-CjC composites. Dashed line in (a) was estimated by
Eq.(2b).

90
 Table 1. Fundamental Microfraeture Parameters
(Jf S (Jd T
T c""
(GPa) (GPa) (AI Pa) (MPa) (MPa)
1.2 2.2 430 3.2 11
±0.2 ±0.4 ±120 ±0.6 ±1

The relationships between the applied pure tensile load toward the reinforcing fibers
and the displacement of the slit of the circumferential deep notch were precisely mea-
sured during the fracture test. When the thickness of the remaining ligament of the
notch is smaller than a critical value, the tensile fracture always occurs through the
fiber failure over the ligament. On the contrary, when the remaining ligament is
thicker than the critical thickness, the remaining ligament is pulled completely as a
fiber bundle out ofthe surrounding composite socket. This important difference in the
fracture modes and the critical thickness of the remaining ligament were successfully
used to calculate the tensile strength of the composite (0" f), the fiber strength (5), the
interfacial shear strength (T), the critical stress for the interface debonding( 0" d), and
the shear strength of the composite (Tcu ), listed in Table 1. The details of the test
and the analysis have been reported elsewhere 32 • This test technique and the spec-
imen geometry make easier the determination of these fundamental micromechanics
parameters which have been estimated with some difficulties and uncertainties33 - 35 .

Pullout Energies for Individual Fibers and for Fiber Bundles

It has been successfully demonstrated by D.C. Phillips 16,17 in the work-of-fracture

tests of carbon fiber reinforced glass matrix composite that the theoretical relation
of Eq.(2b) reasonably suffices the experimental results, although the fracture test
may have not eliminated the energy consumption accompanied by buckling in the
flexural test specimens. The theoretical prediction of Eq.(2b) with T = 3.2 MPa
(see Table 1) is drawn in FigAa by a dashed line. A large discrepancy, an extreme
overestimate in the theory, between the observed values and the theoretical prediction
implies that the several assumptions which have been used to derive Eq.(2b), i.e.,
a constant shear resistance, T, over the frictionally constrained interfaces, an equal
distribution of pullout fiber lengths from 0 to [ma."" and the single pullout process
of individual fibers, will not be valid in the pullout processes of the present 1D-
CjC composite. As a matter of fact, Fig.1a shows a considerable amount of fiber
bundles protruding from the fracture surface, in addition to the pullout of individual
fibers. Furthermore, the interface shear stress must have a maximum value at the
onset of pullout and then rapidly decrease during the pullout process, if the interface
is chemically bonded. In addition, the distribution of pullout fiber lengths is by no
means uniform in the CjC-composite. Ofthese unreal assumptions, the most critical
one which has actually yielded the important difference between the theoretically
predicted and the experimentally observed pullout energies is to be the mixed mode
fractures of the individual fibers and the fiber bundles, since the order of magnitude
difference in the pullout energies between the 1D-CjC and the 2D-CjC composites
(see FigsAa and 4b) stems from the exclusive bundle pullout in the 2D-CjC composite
(see Fig.2b).

91
 Consider a unidirectionally fiber-reinforced composite with continuous fibers of
the radii, r, and the volume fraction, VJ. Suppose the mixed mode pullout fracture of
the fiber bundles and the individual fibers with the area fractions of ¢b and VJ (1- ¢b)
on the fracture plane, respectively. For simplicity, all bundles are assumed to have
the same radius, R, and a uniform pullout distribution. Since the numbers of the
pullout bundles and the fibers are, respectively, ¢b/7rR2 and [Vf(1- ¢b)/n 2j, the
pullout energy of the mixed mode fracture can be written by

(!) .[¢b +
6 R
VJ (1- ¢b)] . T .,2
r rna.. (6)

after assuming the same interface shear stresses, T, for bundle and fiber pullout pro-
cesses and the same maximum pullout length, 'rna.. , for these different processes.

The rate of reduction in the pullout energy by bundle pullout is defined in the
following equation,

f3 = (
_r _
RVJ
1) .¢b + i (7)

where ,po is the pullout energy in a single pullout process for individual fibers and
given in Eq.(2b). In one extreme of ¢b = 0, that is, in the extreme of no bundle-
pullout, f3 becomes unity, and Eq.(7) is reduced to Eq.(2b). On the other hand, in
the extreme of ¢b = 1, f3 is given by r /Vf R, decreasing with the radius of the pullout
bundle. The interrelationships of f3 with Rand 1po with 'rna.. are shown in Figs.5 and
6 for VJ = 0.5, R = 0.4 mm and 0.3 < ¢b < 1.0. It is easily seen in these figures that
both the bundle pullout and the thickness of bundle affect and reduce significantly the
pullout energy, 1po( = f3,po), of the composite which shows a mixed mode fracture of
the individual fibers and the fiber bundles.

The preceding theoretical consideration for the effect of the bundle-pullout on

the pullout energy is bas~d on several oversimplified assumptions, being insufficient to
make the quantitative application to the experimental results obtained in the present
study. However, the model is enough useful to explain the large discrepancy be-
tween the theoretical prediction (Eq.(2a)) and the observed ,po-value of the ID-C/C
composite, as well as the order of magnitude difference in the ,po-values between the
ID-C/C and the 2D-C/C composites. Further extensive studies and estimates of
the fraction (¢b) of pullout bundles as well as the distributions of the lengths (lpo)
and radii (R) of the bundles must be required before we proceed to more quantitative
discussions on the fiber pullout processes of fiber reinforced composites.

CONCLUDING REMARKS

The fracture energy of fiber reinforced composites is superb, exceeding over some
tens of kJ /m 2 • The major contribution to this high fracture energy arises from the
pullout processes of the reinforcing fibers during the crack extension. Microfracture
mechanics and mechanisms for the fiber pullout processes have been addressed in this
work. The pullout energies of two different types of C/C composites, ID-C/C and
2D-C/C composites, were measured with the work-of-fracture technique by the use
of a novel flexural specimens with a circumferential deep notch and a small pin which
supports the compressive stresses of the specimen. The pullout energy was strongly

92
 1.0
VI = 0.5, r = 5 }tnl
0.8
<Pb = 0.3

---
I
'--"
0.6
<Pb = 0.5

~
0.4

<Pb = 0.8
0.2

<Pb = 1.0
0.0
0 100 200 300 400
Bundle Radius, R (ttm)
Fig.5 The rate ofredudion (,8) in the pullout energy by fiber bundle pullout, estimated
by Eq.(7).

250 ,..---TT"1,....-..,.,--....------r--,.---r----,

200

150

--=
o
='
p..
....
o 50
..:.:I-l

~ 2 4 6 8 10 12

Maximum Pullout Fiber Length, e max (mm)

Fig.6 Dependence of the work-of-pullout on the area fraction of fiber bundles (<Pb) for
R = 400p.m. The lines are for <Pb = 0.0, 0.3, 0.5, 0.8, and 1.0 from the left to the
right, respectively.

93
dependent on the pullout lengths of fibers as well as the pullout modes of the fiber
bundles and the individual fibers. The pullout energy of the 2D-CjC composite is
about 10 times less than that of 1D-CjC composite, because of the exclusive bundle
pullout in the 2D-CjC composite. It has been emphasized that the quantitative
characterization of the fraction and the distribution of the lengths and the thicknesses
of pullout bundles is most required for further considerations on the fracture energy
of fiber reinforced composites.

ACKNOWLEDGMENTS
The authors are indebted to Schunk Kohlenstofftechnik GmbH and Nippon Steel
Co. Ltd. for preparing test samples. This work was supported by the Japan Ministry
of Education under a Grant-in-Aid for Science Research (No. 03453073).

REFERENCES

1. D. Broek, Elementary Engineering Fracture Mechanics, Chap. 5, Nijhoff, The

Hague (1982).
2. R.W. Hertzberg, Deformation and Fracture Mechanics of Engineering Materials,
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3. D.B. Marshall and A.G. Evans, J. Am. Ceram. Soc., 68:225 (1985).
4. A. Kelly, Proc. Roy. Soc. London, A-319:95 (1970).
5. B. Harris, Metal Science, August-September:351 (1980).
6. M. Sakai, T. Miyajima, and M. Inagaki, Compo. Sci. and Tech., 40:231 (1991).
7. L.N. McCartney, Proc. Roy. Soc. London, A-409:329 (1987).
8. T. Miyajima and M. Sakai, J. Mater. Res., in press.
9. J. Aveston, G. Cooper, and A. Kelly, p. 15 in NPL·Conj. Proc., IPC Science and
Technology Press, Guildford, U.K., (1971).
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11. M.D. Thouless and A.G. Evans, Acta Metall., 36:517 (1988).
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13. M. Sutcu, Acta Metall., 37:651 (1989).
14. J. Nakayama, J. Am. Ceram. Soc., 48:583 (1965).
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Bradt, A.G. Evans, D.P.H. Hasselman, and F.F. Lange, ed., Plenum Press, New
York (1986). .
16. D.C. Phillips, J. Mater. Sci., 7:1175 (1972).
17. D.C. Phillips, ibid., 9:1847 (1974).
18. G.A. Cooper, ibid., 5:645 (1970).
19. B. Harris, P.W. R. Beaumont, and E. Moncunill de ferran, ibid., 6:238 (1971).
20. J .F-Randolph, D.C. Phillips, P.W.R. Beaumont, and A.S. Tetelman, ibid., 7:289
(1972).
21. J.L. Heleft and B. Harris, ibid., 7:494 (1972).
22. P.W.R. Beaumont and D.C. Phillips, ibid., 7:682 (1972).
23. M. Fila, C. Bredin, and M.R. Piggott, ibid., 7:983 (1972).
24. T.U. Marston, A.G. Atkins, and D.K. Felbeck, ibid., 9:447 (1974).
25. B. Harris, J. Morley, and D.C. Phillips, ibid., 10:2050 (1975).
26. Y.W. Mai, ibid., 14:2091 (1979).
27. Y.W. Mai and 1. Hakeem, ibid., 19:501 (1984).

94
28. J .X. Zhao, R.C. Bradt, and P.L. Walker, Jr., p. 107 in Fracture Mechanics of
Ceramics, Vol. 6, R.C. Bradt, A.G. Evans, D.P.H. Hasselman, and F.F. Lange,
ed., Plenum Press, New York (1983).
29. J.K. Wells and P.W.R. Beaumont, J. Mater. Sci., 20:2735 (1985).
30. H. Stang and S.P. Shah, ibid., 21:953 (1986).
31. F. Zok, O. Sbaizero, C.L. Hom, and A.G. Evans, J. Am. Ceram. Soc., 74:187
(1991).
32. M. Sakai, T. Miyajima, and M. Inagaki, Pmc. Int. Carbon Conl, Paris, p. 488,
France Carbon Society, (1990).
33. A. Takaku and R.G.C. Arridge, J. Phys. D: Appl. Phys., 6:2038 (1973).
34. D.B. Marshall and W.C. Oliver, J. Am. Ceram. Soc., 70:542 (1987).
35. J.D. Bright, D.K. Shetty, C W. Griffin and S.Y. Limaye, ibid., 72:1891 (1988).

95
THE CRACK GROWTH RESISTANCE OF siC-sic CERAMIC COMPOSITE

MATERIALS

Moussa Gomina and Marie-Helene Rouillon

Laboratoire d'Etudes et de Recherches sur les

Materiaux, LERMAT, URA CNRS nOl317, ISMRa,
6 Bd du Marechal Juin, 14050 CAEN Cedex, France

INTRODUCTION

There remains a question about the reliability of the

crack growth resistance curves of continuous fibre-reinforced
composite materials, because of uncertainties about the crack
growth increments. It is now well known that when the dimen-
sions of the fracture specimen are the same order as the
macrostructure of the material, the R-curve behaviour is
greatly affected by the presence of a process zone in front
of the crack (Sakai, 1988) and to the eventual bridging zone
along the crack (Fourvel,1989). Theoretical or semi-empirical
methods have been developed to fit-up such behaviours to the
frame of Linear Elastic Fracture Mechanics (Sakai et al.,
1983; Shah, 1984; Mai et al., 1984, Swain, 1986). But
Whatever the method used for the investigation of the crack
growth resistance behaviour, one needs crack lengths values
along the loading curve.

These crack lengths were gained from theoretical analy-

sis based on the material's elastic constants or from experi-
mental methods as the electrical potential drop and the elec-
trical grids techniques or compliance calibration curves
using different notch depths. Direct crack lengths measure-
ments during experiment had been applied for a polycrystalli-
ne alumina (Haug et al., 1984) and hence for c-sic bidirec-
tionnal materials (Gomina, 1987). For these composites the
experimental measured crack lengths fitted well with the ite-
rative expression of Tada et al. (1973)

W - an - 1
(1)
2

where Cn and an are respectively the compliance and associa-

ted crack length values; (W - a n - 1 ) is the actual ligament
size. But the question remains whether the craok lengths
measured on the polished surfaces are representative of the
crack front position in the volume as straight-through
cracks.

FrOC/UTe Mechanics of Ceramics. Vol. 9

Edited by R.C. Bradt e/ al., Plenum Press, New' York, 1992 97
 In this paper that question is addressed and the experi-
mental crack lengths are used to work out crack growth resis-
tance curves for two types of sic-sic materials using SENB
and CT specimens.

EXPERIMENTAL PROCEDURE

Materials
The materials under study are elaborated by SEP, at
Bordeaux, France. Bidirectionnal weave made of yarns of Nica-
Ion sic fibres were stacked up and densified with Silicon
Carbide matrix deposited by the chemical vapor infiltration
method. The main characteristics of the two types of mate-
rials are a tensile strength of 200 MPa ; Young modulus of
210 GPa and ultimate failure stress E r ~ 0.15 to 0.30 % for
type I material and a tensile strength of 260 GPa'; Young
modulus of 200 GPa and E r ~ 0.6 % for type II material. They
differ mainly by the interphase treatment between the fibres
and the matrix. Opened porosity in these materials is ~ 10
vol % and the final density is 2.5.
The flat specimens for three point bending tests were
100 rom long, 10 mm wide and W (= 2.9 ; 3 or 3.5 rom) depth.
The compact tension specimens had the ASTM E399 (1983) pres-
cribed geometry 2H = 24 rom ; W = 20 rom and B = 6 but also
B = 3 rom. All specimens were tested in the edgewise orienta-
tion i.e the crack opening stress and the direction of crack
propagation lies in the plane of the tissue.

Mechanical tests
For all the specimens, the largest lateral surfaces were
polished to allow the observation of the crack path all along
the test; the notches were obtained using a 60° V-shaped
diamond wheel. A Linear Variable Differential Transducer
(LVDT) was used to monitor the load-point displacement. SENB
specimens were tested at a constant deformation rate of
10 ~m/min using a span of 90 mm and CT specimens were tested
with a crosshead speed of 30 ~m/min while recording the load-
point displacement using a LVDT. The specimens were tested
on an electromechanical Schenck Trebel-type testing machine
fitted out with a 100 kN load cell.
The set up designed for the direct crack length measure-
ment is made of an optical microscope assembled in the hori-
zontal plane and connected to a magnetoscope through a video
camera and also to a camera for photographs. The microscope
and the cameras are stuck together with a mouving stage which
vertical displacement is measured using another LVDT.
A dye penetrant method was used to measure the crack
growth increment from the notch root. A set of identifical
specimens with ao/W = 0.4 were stressed at different load
values and then unloaded for dye infiltration into the notch
root. The specimens were then loaded to rupture and the crack
length measured on both surfaces of rupture. These crack
lengths are termed "volume crack length".

98
Non Linear Fracture Mechanics parameters
Classical developments in linear elastic fracture mecha-
nics were not aimed to take into account the inelastic pro-
cesses induced by microstructural effects in ceramic composi-
tes. The impact of these mechanisms on the R-curve behaviour
has been addressed by a few authors (Barker, 1979 ; Eftis and
al., 1975 ; Sakai et al., 1983) as energy-based approaches to
the fracture of inelastic materials.
Basically, the incremental work of fracture (R) is wor-
ked out as the sum of a quasi-elastic strain energy rate
(GR1) and an irreversible energy consumption rate (GR2). A
graphical analysis of the load load-point displacement leads
to the expressions (Mai and Hakeem, 1984 ; Gomina et al.,
1987) :
p2 dC
GR1 (2a)
2B da

p dh r
GR2 = - (2b)
B da

R GR1 + GR2 (2c)

where P is the load value, a is the crack length, B the
specimen width, C is the compliance and h r the residual
displacement.
other methods for the evaluation of the potentiel ener-
gy-derived crack growth resistance are available but the one
above is easily tractable.
The stress-intensity derived toughness, ~, as a func-
tion of the propagating crack length (a) was calculated by:
p
~ = - Y (a/W) (3 )
BiW
where W is the specimen thichness and Y is the geometrical
factor for compact tension specimen (ASTM E399, 1983).

RESULTS AND DISCUSSION

Three point bending tests

Type I sic-sic materials
A typical load (P) - load-point displacement (h) curve
for a fracture specimen with ao/W = 0.4 is shown in Fig. 1,
along with the crack growth increments (~a) measured on the
polished surface of the specimen (squares), and in the volume
(solid circles). The first microcrack in the frontal portion
of the notch tip appears while the loading curve behaves
linear and the crack growth rate is high until the maximum
load value is reached. To the decreasing portion of the P-h
curve corresponds a lower rate of increase in the crack

99
 7 -,-----------------,-250
o
6
9' '0. 20 SiC-SiC 200
5 G\ EDGEWISE
E4
E
G.
0,
100.10.3,5 ("1("13
QO/w-O.4
150
';3
<J
·0"0. 0 visual 00
y
2 'C'
0
'O'0'-o'.o,.o·,od e
50
1 :
oe-'----+----+-----+---+----+0
o 200 400 600 800 1000
v.m )
Fig. 1 . Correlation of a mean monotonic three point bending
curve ( ... ) with measured crack lengths on the surface (0 or
in the volume (.) for a specimen of type I material.

length, which tip reaches the end surface of the specimen

although the applied load is still high (~ lOON). Using the
dye penetrant technique no crack growth is measured in the
volume of the specimen before the maximum load value is rea-
ched while we observe a principal crack and other secondary
cracks on the polished surface. This is a consequence of the
low deformation to rupture of the sic matrix (~ 0.035 %).
Beyond the maximum load value, the crack lengths in the volu-
me are the same as those measured on the surface.

Fig. 2a illustrates the differences between the crack

lengths measured using a penetrant dye and those obtained
from expression (1). The former are matrix crack lengths (an)
while the later based on the linear elastic compliance values
(C*) are measures of the positions of the first unbroken
fibres (an) in the wake of the matrix crack. The differences
(an) between these values are then estimates of the bridging
zone size (Fig. 2b)
C*n - Cn
(4)
C*
n

where Cn is the local compliance value obtained after

unloading. Although the importance of the bridging zone dimi-
nishes with the extension of the matrix crack, no steady sta-
te value is observed.
This correction term was first proposed to take into
account the diminution of the bridging zone size when type I
SENB specimens were tested at high temperatures in air
(Fourvel, 1989).
Examples of the R-curve behaviour are shown in Fig. 3
for specimens of different widths. The general features are
(i) the particluar shape of these curves in comparaison to
those for large gra~n s~ze ceramics or ceramic composites
with a non-optimized fibre/matrix interface, (ii) the large
amount of energy consumption in non-elastic processes, (iii)
the incremental work of fracture (R) can be raisonnable ap-
proximated by the linear elastic energy release rate G; .

100
 10
e e

o dye
• TADA et 01.
Ll model

SiC-SiC GS
100. 0.3.5 mm 3
oolW-O.4

0 20 40 60 80 100
C* (.lE-7 m/ )

Fig. 2(a) . Measured crack lengths on the polished surface

(0), calculated crack lengths an using expression (1) (e) and
our modelisation an + an (0).

,
I

III ,
I
I I
I I
I
I I
I
ao r---z-1
an an I

Fig. 2(b) . Modelisation of the crack fronts relative to the

structure of the material.

101
 2 OCR'
SiC-SiC CS
100.10.2.9 mm 3 eCR2
0 00/1'.'-0.4 • CRI
OR
~8
N

~6
...,
'"
~4

2
0
0 2 0

12.,---------------,
SiC-SiC OS
00. 0.3.1 mm3
10
oo;w-o.,
'=..1,
~&:-o
o
:l.~x,;.

~~~~~::~
o 2 4 6 8 10
60 (mm)

12.,--------::---------,
SiC-SiC GS • GR1
10 00·10·3.5 m 3 e GR2
00/W=0.4 0 ~
o GR'
~8

~6
...,
'"
~Ir

2
0-1----+-----....
o 2 4 6 8 10
60 (mm)

Fig. 3 Crack growth resistance curves calculated using

crack lengths measured by the dye penetrant technique, for
type I materials.

102
Type II sic-sic materials
Unlike the type I sic-sic materials, it appears a lot of
microcracks parallel to the future principle crack which in-
validates the use of a unique crack length. Moreover, even
when stressing the specimen at a low deformation rate the
crack does not propagate in a quasi-static fashion (Fig. 4).
But the compliance lines obtained when loading-unloading the
specimen meet at the origin (P = 0 ; h = 0) despite there are
irreversible displacements (Fig. 4). Therefore these residual
displacements are a consequence of the hinderance exerted by
the fibres pulled out of the matrix.
In lack of measured crack length values, we have used
the results gained from expression (1) to calculate the R-
curve behavior in the form of the stress-derived fracture
toughness (~) shown in Fig. 5. The rapid rising ~ curve
reaches a plateau-like value of 38 MPafm and then falls as
the damage zone ahead of the crack tip approaches the end
surface of the specimen.
This steep rising curve behaviour is likely to be at-
tributed to the inapropriate use of expression (1) for crack
growth increment calculation in a such material. In fact, ex-
pression (1) neglects the crack tip shielding effects of the
bridging zone, and lead to an "effective crack length" which
meaning is so clear.

I 10 6

"
z
~

cr
'"c.
:)
0
(,,)

100 Z

100

~OO

00

o 0.2 0.4 h(mm)

Fig. 4 . Three point bending loading-unloading curve of a ty-

pe II material with the compliance lines meeting at the
origin.

103
 The results reported above from three point bending
tests suffer from a major handicap : the remaining ligaments
are too small for a sufficient crack growth increment to oc-
cur without the crack tip be affected by the effects of the
compression stress in the specimen. Therefore compact tension
specimens must be tested.

J
III
11.
---,---~ .
~
a:
~

30

25

20

o 2 l1a (mm)

Fig. 5 . ~- curve (corresponding to the loading curve in

Fig. 4) calculated using expression (1) for crack length
estimation.

Compact tension specimens

Fig. 6a and 6b show the load-load-point displacement be-

havior (dashed curves) and associated measured crack growth
increments (solid squares) respectively for the type I and II
sic-sic materials. The type II specimen with aq/W = 0.4
stands twice the maximum load value beared by an 1dentical
specimen of type I, with a nearly constant rate of crack
growth da/dh. That means the type II material damages conto-
nuously while in the type I the matrix crack grows rapidly
towards the end surface and then the fibres break. This later
material should be less damage tolerant than the former. The
~- curves associated to the loading curves in Fig. 6a and 6b
and presented in Fig. 7 behave similar to the energy-derived
R-curves of fig. 3 . The critical stress intensity factors
(K~ni) calculated using the load values, PI' at the end of
the linear behavior are respectively 4.4 and 8.5 MPafm and
the rate of increase is clearly higher for the type II mate-
rial. These critical values are not really different from the
one calculated using the load values at which the first
acoustic emission signals appear (~ 0.95 P l ). Such a ~-curve
was mentionned by Sakai and Bradt (1988) for a SiC fiber/CVI-
SiC matrix with an initiation energy of 100 J/M2 , i.e. K~ni ~
4.5 Mpafm when assuming a young modulus E ~ 200 GPa. These
values are quite comparable to those reported for dense poly-
crystalline sic materials and testify to the mechanical qua-
lity of the cVI-sic matrix despite the high porosity.

104
 ......
a TYPE I monotonic
SiC-SiC C 25.24.3 mm 3 cO/W-OA n 0 14
12 1000
,
0 .... BOO
~B /
,
E / 600
-S6 z
0 / " 400~
4
.' "
<J

2 200

a 0
a 100 200 300 400 500 600
h u.m}

TYPE II monotonic
b
S;C-SiC CT 25.24.3 mm 3 oO/W~O.4 nO '6
12 2000
/'
10
1500
~8 z
E
$5 1000Ci:"
0
<J J"
"
4
" 500
2 / '0

0
0 100 200 300 400 500
a
h (/lm)

Fig. 6 . Monotonic loading curves of CT specimens (dashed

curves) and crack growth increments measured on the surfaces
for type I (6a) and type I I materials (6b).

105
 150.------------,-----------,
o Type II
• Type I
I
f
~
I
E 100 I

'>o ~

,.'/'
I
Q..
:::!
IY 50
/
Y /y

17 19 21 25
a(mm)

Fig. 7 • ~-curves associated to the loading curves of Fig.6.

lYPE \I monotonic
SiC SiC CT 25-24-3 mm 3 00/W=O.4 n0 16
12 - r - - - - - - - - - - - - - - - ,
10 •
o GR-
8 • KR 2/E 0
N •
E
...., 6
....... 0

2S 4
.0
•
2 0
o ,_~,,~"(lQo
13 15 17 19 21 23 25
a (mm)

Fig. 8 • Comparaison of the linear elastic energy release ra-

te G; to the Irwin relation K~/E', for a CT specimen of type
II material.

106
 To evaluate the amount of linear-elastic behaviour of
the type II material as we asserted from the three point loa-
ding curve, we have plotted the usual linear elastic energy
release rate G; and the Irwin relation ~ IE' (~ are taken
from Fig. 7b ; E' ~ 200 GPa) as function of the crack length
(Fig. 8). The good correlation between the two parameters at-
tests that the type II material behaves linear elastic.

The dependence of the ~ curve on the specimen width B

is illustrated in Fig. 9 for two values B = 3 and 6 rom. The
thicker the specimen is, the lower is the crack growth resis-
tance curve. That is the coromon problem of defining the mini-
mum specimen dimensions needed if geometry-free fracture
parameters values are to be found. For these materials sub-
jected to large scale bridging, the resistance curves obtai-
ned from small specimens overestimate the intrinsic resistan-
ce behavior (Zok and Hom, 1990).

TYPE II material (monotonic loading)

SiC-SiC CT 25.24.8 mm 3 00!W=0.4
150

o
(J n'l
n'2
!
8=6mm
I
/
I

.....-- • n014 B=3mm

E 100
';>
0
0...
L
'-../
a:::: 50
~

19 21 23 25
a(mm)

Fig. 9 . Illustration of the dependence of the ~ curves on

the width of the CT specimens of type II material.

As an example, scanning electron microscope observa-

tions of the surfaces of rupture of CT specimens show short
pUllout lengths for the type II material with B = 6 rom, with
multiple matrix cracks joining the fibres (Fig. lOa). This is
also observed for thinner specimens (B = 3 mm). On the oppo-
site pullout lengths are exceptionnaly long for the type I
material with B = 3 mm, with the fibres tightly bonded to the
matrix (Fig. lOb). These differences are very important since
they are related to the nature of the interphase between the
fibres and the matrix. A material with a high value of ulti-
mate deformation to rupture E r is not automatically credited
with long pull-out length. Long pull-out lengths result from
the association of low Weibull modulus fibres (m ~ 4 for in-
situ sic fibres) and a weak interphase which deflects cracks
propagating normal to the interface (type I material). In
type II material, damaging the interface occurs without spec-
tacular pull-out lengths.
These observations coupled to the crack growth resis-
tance curves shown above mean that the results obtained are
dependent on the specimens dimensions.

107
 a

b
Fig. 10 • Scanning electron micrographs of CT specimens (a) :
short pull-out lengths with cracked matrix for type II mate-
rials with B = 6 rom ; (b) : long pUll-out lengths for type I
materials with B = 3 rom.

SUMMARY AND CONCLUSION

The crack growth resistance curves for two types of sic-

-fibres/CVI-SiC matrix materials were investigated using
three point bending specimens and compact tension specimens.
It has been shown that the crack growth increments calculated
using linear elastic asumptions underestimate the measured
crack lengths on the polished surface of the specimen when
crack mouths bridging occurs. It follows that the behaviour
of the K R- ~a curves of advanced fibre-reinforced ceramic
composites are different from the one generally observed for
large grains polycrystalline ceramics. Continuously rising ~
-curves are obtained as a consequence of the extended crack
surfaces bridging zone by intact reinforcement, although the
initiation values are low (3 to 5 MPafm).
The authors are grateful to MM Cavalier, Bourgeon and
Jouin of SEP Bordeaux, for the delivery of the machined spe-
cimens and for the valuable comments.

108
REFERENCES
ASTM Standard E399-81, 1983, Annual Book of ASTM Standards,
part 10, American Society for Testing and Materials,
Philadelphia, PA.
Barker, L.M., 1979, "Theory for determining KIC from small,
non LEFM specimens, supported by experiments on alumi-
nium". Int. Journ. Fract., 15 (6), 515.
Eftis, J., Jones, D.L., and Liebowitz, H., 1975, "On fracture
toughness evaluation for semi brittle fracture". Eng.
Frac. Mech., 7 : 101.
Fourvel P., 1989, "Etude du comportement mecanique a l'am-
biante et a haute temperature d'un materiau composite
ceramique a fibres sic-sic non protege", These de Doc-
teur de l'Universite de CAEN.
Fourvel P., Gomina, M. and Chermant J.L., 1990, "Etude de la
resistance a la propagation de fissure et a l'endommage-
ment d'un composite sic-sic non protege, a haute tempe-
rature et sous air, Actes du Colloque organise par AMAC-
/CODEMAC, edite par NASLAIN et al., Bordeaux, 153.
Gomina, M. 1987, "Crack length measurements in a c-sic compo-
site material", Int. J. Fract., 35 : R69.
Haug, T., Bornhauser, A.C., Schmid, H.G., Gerold, V. and
Pabst, R.F., 1984, "The high temperature crack resistan-
ce Al z 0 3 ceramics containing a glassy phase", in "Creep
and Fracture of Engineering Materials and structures",
Swansea, U.K.
Mai, Y.W. and Hakeem, M.I., 1984, "Slow crack growth in cel-
lulose fibre cements", J. Mat. Sci., 19 : 501.
Mai, Y.W. and Atkins A.G., 1985, "General equations in the
mechanics of fracture accounting for unloading displace-
ment irreversibilities", Int. J. Fract., 27 : R103.
Sakai, M., Urashima, K., and Inagaki, M., 1983. Energy Prin-
ciple of Elastic-Plastic Fracture and its application to
the Fracture mechanics of a Polycrystalline Graphite. J.
Am. Ceram. Soc., 66 : 868.
Sakai, M., and Bradt, R.C., 1988 "The crack growth resistance
Curve of a non-phase-transforming Ceramics", Nippon-Se-
ramikkusu-Kyokai-Gakujutsu-Ronbunski 96 [8] : 801.
Sakai, M., Yoshimra, J., Goto, Y., and Inagaki, M., 1988
R-curve behaviour of a polycrystalline Graphite : Micro-
cracking and grain bridging in the wake region. J. Am.
Ceram. Soc., 71 [8] : 609.
Shah, S.P., 1984, "Fracture of Cement and concrete" in Advan-
ces in Fracture Research Vol 1 495, S.R., Valluri,
D.M.R., Taplin, P. Ramarao, J.F., Knott, R. Dubey, eds.,
Pergamon Press.
Swain, M.V. and Burns, S.J.,1986,J. Am. Ceram., 69, n03: 226.
Tada H., Paris, P.C. and Irwin G.R., 1973, The stress Analy-
sis of crack Handbook Del Research Corp. Hellertown, PA.
Zok, F. and Hom, C.L., 1990, "Large scale bridging in brittle
matrix composites", Acta Metall. Mater., 38 [10] : 1895.

109
EFFECTS OF TEMPERATURE AND OXIDATION OF THE MECHANICAL
BEHAVIOUR OF UNCOATED sic-sic COMPOSITE MATERIALS

Moussa Gomina, Jean-louis Chermant,

and Pascal Fourvel
Laboratoire d'Etudes et de Recherches sur les
Materiaux, LERMAT, URA CNRS nOl317, ISMRa,
6 Bd Marechal Juin, 14050 CAEN Cedex, France

INTRODUCTION
ceramic Composite Materials made of continuous high-
strength ceramic fibres embedded into brittle ceramic matri-
ces are now fully recognized as damage tolerant materials
despite the lower strains to failure of the matrices when
compared with that of the fibres. The increased fracture
toughness that prevents catastrophic failure of the composite
is a consequence of the dissipation of crack propagation
energy as crack deflection at fibre/matrix interfaces and
fibres pUll-out of the matrix. Such fibre-ceramic composite
materials (CMC) are now available for specific applications
at high stress, and it has been shown that their fracture
characteristics at room temperature are dependent on the bon-
ding between fibres and matrix through the interfacial shear
stress. If the bonding is relatively weak, the fibre is allo-
wed to slide through the matrix, and then to bridge the ma-
trix crack before failing at some distance from it.
Since these materials are destined to be used at high
temperatures and severe environment conditions, the question
is whether the good damage tolerance capability is maintai-
ned. This paper deals with the evolutions of the morphology
and mechanical behavior of a sic (Nicalon)/ CVI-~SiC composi-
te material with test temperature under air, from room tempe-
rature to 1200°C.

Material and specimens

Materials
The sic-sic materials investigated are experimental bat-
ches produced by SEP (Bordeaux, France). The reinforcement
(38 vol. %) is a two directional isotropic tissue made of ce-
ramic grade Nicalon sic fibres containing 65 wt % SiC, carbon
as aggregates and SiO z (Fareed et al. 1987 ; Guigon, 1988).

Frtuture Mechanics of Ceramics, Vol. 9

Edited by R.C. Bradt et al., Plenum Press, New York, 1992 1 11
The deposition of the p-SiC matrix using the CVI method re-
sults in an important porosity (~ 15 vol. %) which localisa-
tion, orientation and size distribution had been investigated
(Gomina et al., 1983). Extensive descriptions of the mate-
rials are available in the literature (Lamicq et al., 1985).

Specimens
Flat specimens 70 rom long, 9.5 rom wide and W rom thick
(with W = 9.5; 5 and 2.5) in the edgewise and flatwise
orientations were cut from manufactured plates and tested in
three point bending using a span of 60 rom. The span to depth
ratios were 6.3(thickness 9.5 rom with 23 laminates), 12 (thi~
ckness 5 rom with 16 laminates) and 24 (thickness 2.5 mm with
7 laminates). Notched specimens were machined using a 60·
V-shaped diamond-impregnated wheel at different relative
notch depths (ao/W).

Mechanical tests

Testing eguipments
Three point bending tests were performed on a 1185
Instron machine at a crosshead speed of 20 ~m/mn, using a
10 kN load cell. The displacement of the load application
point was measured under the upper knife from the signals of
two linear differential tranducers (LVDT), through alumina
rods. These transducers were mounted sYmmetrically in respect
of the loading axis, thus ensuring a good in-plane stability.
This displacement signal used for recording the loading curve
P-h was the mean value of the two signals from the transdu-
cers. For this experimental set to be designed for high tem-
perature measurements, the push-rods, the rollers and the
bearing plates were made in polycrystalline alumina (AF 997,
Desmarquest) and were permanently set in the heating enclo-
sure.

Procedure
The first tests on these materials were run putting the
specimens in the furnace at room temperatures and then rising
the temperature to the chosen value, T. The consequence of
this long exposure of the specimens to high temperature in
air were a time effect and probably a deep oxydation effect.
Hence, in this study the specimens were introduced in the
furnace once the test temperature was reached. The excellent
thermal shock resistance of these materials allows this pro-
cedure which shortened the duration of test exposure.

Fracture mode observation techniques

The influence of the test conditions on the modification
of the crack morphology was documented using optical micros-
cope observations on the outer surfaces of the specimens,
while fracture mechanisms were analysed through scanning
electron microscope micrographs (Jeol GLS 840). The fibre-

112
coating-matrix interfaces evolution was checked using trans-
mission electron microscopy observations (Jeol 120 CX).

Non linear fracture resistance parameters

Because the unloading line in the load (P) versus dis-
placement (h) diagram does not return to the origin (P = 0 ;
h = 0) after some crack growth increment (6a), the potential
energy-derived crack growth resistance (R) is calculated as
proposed by Sakai et al. (1983). R is shown to be a superpo-
sition of the elastic non-linear processes contribution (J s )
and the energy associated to the irreversible deformation
(lfl) •

The crack growth increments (6a) were calculated from

the reloading compliance values C(a) measured on loading-
unloading curves, using the iterative expression (Tada et
al., 1975) :

w- an _ 1 Cn - Cn - 1
( 1)
2 Cn

Results and discussion

Measurements of the flexural strength and the elastic
modulus of unnotched specimens were performed in order to
check the influences of specimen thickness and temperature.
These two parameters, when associated to the loading rate and
duration, are very important for parts survival predictions.

Flexural strength u R and Elastic Modulus E

Figures l(a) and l(b) show the load versus deflection
curves for the tests run at room temperature and 900°C for
specimens of dimensions 70 * 9.5 * 5 mm3 . The change in the
slope of the composite loading curves at approximately one
half of the maximum load represents the onset of matrix cra-
cking and fibre/matrix interface microcracks. This non-linea-
rity is less pronounced as temperature increase.

Flexural strength
The maximum flexural tensile stress u R was calculated at
fracture using simple elastic beam theory and the resultant
data are represented in Fig. 2 as function of temperature for
the three groups of specimens studied. The apparent strength
increases slightly in the temperature range 22°C < T ~ 700°C
except for the thinner specimens, and then continuously drops
off. These results look very different from those reported by
Bernhardt et al. (1985) when testing these materials under
vacuun (Fig. 3). This shows the effect of the atmosphere du-
ring test : in our tests conditions the oxidation of the car-
bonaceous fibre/matrix interface is responsible of the
decreasing u R values from temperature as low as 700°C. This
point will be discussed further from microscopy observations.

113
 SIC-SIC
7Ox95x5 mm3
T=900 'C

4.50

300

150

o 50 100 hl'm-

Jg SIC-SIC
70x9.5x5 mm J
'"" T=22 'C
800

400

o 50 100 -
h(l'm)

Fig. 1. Experimental flexural curves of unnotched sic-sic

specimens of dimensions 70 * 9.5 * 5 mm3 , tested at
22·C and 900·C.

t
I
o9.5mm
:. -- ----_.~ w= • 5 ..
b-------
_::i; "
- Il-.-._.-.-. _._.- \ "'-
t> .. 02.5 ..

=--- ----A '-". '"',

., "~

..
300 "
~,". --',
.... ) . • ''0

150
"""' .....
......

o 300 600 900

Fig. 2. Flexural strength of sic-sic materials as a function

of test temperatures in air for the three specimens
depths, w.

114
 G. BERNHART-1985

C-SiC
600

500

400 SiC - SiC ~_ .......

300

200

100

o 500 1500 2000 T"C. . .

Fig. 3. Flexural strength of sic-sic and c-sic materials as a

function of test temperature in vacuum, according to
Bernhart (1985).

Elastic Modulus
The elastic modulus E measured from the linear part of
the load-deflection curve appears to be a decreasing function
of the test temperature beyond 700·C (Fig. 4), although the
measured values on thick bent specimens are to be taken with
care. since the initial value of 210 GPa at room temperature
is identical to the fibres modulus, the observed decrease of
the elastic modulus from temperature as low as 700·C is at-
tributed to thje progressive vanishing of the carbon inter-
phase under oxidizing atmosphere. Such results have been
reported by Gault and Huger (1990) when using ultrasonic
echography technique to measure Young's moduli of ceramic-
ceramic composites at high temperatures.

t
I
C9 5mm
0

-: 0
w=.2.5 ..
g :J--------------~, C 05 ..
C 'Q
~ • C ~

150
. '\
o '.tl •
C

75

o 300 600 900 T('Cl-

Fig. 4. Elastic modulus of sic-sic materials as a function of

test temperature in air for three specimen depths.

115
 Effect of span oyer depth ratio
In these sic-sic specimens, the interlaminar shear
stress is high (40 MPa) relatively to the tensile strength
(300 MPa), so the unnotched specimens do not fail by delami-
nation. The apparent flexural stresses are reported in Fig. 5
as function of specimens depth W for five values of tempera-
ture :
- at room temperature the flexural stress is unchanged from
W = 2.5 to 5 rom depth, whereas the increase from W = 5 to
9.5 rom depth is due to a smaller interlamellar shear effect,
- except for the tests run at 700·C, the flexural stresses
measured at high temperature are lower than those at room
temperature. This exception occurs from W = 5 rom and may be
due to a modification of the fibre/matrix interface which
results in a better contact between these two phases. The
tensile stress is then enhanced while the sliding of the fi-
bres is lowered,
- at higher temperatures the flexural strength increases li-
nearly with the specimen depth, that is the material becomes
less sensitive to defects. That behavior is the consequence
of two oxidation effects : first the carbonaceous interphase
is distroyed and the friction becomes more important i the
second effect is the embrittlement of the fibres. Thus the
entire material behaves brittle. Fig. 6 illustrates this em-
brittlement from 700·C to 1000·C.

Fracture resistance parameters

Like for the monotonic loading curves, the behavior of
the loading-unloading curves is unchanged up to 700·C. Beyond
this temperature, the breaks at the top of the reloading
loops clearly show occurrence of local ruptures in the speci-
men we associate to a premature breakage of the fibres (Fig.
7(b)). The residual displacement observed are very small, the
pull-out lengths shorten with the increase of the test tempe-
rature. The corollary of these observations is that the crack
growth increment (~an) calculated using equation (1) underes-

_. ..., .-. .-..-

o
.
.---- ......... -" o

300 ••
-
---..-· --
--;;
¢ --
150
o uoc
"00
0100
0'000
.1200

2.5 5 9.5
W(mm) _

Fig. 5. Flexural strength of sic-sic materials as a function

of specimen depth and test temperatures in air.

116
 t SIC-SIC
70.9.5.9.5 mm3
T= 700'C

o 50 100 h(~m)"""

Fig. 6. Three points bending monotonic loading curves of siC-

sic materials tested in air : a) non linearity before
maximum load at 700·C ; b) total linearity at lOOO·C.

timates the matrix crack length for test temperature T ~

700·C. We propose an empirical correction term (an) to take
into account the bridging zone size. This value an is expres-
sed as a function of the remaining ligament (W - an)' the
local reloading compliance value (C n ) and the compliance
value (C~) calculated assuming a linear elastic behaviour
(no crack bridging) :

a
SiC-SiC(1.21
D 1.3
25°C

400

300

200

100

o 0.1 0.2
h(mm)

Fig. 7. Superposition of monotonic loading curves (a) and

change in the energy parameters obtained as a func-
tion of ao/W (50xlOx4.25 mm3 ) (b).

117
 b
SiC-SiC

800·C

50

o 0.1

Fig. 7. Superposition of monotonic loading curves (a) and

change in the energy parameters obtained as a func-
tion of a o /W (50xlOx4. 25 mm3 ) (b).

W - an _ 1 Cn - Cn - 1
2 Cn

c·n - Cn
(2)
c·n

The total crack length is then an = an + an (Fig. 8) and

the associated resistance to crack propagation is termed R.
Fig. 9 shows the variations of J s ' Rand R with the test tem-
perature. The main features are the important differences
between Rand R in the range T ~ 700·C (the bridging effect
is appreciable), whereas a common value is observed for R, R
and J s beyond 800·C (the effects of the wake is reduced).

III!

Fig. 8. Modelling of the crack length.

118
 t ~---------- SiC,SiC (1,Z)
N I
E \ 8./w:O,5
~ \ • Js
Ia::. -, oR
a::
\ oR
••••••."'l, \
.. , ....
5
.\
/ '.\
0'- •• ' '.\

2.5 ·.b 0.5

.\
q,
"~

'~-----
- --0

o ZOO 400 600 800

Fig. 9. Change in Js ' R, R as a function of temperature.

Electron microscopy observations

Scanning electron microscopy

Scanning electron microscope observations of the surfa-
ces of rupture of unnotched specimens show a large extent of
fibre pull-out (length > 100 ~m) from the bundles normal to
the crack plane (Fig. lOa and lOb), whereas the fibres in the
other direction debond from the matrix. On the debonded
lengths, the fibres surface is free of any matrix, but the
embedded part is strongly bonded to the matrix. The surfaces
of rupture are covered with debris of the sic matrix (Fig.
lOc) .
At higher temperatures (beyond 800·C) the crack propaga-
tion in a straight line means that the fibre/matrix interface
is stronger. The absence of non-linearity on the loading cur-
ves corroborates the idea that the interphase grows hard and
is no more favorable to fibres sliding. This results in less
important total deformation and residual displacements. No
crack mouth bridging is observed and scanning electron mi-
croscope images show brittle rupture of the fibres (Fig.
lOd). Only few debris of the sic matrix are observed on the
surfaces of rupture. As a consequence of the intimate adhe~
sion of the matrix to the fibres, when pUll-out occurs,
lengths are very short.

Transmission electron microscopy

TEM observations confirm the fibres are amorphous while
the matrix reveal columnar crystals (of mean size 50 nm) due
to the CVI process. Magnified views show the transition from
the matrix to the carbon interphase and the ones from the in-
terphase to the fibre are very distinct and there is a per-
fect cohesion of the interphase to the fibres and to the
matrix. The carbon layer is not destroyed at 700·C (Fig.
lla). From 700°C to l300·C there is no clear change in the
contact between the fibres and the interphase, although we

119
Fig. 10. Surfaces of rupture of siC-siC specimens tested at
700·C (a, b, c) and 1000·C (d).

have observed modifications in the mechanical parameters. But

at 900·C the transition from the matrix to the carbon layer
is less distinct than at lower temperatures.
At 1300·C, it clearly appears decohesions between the
fibres and the interphase (Fig. 11b). The reason of these de-
cohesions are two fold : (i) the original carbonaceous inter-
phase is oxidized at high temperature in air i (ii) the dif-
ference in thermal expansion coefficients between the fibres
and the interphase. The decohesions lengths are about 0.30 ~m
and the initial layered structure of the pyrocarbon interpha-
se is now riddled with discontinuities like "holes" (~ 25 to
50 nm). Other observations after ageing at high temperature
in air or in inert atmosphere, coupled to microprobe analysis
and spectroscopy teChniques are reported in the literature
(Lamicq and al., 1986 i Jamet, 1983 i Frety and Boussuge,
1990). Generally it is admitted that the oxidation of the
fibre/matrix interface is due to the migration of oxygen
along the Nicalon SiC fibre, even when carbon interphase is
present. Hence the coatings deposited on these materials for
use at high temperatures are again outside sources of oxygen.

CONCLUSION

The effects of the exposure of uncoated sic-sic speci-

mens to high temperature in air have been investigated. It
has been shown that the pyrocarbon interphase deposited on

120
 a ,
Maltll'

b
---- ..-..--
~
~

Fig. 11. Specimens annealed at high temperature: (a) : 700°C:

intact interphase: (b) : 1300°C : debonding cracks
between fibres and transformed interphase with
"bubles".

the fibres before the CVI process of the matrix is at the

origin of the hight resistance to crack propagation observed
up to 700°C. Beyond this temperature, the structural modifi-
cations of this pyrocarbon layer leads to a quite total em-
brittlement of the materials.

ACKNOWLEDGEMENTS

Part of this work has been supported by E.E.C. BRITE

Programm, Project P-1348-6-85, contract nORI 1B-0098. The au-
thors wish to thank MM. Bourgeon, Cavalier, Chataignier and
Jouin for delivery of the samples and helpfull suggestions.

REFERENCES

Bernhardt, G., Lamicq, P., and Mace, J., Fiabilite des compo-
sites ceramiques-ceramiques. Ind. Ceram. 1/85 [790] : 51
(1995) _

121
Fareed, A.S., Fang, P., Koczak, M.J., and Ko, F.M.,"Thermome-
chanical properties of sic yarn". Am. Ceram.Soc. Bull;
66 [2] 353 (1987).
Frety N., Boussuge, M., "Relationship between the high tempe-
rature evolution of different fibre-matrix interfaces
and the mechanical behavior of Sic-sic composites".
Compo Sci., Tech., 37, 177 (1990).
Gault, C., Huger, M., "Caracterisation ultrasonore a haute
temperature des evolutions microstructurales de composi-
tes fibreux ceramique-ceramique. Influence de l'atmos-
phere", in "Materiaux Composites pour applications a
hautes temperatures". Proceedigns by AMAC/CODEMAC, March
29-30 1990, R. Naslain, J. Lamalle and J.L. Zulian,
eds., AMAC, Paris, p 303 (1990).
Gomina, M., Chermant, J.L., and Coster, M., "Radial distribu-
tion of the fibres in composite materials", Acta Ste-
reol., 2 Suppl : 179 (1983).
Guigon, M., "Microstructure de fibres de carbure de silicium.
Etude par microscopie electronique a transmission", Rev.
Phys. Appl. 23 : 229 (1988).
Jamet, J., "Les composites a matrice fragile, leur mecanique
de la rupture, leur elaboration via les organometalli-
ques", Techn. Rep. 7/3448 M (1983).
Lamicq, P., Bernhardt, G.A., "Energy principle of elastic-
plastic fracture and its application to the fracture me-
chanims of a polycrystalline graphite",Amer. Ceram. Soc.
Bull., 64 : 298 (1985).
Lamicq, P., Bernhardt, G., Dauchier, M., Mace, J., "sic-sic
composite ceramics", Amer. Ceram. Soc. Bull., 6S [2] :
336 (1986).
Sakai, M., Urashima, K., and Inagaki, M., "Energy principle
of elastic-plastic fracture and its application to the
fracture mechanims of a polycrystalline graphite", ~
Amer. Ceram. Soc., 66 : 868 (1983).
Tada, H., Paris, P.C., and Irwin, G.R., "The stress analysis
of crack handbook", Del. Research corp., Hellertown, PA
(1973).

122
FRACTURE TOUGHNESS OF CARBON FIBER
REINFORCED CERAMIC COMPOSITES

K. Nakano and A. Kamiya

Government Industrial Research Institute, Nagoya
Hirate-cho, Kita-ku, Nagoya, Japan
S. Yamauchi and T. Kobayashi
Toyohashi University of Technology
Tempaku-cho, Toyohashi-city, Japan

ABSTRACT
Continuously aligned carbon fiber reinforced SiC, SbN..-Sialon and
Si3N.. matrices composites have been fabricated by using slurry
impregnation process, followed by hot pressing. The dynamic
elastic-plastic fracture toughness CJd) as well as the dynamic stress
intensity factor CKd) of the composites were evaluated by the computer
aided Charpy impact testing system at room temperature. The Jd of the
composi tes were evaluated to be 10.48, 3.60 and 1.96 kJ/m2 corresponding to
the SiC, SbN..-Sialon and Si3N.. matrices, respectively.

INTRODUCTION

Ceramics have excellent characteristics for use in high temperature

structural materials and mechanical parts because of their heat-stability
superior strength at high temperatures. However, they are brittle as
monolithic state. The major concern in utilizing ceramics as structural
materials is improving toughness.

Continuous fiber reinforcement has recently been considered as a

hopeful method for toughening ceramics 1 ....... 3>. Several processes have been
carried out for the fabrication of continuos fiber reinforced ceramic
matrix composites CCFC)"-...O) .

The fracture toughness is one of the most important properties which

characterize the ceramic matrix composite. The method of evaluating the
CFC has not been established yet7). In this paper, the dynamic fracture
toughness of continuous carbon fiber reinforced SiC, Si3N..-Sialon, and
Si3N.. matrices composites were evaluated by using the instrumented Charpy
impact testing method which is easily able to estimate the fracture
toughness of the CFC.

Fracture Mechanics a/Ceramics, Vol. 9

Edited by R.C. Bradt et al., Plenum Press, New York, 1992 123
EXPERIMENTAL PROCEDURES
Fabrica tion of composi tes
Three kinds of composites were adopted in the present experiment:
1) carbon fiber/SiC matrix (C/SiC), 2) C/SbN4-Sialon (3 : 7 by weighD, 3)
C/Si3N4. A high modulus pitch carbon fiber (PETOCA HM50 : 10 JJ.m¢ :
crystalline graphite phase) was used as reinforcement, whereas fine
powders of ,B-SiCCO.3 JJ.m), a-SbN4 00.6 m2 /g) and a-Sialon (containing 6.8 %
of Y : 1.25 m2 /g) were used as fillers. Organosilicon resins such as a
polysilastyrene (in the case of SiC matrix: Nihon Soda PSS400 : average
molecular weight, 8000 ....... 12000), and a polysilazane (in the cases of
SbN4-Sialon and Si3N4 matrices: Chisso NCP201 : average molecular weight,
1310>, and a toluene were used as elements of slurries.

The unidirectional carbon fiber reinforced ceramic composites were

fabricated in the following process: 1) The slurry consisting of the
filler, the organosilicon resin and the toluene was impregnated into
interstices of carbon yarn by the filament-winding method in order to make
a prepreg, 2) The prepregs were stacked and pressed to make a
unidirectional fiber aligned body, 3) The body was heated for the
pyrolyzation of the organosilicon resin, and then hot pressed (the fiber
fraction of the composi tes were ....... 0.35).

Procedure for the evaluation of the fracture toughness

The specimen having rectangular bar form (4 X 8 X 35 mm 3 : each side
face was polished with #400 diamond wheel) was made from the composite
(fiber axis coincided wi th longi tudinal direction of the specimen). The
specimen had a slit CO.2 mm wid th and the half length of the specimen
width) in its central part.
Fracture toughness of the specimen was evaluated by the Computer
Aided Instrumented Charpy Impact Testing System (CADS> (energy capacity
of the system: 14.7J; impact velocity of the hammer was 0.95 m/sec; span
length 30 mm ) at room temperature. The block diagram of the CAl is shown
in Fig. 1. The Et (total absorbed energy), Ei (apparent crack initiation
energy) and Ep (apparent crack propagation energy) were directly
measured from the CAl system (Fig.2).

Deflection AMP
Pot~ntiOlMt~

Load AMP

Digital storag~
osci Iloscop~

Fig.1 Block diagram of the computer aided instrumented

Charpy impact testing system.

124
 The total absorbed energy Et may be analyzed and described as
following equation.

Et=Ei +Ep

Et : total absorbed energy

Ei : apparent crack initiation energy

(the energy absorbed up to the maximum load point m)

Ep : apparent crack propagation energy

(the energy absorbed after point m)

Since the crack initiation point was not well-defined in the

specimens of present experiment, a point where the sudden changing of
compliance was adopted as real crack start pointS> (p in Fig.2). Then the
following equation can be obtained in the parameters between Et, Eo' (true
crack initiation energy) and Ep' (true crack propagation energy).

m : Maximum load point

m p : Compliance changing point

y : Yield point

Et Total absorbed energy

Ei Apparent crack initiation t'nergy

Ep Apparent crack propagation energy

Eo' True crelck initiation energy

Ep' True crcl.ck propagation energy
Deflection
Fig.2 Schematic illustration of parameters obtained
from the CAl system

Et=Eo' +Ep' (2)

Eo' : true crack initiation energy

(the energy absorbed up to the point p)
Ep' : true crack propagation energy
(the energy absorbed after point p)

Similar to the case of equation (1), Et, Eo' and Ep' can be directly
obtained from CAl system, and the total absorbed energy Et is therefore
given by the equation (2).

125
 The dynamic fracture toughness Jdi and Jdo' were calculated from
g
the Rice's equation ) (3), (4») , assuming that the composite specimens
show elastic-plastic behavior.

Jdi = 2Ei/B(W-a) (3)

Jdo' =2Eo' IB(W-a) (4)

Jdi, Jdo' : nominal and true dynamic fracture toughness

B : thickness of the specimen

W: wid th of the specimen

a: length of slit

In the case of the plane strain condition, the dynamic stress

intensity factor (Kd) can be converted by the well-known equation:

(5)

Kd : dynamic stress intensity factor

Jd : dynamic fracture toughness
Y : Young's modulus
1/ : Poisson's ratio

From the equation (5), the dynamic stress intensity factor was
evaluated with the parameters such as the dynamic fracture toughness (Jd),
the Young's modulus and the Poisson's ratio.

3. RESULTS AND DISCUSSION

Typical load-deflection curves recorded by the CAl system are shown

in Fig.3. The values of Ei, Ep, Eo', Ep' and Et obtained from the CAl are
listed in Table 1 (open porosity and bulk density of the samples are also
listed in the Table). Each value is an average of 3 tested specimens. It is
evident that the total absorbed energy (Et) and the apparent and true
crack initiation energy mi, Eo') of the sample CISie were much higher than
those of the other two samples (Fig.3, Table D.

126
 50.0
elSie
40.0

30.0

20.0

10.0

0 1.0 2.0
50.0
el<si3N4 -Sialon)
40.0

-
~

~
01 30.0

u 20.0
0
0
...J
10.0

0 1.0 2.0
50.0

40.0

30.0

20.0

10.0

0 1.0 2.0
Deflection (mm)
Fig.3 Typical load-deflection curves of composite specimens.

127
 Table 1 Absorbed energy of the samples obtained by the CAl system

Ei Ep Eo' Ep' Et Open Bulk

sample porositc;. denSi\J;;
( J ) ( J ) ( J ) ( J ) ( J ) %) g/cc)

C/SiC 0.0724 0.2592 0.0534 0.2782 0.3316 4.7 2.38

C/(SisN4
-Sialon) 0.0249 0.0990 0.0196 0.1043 0.1239 23.4 1.90
C/SisN4 0.0136 0.0352 0.0105 0.0383 0.0488 0.4 3.03

The (crack ini tia tion energy)/( to tal absorbed energy) ratios are
listed in Table 2. The ratios Ei/Et and Eo'/Et of the sample C/SiC were
nearly the same as those of the sample C/(SisN4-Sialon) and lower than
those of the sample C/SisN4. This indicates that in the case of C/SisN4
sample the fraction of the crack initiation energy in the total absorbed
energy is higher than those of the other two kinds of samples
(Consequently, the fraction of the crack propagation energy in the total
absorbed energy is lower than those of the samples C/SiC and
C/SisN4-Sialon)).

Table 2 The (crack initiation energy)/(total

absorbed energy) ratios (%)

sample Ei/Et Ep/Et Eo'/Et Ep'/Et

C/SiC 22 78 16 84
C/(SisN4-Sialon) 20 80 16 84
C/SisN4 29 71 23 77

Values of the dynamic elastic-plastic fracture toughness calculated

from the equation (3) and (4) are shown in Table 3, which have similar trend
to the case of Ei and Eo' values. Because of large notch radius of slit
front ( f =0.1 mm) in the specimens, these values would be over estimated
to some extent 10l. Strict evaluation should be carried out under the
condi tion of f =0.

Table 3 Dynamic fracture toughness of the samples

sample JdHkJ/m2 ) Jdo'(kJ/m 2 ) Jdo' I JdH%)

C/Sie 10.48±0.56 7.72 ±0.06 73.7

C/(SisN4-sialon) 3.60±0.41 2.83 ±0.24 78.6
C/SisN4 1.96±0.30 1.52±0.19 77.6

128
 Values of the dynamic stress intensity factor (Kd) evaluated from
the equation (5) are shown in Table 4. Two kinds of the dynamic stress
intensity factors Kd(m) and Kd(p) were evaluated based on Jdi and Jdo'
respectively, since no crack extension can be maintained up to the point p
(the sudden changing point of compliance) in each load-deflection curveS)
(Fig.3). For the evaluations of the Kd, the Young's modulus of the samples
were directly measured according to the (JlS R1602) 1 IJ method and are
listed in the Table 4. In the evaluation of the Kd, the following Poisson's
ratios were adopted. instead of real ones because of the lack of direct
measurement: for the C/SiC, 11 =0.17 (hot pressed SiC (99 % theoretical
density» 12); for the C/(SiaN4-Sialon), 11 =0.16 (reaction sintered Si3N4 (74%
Ld.»l31; for the C/Si3N4, 11=0.21 (hot pressed Si3N4 (95% Ld.»'41.

The values of the Young's modulus of the C/SiC and C/Si3N4 samples
which listed in the Table 4 are about 30 and 60 % of the theoretical ones
(calculated from the rule of mixture), respectively. The former ratio is
far less than the latter one. This would closely related to the facts that
the open porosity of the C/SiC sample was higher than that of the C/Si3N4
sample (Table 1) and that the former sample had the lower value of the
Jdo'/Jdi than that of the latter one <Table 3), which means that in the case
of C/SiC sample the non-linear phenomena with microcracking in the
load-deflection curve easily occurs compared to the case of C/Si3N4
sample.

Table 4 Dynamic stress intensity factor and

Young's modulus of the samples

sample C/SiC C/(Si3N4-Sialon) C/SiaN4

Kd(m) 37.1 17.8 21.1
(MPavm)
Kd(p) 31.8 15.7 18.5
(MPavm)

Y(GPa) 127.5 85.3 215.7

Figure 4 shows fracture surfaces of specimens after the Charpy

impact testing. In the case of the SiC matrix, long pull-out fibers were
predominantly observed(a). Somewhat long pull-out fibers were also
observed in the SiaN4-Sialon matrix(b), whereas slight fiber pull-out were
detected in the SiaN4 matrix(c). The resul ts of the observation correspond
to the order of magnitude of the total absorbed energy (i.e. Et(SiC) >
EHSi3N4-Sialon) > EHSiaN4», the apparent and true crack initiation
energy, and the apparent and true crack propagation energy. This
suggests that the fiber pull-out has remarkable contribution to the
fracture energy of the sample.

129
w
o

CJ c
V
'11
'-
J
-
011

Vi

c
0
~
01
to
Q
0
'- C
Q 0
~;
v v
ttl CJ
1Uu'- '-

Fig.4 Fracture surfaces of specimens after the Charpy testing: a) SiC, b) SiaN4-Sialon, c) SiaN4 matrices
SUMMARY

1. The total absorbed energy and the crack initiation energy of the C/SiC
composite were much higher than those of the other two kinds of
composi tes.

2. The fractions of the crack initiation energy in the total absorbed

energy on the C/SiC composite were nearly the same as those of the
C/SbN4-Sialon and were lower than those of the C/Si3N4.

3. The dynamic fracture toughness as well as the dynamic stress intensity

factor of the C/SiC composites were much higher than those of the other
two kinds of composi tes.

4. Remarkable fiber pull-out was observed on the C/SiC composite sample

after the Charpy impact testing, whereas medium and slight fiber pull
out were observed on the samples corresponding to the C/Si3N4-Sialon
and C/SbN4 composites, respectively.

ACKNOWLEDGEMENT

The authors wish to thank Mr. Toshiya OGAWA for the help of the
experimental work.

REFERENCES

1. Y. Kagawa, Seisan-Kenkyu, 42: (8)31(1990),

2. A. G. Evans, The mechanical behavior of ceramic composites, in : "The

Modeling of Material Behavior and Its Relation to Design" J. D. Embury
and A. W. Thompson, ed., TMS, (1990) P.245.

3. W. C. Carter, E. P. Butler and E. R. Fuller, Jr., Scripta METALLURGICA et

MATERIALIA, 25:579(1991).

4. E. Fitzer and R. Gadow, Am. Cer. Soc. Bull., 65:(2)326<1986),

5. H. Hannache, J. M. Quenisset and R. Naslain, J. Mater. ScL, 19:202(1984).

6. K. Nakano et al., Carbon Fiber Reinforced Silicon Carbide Composites,

in: "Developments in the Science and Technology of Composite
Materials" J. FUller et al. ed., Elsevier Appl. Sci. (1990)P.419.

7. D. B. Marshall and A. G. Evans, J. Am. Cer. Soc., 68:(5)225<1985).

8. T. Kobayashi and M. Niinomi, Nuclear Eng. and Design, 111:27(1989),

9. J. R. Rice, P. C. Paris and J. G. Merkel, ASTM STP, 536:231(1973).

10. T. Kobayashi, K. Matsunuma, H. Ikawa and K. Motoyoshi, Eng. Frac.

Mech., 31:873(1988).

131
11. "Japanese Industrial Standard Testing Methods for Elastic Modulus of
High Performance Ceramics" , JIS R 1602 (established 1986).

12. "Engineering Property Data on Selected Ceramics" vo I 2, Carbides,

Metals and Ceramic Information Center Battel, Columbus Lab. (979)
P.5.2.3-10.

13. "Engineering Poperty Data on Selected Ceramics" vol 1, Nitrides,

Metals and Ceramic Information Center Battel, Columbus Lab. (976)
P.5.3.3-23.

14. ibid. P.5.3.3-9.

132
DYNAMIC FRACTURE RESPONSES OF Al203, Si3N4 AND SiCw/Al203

Yoshio Takagi* and Albert S. Kobayashi

University of Washington
Department of Mechanical Engineering
Seattle, Washington 98195, USA

ABSTRACT

A hybrid experimental-numerical procedure was used to characterize

the dynamic fracture responses of alumina (Al203), silicon nitride
(Si3N4) and silicon carbide whisker/alumina matrix (SiCw/Al203) com-
posite. The instantaneous crack tip location during rapid fracture at
room and 1000°C was determined by the crack opening displacement (COD),
using laser interferometric displacement gage. Consistent with
previous finding, the dynamic crack arrest stress intensity factor did
not exist in the ceramics and ceramic matrix composite studied.

INTRODUCTION

The projected use of ceramics and ceramic matrix composites in

heat engines will subject these components to severe loading condi-
tions, such as particulate impact at elevated temperature. While
recent literature is abundant with data on impact studies of monolith-
ic ceramics, similar research at elevated temperature is missing.
From the user's viewpoint, impact studies provide practical failure
data which relates directly to the functional capability of the cer-
amics and ceramic matrix composite components. These impact failures
are characterized by shattering which is a complex phenomenon involv-
ing microcrack generation, growth and coalescence into macro-cracks
which in turn grow, branch and coalesce.

A more generic analysis of impact failure is to study the dynamic

crack ~nitiation, propagation and arrest stress intensity factors,
yn
KId, KI and KIa, respectively as well as crack branching in these
brittle materials. While dynamic fracture mechanics has been the
subject of active research for the past two decades, it has been ex-
clusively confined to traditional metallic structure with polymers
used as a model material in basic research. Similar dynamic fracture
mechanics study of ceramics and ceramic matrix composites are

* On academic leave from NKK Corporation, Advanced Technology Research

Center, Kawasaki 210, Japan at the time of this research.

Fracture Mechanics of Ceramics. Vol. 9

Edited by R.C. Bradt et aI., Plenum Press. New York., 1992 133
virtually non-existent except for Reference I in addition to those of
the authors and their colleagues 2- 10

In the following, we report on the recent results generated

through our continuing study on this subject.

METHOD OF APPROACH

The hybrid experimental-numerical technique, which was developed

by Yang et al 7 for dynamic fracture characterization of high tempera-
ture ceramics and ceramic composites, was used in this analysis with
improved sensitivity. In the following a brief description of the
procedure is provided.

Material and Specimen

Materials for the fracture specimen consists of commercially

available alumina (AI203)*' silicon nitride (Si3N4)** and a alumina
matrix composite with 25% silicon carbide whisker (SiCw/AI203)***.
The fracture specimens, which are single edge notched three point bend
specimens, were machined to the dimensions shown in Figure 1. Three
point bend specimens were used because of their simplicity in geometry
and relative ease in alignment at elevated temperature. A shallow
chevron notch was machined as a starter crack for initiating a true
crack by the single-edge-precracked-beam (SEPB) method of Reference
11. These true crack were normally about 3-4 mm in depth.

Experimental Procedure

The loading system consisted of a drop weight tower, which is

mounted integrally with the furnace which in turn can operate at a
temperature up to l500°C. The door and two port holes, which are
shielded with fused silicate glass panes to prevent undesirable con-
vection current of air in the furnace chamber, provided access for the
input and output laser beams of the laser interferometric displacement
gage (LIDG)4,8. The mass of the steel impactor was 2.2 kg. The spec-
imens were rapidly loaded by the dropweight with an impact velocity of
0.7 m/sec. The impact load was monitored by a load transducer at the
top end of a push rod and outside of the furnace as shown schematical-
ly in Figure 2.

A pair of LIDG targets were placed at the crack mouth of the

specimen. The crack mouth opening displacement (CMOD) obtained from
the LIDG records was used to determine directly the crack tip location
in a rapidly fracturing three point bend specimen. The LIDG targets
were platinum tabs which were mounted directly on the specimen after
pre cracking and then indented by a Vickers microhardness tester to
minimize possible experimental error in locating the LIDG targets.

* AD-995 Coors Porcelain Company, Golden, Colorado 80401

** NKK Corporation, Kawasaki 210, Japan
*** A30SC Nippon Steel Corporation, Kawasaki 211, Japan.

134
 All Dimensions
Inmm

280~
Ol
co
cx:i
0.25 _olk--
6.3~ ~ 66.7

76.2

Figure 1. Precracked three-point bend specimen.

Gu1de Shaft
jtt'

Impact Body

Load
up Transducer

Furnace

Push Rod

IDG Port L1DG Port

BendIng
FIxture

Figure 2. Drop-weight impact tester and furnace with LIDG ports.

A series of static tests were also conducted at room temperature

in order to obtain dynamic fracture data at low crack velocity. This
data was necessary to highlight the significant differences between
the dynamic fracture rea?onses of metals and brittle ceramics and
ceramic composites at KI n substantially lower than the static frac-
ture toughness, KIC.

135
Numerical Procedure

The crack tip location versus time history together with the load-
ing history were used to execute a dynamic finite element code in its
generation mode in order to compute the dynamicdinitiation and the
yn
propagation stress intensity factors, KId and KI , respectively,
associated with the propagating crack. Details of this hybrid experi-
mental-numerical procedure as well as its validation are given in
References 7 and 8.

TOP LOAD TRACE

t 500 N
CMOD L1DG LEFT

t
ONSET OF
CRACK PROPAGATION
CMOD L1DG RIGHT ~
20llS

Figure 3. Loading and CMOD Histories at lOOO°C. SiCw/Al203 Specimen.

RESULTS

The above mentioned pr~cedure was used to generate the dynamic

yn
stress intensity factor, KI , versus crack velocity relations for
A1203, Si3N4 and SiCw/Al203 composite at room temperature and lOOO°C.
Figure 3 shows a pair of typical LIDG data together with the loading
history obtained for the SiCw/Al203 specimen tested at lOOO°C. Figure
4 shows the resultant crack extension history obtained by this LIDG
data at the crack mouth. Figure 5 shows the CMOD and the crack exten-
sion histories for the Si3N4 specimens tested at room temperature.

As mentioned previously, the crack extension and load· histories

were then used to compute the dynam~c initiation and propagation
yn
stress intensity factors, KId and KI , respectively, the results of
which are reported in the following.

136
 2 10

Crack Extension
CMOD
S 8
E ~
c
0 6
""toC
'mCo :...
QI
1
:::,
X
UJ 0
..II: 4 0
u U
...
ell
U
2

o Jot,.;",.------'-'-----L------'----~O

o 5 10
Time (!!S)
Figure 4. CMOD and crack extension histories at lOOO°C. SiCw/A1203
specimen.

2 10

Crack Extension ./

6 1.5 CMOD ./
./
./
18
./ I
E ./
./
./
:il
c;
C ./ 6 to
c
,9 ./
rJl ./ '<:
cQI 1
./
./ :::,
X ./
./
4 0
UJ
..II: ./
./ 0
U
...
U ./
~t;
./
U 0.5 ./

./
./
2
./
./
./
./
0 0
0 5 10 15 20
Time (s)
Figure 5. COD and crack extension histories at room temperature.
Si3N4 specimen.

137
 500
o Impact Loading (RT.)
400 • Impact Loading OOOO°C)

.,
<il
.......
E <tb
0 300 <b
'g O.~
dJ
> 200
,.,.;
• g 0
u
C!
U
100
KId

0
~
0 2 4 6 8
Dynamic Stress Intensity Factor (MPavrn)

Figure 6. Dynamic SIF versus crack velocity relation of A1203.

Table 1. Comparison of fracture toughnesses

Alumina Silicon SiCw/ A1 203

Fracture Nitride Composite
Ref. Toughness Temp. Temp. Temp.
(MFa ..jffi) Room 1000° Room 1000 0 C Room 1000°
C C
This study KId 4.9 4.4 9.9 - 5.6 5.9
KIC - - 9.0 - 6.0 -

Yang and KId 5.7 5.1 - - 7.9 6.9

Kobayashi KIC 4.3 - - - 6.6 -
(1990)
Duffy et KId 5.6 - - - - -
al. (1988) KIC 3.4 - - - - -

138
Dynamic Fracture Initiation Toughness, KId

Since the initial cracks generated by the SEPB method is a true

crack, the dynamic initiation stress intensity factor, KId, obtained
in this study should be less than those reported previously8-l0.
Table 1 shows a tabulated comparison of these KId where KId in this
study is slightly higher than those of Reference 10, but is within the
expected scatter band of ± 10%. The high KId and KIC for Si3N4 are
attributed to acicular Si3N4, which acts as whiskers in the crystal-
line Si3N4 matrix.

300,-------------------------,
o Impact Loading + Static Loading

250
o Impact Loading

~ 200
-5
.....>,
'g ]50 0
0 0
Q) 0

~
> 0 0
u 00 0
~ 100 0
U
0 0
+
50 + + +
+
KIC KId

o ~ J;
o 2 4 6 8 10 12 ]4
S tress Intensity Factor (M Pa.Jm)
Figure 7. Stress intensity factor versus crack velocity of Si3N4
at room temperature.

dyn
Dynamic Stress Intensity Factor, K and Arrest
I

d Figures 6, 7 and 8 show the dynamic stress intensity factor (SIF),

yn
KI versus crack velocity relations for A1203, Si3N4 and SiCw/Al203
composite, respectively. Data points for the lower dynamic stress
intensity factors and lower crack velocities were obtained through
statically loaded specimens. These results show an unambigu-ous lack
of dynamic crack arrest stress intensity factor below which dynamic
crack propagation will cease. The crack velocities for im-pacted
specimens in this study were on the average about four times of that
of Reference 10 for identical alumina fracture specimens. It was
about twenty percent higher for the different SiC w/A1203 specimens
used in this study.

Figures 7 and 8 show thJ,t the crack can propagate at a larger

yn
crack veaocit y under high KI . Therefore no unique crack velocity
yn
versus KI can be observed in these materials.

139
 300 . . . - - - - - - - - - - - - - - - - - - - - - - - - - - - - ,
0 Impact Loading (RT.)
t.
0 Impact Loading (RI.) t. t.
250
t. Impact Loading (RT.) 0
• •
• Impact Loading (1000~)
~ 200
E • Impact Loading (lOOO'C) 0
•
....
>, + Static Loading (R.T.) CD
t. • Ot.
'g 150 0 0 0

•
X Static Loading (R.T.)
Q)
:>
\
X Static Loading (R.T.)
~
u 0
U
~ 100
•
50 +
X X Xx X+ X +
KId KIC +
o ~ J;.......,..J, ....
o 1 234 567 8 9 10
Stress Intensity Factor (M Pa"Jffij
Figure 8. Stress intensity factor versus crack velocity of
SiCw/AI Z0 3.

CONCLUSIONS

The hybrid experimental-numerical procedure was used to determine

the crack velocity versus dynamic stress intensity factor relations in
A1203, Si3N4 and SiCw/AIZ03 composite at room temperature and 1000°C.
The results, which are in qualitative agreement with References 2-10,
again showed conclusively the lack of a dynamic crack arrest intensity
factor and of a unique crack velocity versus dynamic stress intensity
factor relation.

DISCUSSIONS

The fracture surfaces were scanned by SEM and the relative areas
of transgranular failures of the silicon nitride grains and the alumi-
na grains in the statically loaded and impact loaded Si3N4 and
SiCw/AIZ03 composite were compared.

Figures 9 and 10 show typical fracture surfaces of a dynamically

and a statically loaded Si3N4 and SiCw/AIZ03 specimens at room temp-
erature. Transgranular fracture dominated the fracture in the stati-
cally loaded specimen while the dynamically loaded specimen is
characterized by the predominant intergranular fracture.

140
 Statically

Impact Loaded Specimen

Figure 9. Fracture Surfaces of Si3N4 Specimens tested at room

temperature.

141
 Impact Loaded

Figure 10. Fracture surfaces of SiCw!A1203 specimens tested at

room temperature.

142
 70
0 Static loading
~
~
;:l
60 • Dynamic Loading •
ti

••
tU
tt
1-0
tU 50
'3s::
tU 0
bh 0
a 40
(/)

1-0
!-<

30 L..,....--'---'---'--I-"'""'-~ ........."'--.L-.'---'---'----'---l.--"--'-.............J..-...J

o 2 4 6 8
Stress Intensity Factor (M Pavrn)
Figure 11. Percentage area of transgranu1ar fracture versus stress
intensity factor. Sicw/A1203 specimens.

70 , . . - - - - - - - - - - - - - - - - - - - - - - ,
0 Static loading

• Dynamic Loading •

••
0
0

30L..J.,..., .-...J.- ~ ~

o 50 100 150 200

Crack Velocity (m/s)
Figure 12. Percentage area of transgranu1ar fracture versus crack
velocity. SiCw/A1203 specimens.

Figure 11 shows the percentage area of transgranular fracture

versus dynamic SIF relation for SiC w/Al203 specimens. The percentage
area of transgranular fracture is in excess of 45% at the lowest SIF
of about 1 MPa~. These results are consistent with those of Figure 8
thus suggesting a correlation between the percentage area of trans-
granular fracture and the crack velocity which is shown in Figure 12.
The percentage area of transgranular fracture increases almost linear-
ly with the crack velocity in this figure. The percentage area of

143
transgranular is more than 40% even with the low crack velocity of 40
m/s. The kinematic constraint of a rapidly propagating crack probably
enforces transgranular fracture which in turn enables the crack to
propagate at a subcritical dynamic SIF. The lack of crack arrest of
the propagating crack in this study was thus attributed to the large
percentage area of transgranular failures in contrast to that of the
arrested pre crack tip region discussed previously10,14.

ACKNOWLEDGEMENT

This research was supported by Office of Naval Research Contract

No. N00014-87- K-0326. The authors wish to thank Drs. Yapa Rajapakse
and Steve Fishman, ONR for their patience and support. The authors
are specially indebted to Mr. Tetsuo Nose, Nippon Steel Corporation
for providing the SEPB fixture and the SiCw/A1203 specimens for this
study and to NKK Corporation for providing the Si3N4 specimens.

REFERENCES

1. S. T. Gonczy and D. L. Johnson, "Impact Fracture of Ceramics at High

Temperatures," Fracture Mechanics of Ceramics, vol. 3,
R.C.Bradt, D.P.H. Hasselman and F.F. Lange, eds., Plenum
Press, 495 (1978).
2. A.S. Kobayashi, A.F. Emery and B.M. Liaw, "Dynamic Toughness of
Glass," Fracture Mechanics of Ceramics, Vol. 6 eds R.C.
Bradt, A.G. Evans, D.P.H. Hasselman and F.F. Lange, eds.,
Plenum Press, 47 (1983).
3. A.S. Kobayashi and K.-H. Yang, "A Hybrid Technique for High-
Temperature Dynamic Fracture Analysis," Applications of Ad-
vanced Measurement Techniques, Brit. Soc for Strain
Measurements, Whittles Pub., Caithess, U.K., 109 (1988).
4. A.S. Kobayashi, K.-H. Yang and A.F. Emery, "Dynamic Fracture Test-
ing of Alumina," Impact Loading and Dynamic Behavior of
Materials, C.Y. Chiem, H.-D. Kunze and L.W. Meyer, eds. DGB
Informationsgesellschaft mgH, 113 (1988).
6. B.M. Liaw, A.S. Kobayashi and A.F. Emery, "Effect of Loading Rates
on Dynamic Fracture of Reaction Bonded Silicon Nitride,"
Fracture Mechanics: Seventh Volume ASTM STP 905, 95 (1986).
7. Kwan-Ho Yang and Albert S. Kobayashi, "An Experimental-Numerical
Procedure for High Temperature Dynamic Fracture Analysis,"
Computational Mechanics '88, ed. S.N. Atluri and G. Yagawa,
eds., Springer-Velag, 48v.1(1988).
8. K.-H. Yang, A.S. Kobayashi and A.F.Emery, "Dynamic Fracture
Characterization of Ceramic Matrix Composites," Journal de
Physique. ColloQue C3, supplement au No.9, C3-223 (1988).
9. K.-H. Yang, A.S. Kobayashi and A.F. Emery, "Effects of Loading
Rates and Temperature on Dynamic Fracture of Ceramics and
Ceramic Matrix Composites," Ceramic Materials and Components
for Engines, V.J. Tennery and M.K. Ferber, eds., American
Ceramic Society, 766 (1989).
10. K.-H. Yang and A.S. Kobayashi, 1990, "Dynamic Fracture Response of
Alumina and Two Ceramic Composites," J. of Amer. Ceramic
~ , 73 (8): 2309 (1990).

144
11. T. Nose and T. Fujii, "Evaluation of Fracture Toughness for
Ceramic Materials by a Single-Edge-Precracked-Beam Method,"
J. of the Amer. Ceramic Soc., V. 71(6): 328 (1988).
12. J. Duffy, S. Suresh, K. Cho and E.R. Bopp, "A Method for Dynamic
Fracture Initiation Testing of Ceramics,H J. of Eng.
Materials and Techn. , V 110 (4), 325 (1988).
13. C.-T. Yu, and A.S. Kobayashi, "Fracture Process Zone in Ceramics
and Ceramic Composites,H to be published in Proc. of 6th
Int'l Conf. on Mechanical Behavior of Materials, Kyoto, Japan
(July 1991) .
14. W.-J. Yang, C.-T. Yu and A.S. Kobayashi, "SEM Quantification of
Trans- versus Inter-granular Fracture,H J. of Amer. Ceramic
SQQ....., 74 (2): 290 (1991).

145
FRACTIJRE TOUGHENING MECHANISMS
IN THE SiCw/A1203 COMPOSITE SYSTEM

Laurent Guazzone and Kenneth W. White

College of Engineering
University of Houston
Houston, TX, USA 77204-4792

ABSTRACT

Crack growth resistance studies of a SiC whisker reinforced A1203 matrix composite
have been correlated with the composite microstructure to determine the active fracture
toughening mechanism, at each of three test temperatures through 1400°C. Evidence of
cumulative toughening at all temperatures, as reported in the literature, was validated by R-
curves, however, isolation of the following wake zone effects from that of the frontal process
zone elicit a departure from published assumptions. A frontal zone mechanism, presumably
microcrack toughening, dominates at room temperature, while a following wake zone
mechanism of crack face whisker-bridging controls at temperatures near 12()()OC. Fracture
data obtained from composites with substantially increased whisker/matrix interphase
demonstrates the influence of the interphase thickness, where microcracking and pullout are
both suppressed at room temperature, while pullout at reduced loads persists at elevated
temperatures.

INTRODUCTION

Recent fracture mechanism studies of the SiC whisker reinforced / Alumina matrix
system have attributed the marked improvement in KIC over that of monolithic alumina to
crack deflection 1-6, reinforcement bridging in the following wake zone 2-5,7,8 and
microcrack development I. From these, crack face bridging emerges as the most widely

Fracture Mechanics of Ceramics, Vol. 9

Edited by R.C. Bradt et aI., Plenum Press, New York, 1992 147
accepted. Elevated temperature studies of similar composites 9,10,11 have demonstrated a
consistent element of damage tolerance throughout the temperature range of 20°C -l400°C, as
indicated by rising R-curve behavior. The significance of crack face tractions was cited in
these studies, as well.

The strong dependence of KIC upon whisker orientation 1suggests a significant

interaction between the crack front and the whisker aspect ratio and orientation. Pullout
lengths have been compared with computed crack opening displacements, to geometrically
validate the bridging mechanism as an explanation for the rise of both the arrest and initiation
stress intensity factors with increasing crack length 7. Elevated temperature tests have shown
little influence upon KIC, however, R-curve behavior was observed to dramatically increase
above lOOO°C 9,10,12. These considerations, along with direct observations of various
lengths of pulled-out whiskers has prompted a strong support for whisker bridging in the
following wake zone as a predominant toughening mechanism 13,14,15,

Crack deflection has also been advanced as a viable explanation for the significant
fracture toughness improvement reported over that of monolithic alumina. Following the
early analytical treatments of the problem 16-18, the experimentally observed influence of
crack orientation by the whiskers has prompted several considerations of crack deflection as a
toughening component in this composite 1-3,5,11, Observations of KIC improvements over
monolithic alumina, even with the crack running in the whisker plane 1, provide convincing
evidence of the importance of this mechanism to the performance of brittle matrix
composites. However, despite a strong case for its contribution toward fracture toughness,
crack deflection cannot explain the cumulative component indicated by the observed R-curve
behavior.

Although both interfacial and transgranular microcracking has been shown to

influence both initiation and crack growth resistance 16,17, only mention of a possible
cumulative contribution to this composite exists in the literature 1. Accordingly, crack
bridging, alone, has been advanced to explain the R-curve dependency upon whisker
additions. The early observations of strong improvements in both KIC and dR/Ma, with
additions of SiC whiskers to monolithic A1203, support suggestions of multiple operative
mechanisms 2. The present paper considers the various components of the toughening, and
relates them to the microstructure and the test temperature.

EXPERIMENTAL METIIODS

Materials and Specimens

The SiC whisker reinforced AIz03 matrix composite was obtained in the form of hot
pressed disks£. These rice hull-derived whiskers typically measure about O.751lm in

£ SA-Z5; Advanced Composite Materials, Greer, SC

148
diameter, by about 20 11m in length. The whiskers are predominantly ~-SiC, of the 3C
polytype, with <111> aligned with the whisker axis.

This composite was supplied in two fonns, differing only in the whisker/matrix
interphase chemistry. The nonnal processing for this material includes a whisker cleaning
step, which involves both thennal and chemical treatments. The data obtained from this
materials is designated type Z. A type N material has been processed identically except for
the omission of this cleaning step, leaving carbon residues at the interface.

All single edge notched beam (SENB) specimens were machined to maintain cross
sectional dimensions, W=B,.,8mm and span, S=60mm. Both chevron-notched and straight-
notched configurations of this specimen were used, the details of which have been previously
reported 19. Analysis of the whisker orientation within the hot pressed disks indicates a very
strong preferred whisker orientation within the plane nonnal to the hot pressing direction.
Accordingly, all specimen notches are orientated nonnal to the plane of the whiskers and
extend in a direction through the disk thickness, so as to cross the whisker planes nonnal to
whiskers. Notch depths were O.44W for the chevron-notch and 0.47W for the straight-notch
configurations, and re-notching was perfonned at a crack length of a/W=O.80±0.02.

Equipment

Fracture testing was accomplished on a screw-driven universal load frame§ with a

total measured system compliance of 0.03 11m /kg and a load capacity of 100 kN. Loading
fixtures were machined from a-SiC bar and tube stock. All fracture tests were loaded at a
rate of 0.005 mrn/min. The elevated temperature environment was obtained from a vertical
clam-shell type fumace¥ , mounted to the load frame.

Data Analysis

The stress intensity factor, K, is computed from the load, P, the specimen width, B,
and thickness, W, and the geometry correction factor, Y, which requires knowledge of the
instantaneous crack length. This effective crack length is obtained using the compliance
method, already described elsewhere 19,20. Instantaneous stress intensity factors, Kr, are
evaluated according to the following convention 20,21:

KI=[B~JY (1)

For the special case of P = PMAX and the appropriate value of Y applied, as detailed
elsewhere 19, this relationship will yield the critical stress intensity factor, KIC. KR-curves
are constructed from subsequent stress intensity factors, starting with KIC

§ Model 4505: Instron Corp.. Canton. MA.

¥ Deltech Co., Denver, CO.

149
RESULTS AND DISCUSSION

Fracture Mechanisms for Standard Composite - Txpe Z Composite

The load and displacement information, representative of at least three tests each, at
temperatures of 20°C, 1200°C and 1400°C are shown in Figure 1. Although the exact
magnitude of the loads depend upon the specific specimen geometries, the variances of these
dimensions are small compared with the load differences between these three curves.
Subcritical crack extension is observed in each case, corresponding to crack growth from the
tip of the chevron notch to the critical conditions for instability at !>MAx. In all cases,
continued crack extension beyond maximum load remains stable, permitting the
determination of valid R-curves for each of the three test temperatures.

This unreduced data shows that the highest loads are supported by those specimens
tested at 1200°C. The 1200°C data not only supports higher loads, incurring a higher stored
elastic strain energy to drive the crack, but also shows an improved crack growth stability,
indicated by the rate of load drop following PMAX. The room temperature performance, as
treated by a majority of the literature, falls intermediate to the two elevated temperature
results.

With no fracture mechanics assumptions, the character of these curves provide a

direct indication of the crack growth resistance behavior. The slopes of the load-
displacement relationships, which correspond to the compliance changes with crack
extension, indicate a steady improvement in the ability of the material to support a larger load
at an advanced crack length. This improved tolerance to damage is expected to yield

120
SiC(w)/Alumina
Chevron-Notched SE B
100

80

~ 60
'0
os
0
...:l
40

20

00 20 40 60 80 100 120 140 160 180 200

Displacement (11m)

Figure 1. Load-Displacement Curves for SiCw/A1203 at 20°C to 1400°C

(Type Z).

150
optimum R-cmve behavior at higher temperatures. Additionally, the larger value of PMAX at
1200oe, followed by a decrease at 14000 e will be reflected in the levels of the R-cmves
which follow.

The KR-curves generated from the above data and shown in Figure 2, indicate a
strong cumulative toughening mechanism present at all temperatures. The tendency for run-
arrest behavior apparent in the room temperature results, has been reported earlier for a
similar composite 7. At 1200o e, initiation at a higher stress intensity factor shifts the curve
above the room temperature data where it rises smoothly, and at an increasing rate with crack
extension. This behavior is even more pronounced at 1400oe, although initiating from an

14
SiC(w)/Alumina
13 Chevron-Notch SENB
12
11
..-. 10
E!
7
'"
Q.,
::!:
9
8
'-'
=.: 7
~
6

5
4

2
0.6 0.7 0.8 0.9 1.0

a1W

Figure 2. KR-cmves: 20 0 e to 14000 e (Type Z).

initial stress intensity factor that is well below that of the room temperature behavior. This
consistent accumulation of damage resistance, indicated at all temperatures by the similar
values of dKRfMa, proves the existence of some cumulative toughening mechanism with the
progress of the fracture process zone. Additionally, since the value of dKR/Ma changes little
with temperature, the intensity of this total effect also is expected to remain constant with test
temperature. Although, fiber bridging in the following wake zone has been suggested as the
likely mechanism 2,7, these data do not specifically isolate the location of the developing
damage.

The re-notching experiments, reported earlier for monolithic alumina 19,22, may be
adapted to the present concern, as a means of isolating the toughening contribution of the
frontal process zone from that of the following wake region. This will provide a more direct

151
 120
20"C
Chevron-Notched SENB
100

80 A
Initial
loading
~ (,()
'0
co
0
..J
After
40 renotching

20

0
0 10 20 30 40 50 (,()

Displacement (l1m)

Figure 3. Re-Notch Load Displacement Behavior: 20°C (Type Z).

indication of the specific toughening mechanism which is operational under each test
environment. The re-notch load-displacement records, characteristic of each test
temperature environment, are shown in Figures 3 through 5. The initial loading segment of
each test closely resembles that of the monotonic fracture test, however, following a
predetennined extension of the crack (A to B), the fracture event was interrupted for the
mechanical removal of the wake zone following the primary crack tip (point C). Continued
testing of the re-notched sample generates the second segment (C-D-E), which is shown
superimposed onto the initial test for each of the three cases. Consistent with the previous

120
1200°C
Chevron-Notched SENB
100

80

g (,()
...
'0
0
..J
40

20
After
renotching

ob---L.o...o-.l......-...l.~........~.....&..._..................10..0._......-~......---.1
o 20 40 (,() 80 100 120 140 I(,() 180 200

Displacement (Ilm)

Figure 4. Re-Noteh Load Displacement Behavior: 1200°C (Type Z).

152
 120
1400°C
Chevron-Nolched SE B
100

80

Initial
~ loading
-= 60

j'"
40 After
renotching
20

20 40 60 80 100 120 140 160 180 200

Displacement (11m)

Figure 5. Re-Noteh Load-displacement: 1400°C (Type Z).

treatment of the problem 19, the load drops between points B and 0, in each case, represent
the load supported by the following wake zone which was removed by re-notching.

The three pairs of fracture tests represented by Figures 3 through 5, are reduced to
terms of stress intensity factor, thereby removing specimen geometry influence. In each of
these, presented together in Figure 6, the initial segment shows a rise with the development
of a process zone, followed by a stress intensity factor drop, AKR, prior to continuation of
the fracture test. The magnitude of this effect will be used as an indicator of the
"effectiveness" of the following wake region.

14
13
12OO"C
12
,-.. 11

~
S
(>
C': 10
Q.,

6 9

/
8 2O"C
l:l:
~ 7
6 -------."
~ ~
5 1400"C

4
3
2
0.6 0.7 0.8 0.9 1.0
a/W

Figure 6. Re-Notch KR-Curves: 20°C, 1200°C, and 1400°C (Type Z)

153
 As expected, each of these curves agree very well with the monotonic fracture test
results shown in Figure 2, with similar initial stress intensity factors and about the same total
rise over comparable crack extensions. ~KR is very small for the room temperature test and
rises to a maximum at 1200°C. At higher temperatures, the softening of the intergranular
glass phase appears to diminish the wake zone effectiveness, however, to a level that still far
exceeds that observed at room temperature.

To further evaluate the effectiveness of the wake zone, a comparison between the critical
stress intensity factors determined from both straight-notch and chevron-notch SENB
specimen configurations has been included. Although crack growth instability precluded R-
curve determination from the straight-notch configuration, the KIC values represent critical
crack instability criteria initiated from the root of a machined notch. This quantity will be
compared with the chevron-notch critical stress intensities, which have previously been
characterized as a sharp crack phenomenon, following a fmite quantity of subcritical crack
extension 7,9,10,19. The evaluation of "KIC" following the development of a following wake
zone, accounts for the characteristically higher critical stress intensity factors obtained from
chevron-notch tests for rising R-curve materials 10.

The relatively consistent area defmed by the triangular crack face region between the
chevron tip and the critical crack front location, provides a predictable following wake zone
which modifies the crack tip stresses at critical conditions. The chevron-notch critical stress
intensity factor has been shown to approach that of the straight-notch configuration, upon
renotching at an advanced crack length 19. Therefore, the difference between the critical
stress intensity factors determined from these two specimen configurations provides an
alternate measure of the following wake zone "effectiveness", under distinctly different crack
tip conditions from that of the re-notch experiments discussed above.

The average chevron-notch "KIC" values, which include the initial KR-curve entries from
Figure 2 as well as the remainder of the test results, constitute the upper curve of Figure 7.
The maximum chevron-notch toughness obtained at 1200°C is contrasted with the results of
the straight-notch specimen, where the behavior is virtually unchanged, or perhaps drops
slightly though 1200°C, followed by a decrease to less than half of the room temperature
toughness. The difference between the critical stress intensity factors determined from these
two notch types provides an additional wake zone effectiveness parameter, denoted here as
~"KIC". The nearly identical room temperature critical stress intensity factors are followed

by a maximum departure at 1200°C. At yet higher temperatures, through 1400°C, an

intermediate value is maintained, well in excess of the room temperature quantity.

This data confirms the re-notch results, in that the following wake zone provides a
maximum influence upon the fracture event at temperatures near 1200°C. At room
temperature, very little effect can be attributed to the following wake region. Very high test

154
 10 r----------------------,
9

E 7

!
~ 6
5[--------0--...
Straight-Notch

1
(SENB)
ot......~.......L~~....L....~.........IL.....-_-..L. _ _..&..._.........I'___~.....LI
o 200 400 600 800 1000 1200 1400
Temperature (OC)

Figure 7. Fracture Toughness vs. Test Temperature: Chevron-

Notch and Straight-Notch SENB Specimens. ([ype Z)

10ilm

Figure 8. SEM Fractograph of Type Z SiCw/AI203: 20°C

155
 10 11m

Figure 9. SEM Fractograph of Type Z SiCw/AI203: 1200°C

temperatures diminish the critical stress intensity factors, consistent with the drop in load
capacity denoted in Figure 1.

Microstructural Analysis

Figures 8 and 9 are representative scanning electron microscopy (SEM) images of the slow
crack growth region of the fracture face, for two of the test temperatures. Since the fracture
mode of the A120:3 grains and the whisker pullout length are of primary importance to the
present fracture mechanism analysis, only the 2000X images are included here. An increase
in long range surface roughness with test temperature, apparent at lower magnifications,
indicates a higher level of crack interaction with the microstructure. This topography is
similar to that reported earlier, and is consistent with the increased crack growth resistance
observed at large crack extensions and at the high temperatures 10.

The propensity for transgranular fracture of the A120:3 at room temperature, especially
at these relatively small grain sizes, suggests an influence from the presence of the whiskers
in the A1203 matrix. For monolithic A120:3, fractographic studies have indicated that
transgranular fracture is predominantly confined to those grains larger than about 20
11m19,23, far in excess of those found in the present composite matrix. This implies that the
small following wake zone toughening contribution possible from the 2-5 11m matrix grains,
is likely to vanish for the present composite, as negligible crack face bridging can be expected
from grains which have fractured in the crack plane.

156
 Whisker pullout lengths for all three test conditions are readily apparent at these
magnifications, averaging less than one micrometer at 20°C (range: O-ll1m), about I whisker
diameter; 2.4 11m (range: 2-5I1m), or about 5 whisker diameters, at 1200°C, to as much as 8
11m at 1400°C (range: 4-8I1m). The whisker pullout mechanism, therefore, is expected to
impose an increasing impact at higher test temperatures. Becher, et al. 2 report room
temperature pullout lengths for similar SiCw/A1203 composites to be about one whisker
diameter, or 0.4 11m for their case; while Jenkins, et al. 7 find about 311m, about 2 whisker
diameters. Recognizing the large dependance of the intergranular glass phase chemistry on
this topographic feature, which undoubtedly varies between fabrication processes, the
present findings agree very well with these reported values. Also of interest is the factor of
ten variation of pullout length, from less than one whisker diameter to as much as ten,
observed within the same composite subjected to different test environments. Contrary to
earlier suggestions 13, the same fiber provides a vastly different pullout toughening
contribution, with no apparent dependence upon its length unless matrix conditions favor
pullout.

Fracture Mechanisms

The existence of the rising R-curve, demonstrated in Figure 2, confirms the operation
of a cumulative toughening mechanism with crack extension. The measured toughness,
represented by the general stress intensity factor, K, is composed of two primary elements of
significance here 13:

(2)

The initiation stress intensity, Kj, relates to the resistance to crack extension from a
flaw. In the absence of a formal definition of this flaw, this quantity is taken here as the
point of instability, represented by the first point of the R-curve. The sharp initiating flaw of
the chevron-notch specimen provokes an influence from both the following wake region and
the frontal process zone on the stress intensity factor. By comparison, the critical flaw
associated with the straight-notch specimen is a virtually traction-free machined notch.
provided subcritical crack growth is absent or neglected. Therefore, different toughening
mechanisms may be contributing the the value of Kj for the two notch configurations studied.
The value of M<:IC, defined above as KIC(C-N) - KIC(S-N), approximates only the wake
component of Kj(C-N).

The change in stress intensity with crack extension, .1K, will depend upon only the
cumulative mechanisms available from the microstructure. This will necessarily include both
the frontal and following wake process zone components. Therefore, for flat R-curve
materials, where no cumulative mechanisms exist, this quantity will vanish. The present
material exhibits a strong value of .1K, as typified by the rising KR-curves shown in Figure
2. The quantity .1KR isolates the following wake component of M<: for analysis.

157
 These two indicators of the following wake effectiveness are plotted in Figure 10,
along with the average length of whisker pullout, measured directly from the fractographs for
each test temperature. Although these fracture-derived parameters arise from different
locations on the R-curve and are based upon different notch geometries, coordinating them
with the fractographic data semi-quantitatively confmns the thesis of the foregoing
arguments. That is, the very small following wake contribution at room temperature
corresponds with very small pullout lengths, and rises to a maximum at 1200°C,
accompanied by a strong improvement in pullout length. Despite the continued improvement
in pullout length, the wake effectiveness diminishes at still higher temperatures, but remains
significantly more important than at room temperature.

6 5
,-..,
e
=l
5
4
'-'
£OIl ,-..,
r:: 4 e
~ 3~
'5
oS 3 ~
'-'
"3
c.. 2~
«) 2
...~
«)
> 1
~

L-.-""'"--.......- - - ' - - - - ' - -......- " " ' " - -....... o

200 400 600 800 1000 1200 1400

Temperature (OC)

Figure 10. Comparison of the Type Z Microstructural Results With

the Wake Zone Indicators.

The pullout component is explained from the linear increase in frictional interfacial
shear stress, 'tf, as the temperature deviates below the processing temperature, AT, and may
be estimated as 'tf = fl cr(AT). Below about ll00°C, the coefficient of friction, fl, is
approximated as a constant, and only the normal interfacial stress, cr(AT) is influenced by
temperature 11. This behavior would restrict whisker pullout at the lower temperatures. As
the temperature approaches ll00°C, the diminishing AT term will permit easier pullout
without fiber failure. Since the coefficient of thermal expansion of the AIz03 exceeds that of
the SiC whiskers, the residual stresses imposed by the cr(AT) term would promote
microcracking at the lower temperatures (large An I4 . Above this temperature range,
softening of the intergranular glass phase will introduce a non-linearity to the coefficient of

158
 I5.4llm

Figure 11. Scanning Acoustic Microscope image of microcrack at

Illm below the surface of the Type Z SiCw/A1203: From 20°C
sample; central spot is longitudinal view of whisker, microcrack
radially oriented with respect to the whisker.

friction, lowering Il exponentially with temperature 24. Therefore, at the highest test
temperature the interfacial shear stress reduces precipitously, promoting massive whisker
pullout with little resistance, and therefore little whisker breakage.

For the present non-transforming material, the two candidate cumulative toughening
mechanisms are bridging in the following wake region and microcracking in the frontal
process zone. Since the value of AI< increases only slightly with temperature, the total
contribution from each must vary proportionally with temperature. The absence of wake
zone toughening at low temperatures suggests frontal zone microcracking as the primary
contributor to the room temperature t1K component. The large fraction of transgranular
fracture may support this hypothesis, as fracture-induced microcracks may promote cleavage.

Microcrack Analysis

Although, the above fracture data falls short of directly identifying the existence of
matrix microcracking, scanning acoustic microscopy (SAM) studies have unambiguously
identified microcracks within the subsurface layer adjacent to the fracture surfaces.
Microcracks such as those shown in Figure 11, were found only in the fracture specimens

159
tested at room temperature. Consistent with the thermoelastic stress arguments 14,15,25, no
such cracks were found in those specimens tested at the higher temperatures.

Details of this SAM work will appear in a later publication, so only a descriptive
treatment is included here. The microcracks found in these samples were always associated
with SiC whiskers, and the rnicrocrack plane always contained the whisker. As shown in
Figure 11, the microcracks typically formed in pairs, growing radially from the whisker.
The thumbnail shape of the crack front could be determined by defocusing to as much as 4
!!m below the surface, causing the apparent crack length to increase from end to center of the
whisker.

Interfacial Phase Effects - Type N Composite

Figure 12 provides a representative comparison between the two composite

compositions. The type N composite, which contains an interphase, supports larger initial
loads, however, at the expense of some of the stability characteristic of the type Z
composition, repeated here for comparison from Figure 1. Although specimen dimensions
varied slightly between these two materials, the representation of crack stability provides an
accurate characterization of the behavioral differences.

120
20°C

100

80
~
'0 60
C':
0
..J
4l)

20

Di placement (fJ.m)

Figure 12. Load-Displacement Curves at 20°C for Type N and Type Z

SiCw/ AI20:3

160
, 61
 8 -r----------------------,
iC(w)/Alumina
Chevron-Nolched SE B
7

2+-..........T""'T'"""T"""<~T""'T'"'T"""~T""T'" .........."""T"""............................."T'"""T..................._t

0.6 0.7 0.8 0.9

a/W

Figure 15. KR-Curves at 1400°C for Type N and Type Z SiCw/A1203

Reduction of this room temperature data provides the type N KR-curve, compared in
Figure 13 with that of the type Z, taken from Figure 2. The dramatic loss of the rising
component (M<:) with the intervention of the interphase suggests the suppression of the
microcracking component of the toughening contribution. The whisker bridging component
remains to provide a small rise over the crack lengths studied, as the pullout length observed
for this composite was found to differ little from that of the type Z, shown in Figure 8.

The elevated temperature results are shown in Figures 14 and 15. In this temperature range,
where whisker pullout has been shown above to dominate, the fractographic results, again,
indicate very similar appearance to that of the type Z material. The interfacial fIlm, therefore,
appears to alter the propensity for whisker bridging, but limits the pullout stress. The
lubrication expected from the softening interfacial glass phase may provide this mechanism,
where the lower glass content of the type Z composite continues to support significantly
higher loads throughout the test temperature range.

CONCLUSIONS

Data has been presented to identify the fracture toughening mechanisms active in this
SiCw/A1203 composite. Cumulative toughening mechanisms dominate throughout the test
temperature range of 20°C through 1400°C, however, the active mechanism changes from a
predominantly frontal zone type at low temperatures, to one operative only in the following
wake zone at 1200°C. Above this temperature, the behavior of the softening glass phase
dominates the fracture properties. The influence of thicker interfacial films, adjacent to the
whiskers, has been shown to suppress the microcracking component at low temperatures
and reduce the loads supported by the bridging whiskers at elevated temperatures.

162
REFERENCES

1. Becher, P.P., and Wei, G.C., "Toughening Behavior In SiC-Whisker-Reinforced

Alumina," Cornrn. 1. Am. Ceram. Soc., 61[12], pp.C267-9 (1984).
2. Becher, P.F., Tiegs, T.N., Ogle, 1.C., and Warwick, W.H., "Toughening of Ceramics
By Whisker Reinforcement," in : Fracture Mechanics of Ceramics, Bradt,RC., et.
al. eds., 1, pp.61-73 (1986).
3. Homeny, 1., Vaughn, W. L., Ferber, M.K., "Processing and Mechanical Properties of
SiC-Whisker-AI203-Matrix Composites," Am. Ceram. Soc. Bull., Q1(2], pp.333-
38 (1987).
4. Homeny, 1., Vaughn, W. L., Ferber, M.K., "Silicon Carbide Whisker/Alumina Matrix
Composites: Effect of Whisker Surface Treatment on Fracture Toughness," J. Am.
Ceram. Soc., 1J.[2], pp.394-402 (1990).
5. Chakraborty, A, Bhaduri, S.B., Reddy, lJ., Mohan Rao, R., and Mahajan, YR.,
"Toughening Mechanisms in A~03-SiCw Composites," ICF7 Proceedings,
Salama, K., Ravi-Chandar, K., Taplin, D.M.R, Rama Rao, P., eds., 1, pp.2905-
11, Houston, U.S.A., March 20-24 (1989).
6. Faber, K.T., Evans, AG. "Crack Deflection Processes: I.Theory," Acta Metal!. 31[4],
pp.565-76 (1983).
7. Jenkins, M.G., Kobayashi, A.S., White, K.W., and Bradt, RC., "Crack Initiation
And Arrest in a SiC Whisker/~O] Matrix Composite," 1. Am. Ceram. Soc.,
1ill6],pp.393-5 (1987).
8. Homeny, J., Vaughn, "R-curve Behavior in a Silicon Carbide Whisker/Alumina Matix
Composites," J. Am. Ceram. Soc., 73[7], pp.2060-62 (1990).
9. Jenkins, M.G., Kobayashi, A.S., White, K.W., Bradt, R.C., "Elevated Temperature
Fracture Resistance of a SiC Whisker Reinforced/Polycrystalline A~03 Matrix
Composite," Eng. Frac. Mech. .N[4], pp.505-15 (1988).
10. Ghosh, A.,White, K.W., Jenkins, M.G., Kobayashi., A.S. and Bradt, RC.,"The R-
curve Behavior of a SiC Whisker/Polycrystalline Alumina Matrix Composite to
1400°C," ORNL/ASM SiC Whiskers Symposium Proceedings, June, 1988.
11. Shaw, N.C., Faber, K.T.,"Temperature-dependent Toughening in Whisker-Reinforced
Ceramics," Materials Science Research, 21, 929-38, in: Ceramic Microstructures
'86, Role of Interfaces, Pask, Evans, eds., Plenum Press, NY (1986).
12. Angelini, P., Mader, W., and Becher, "Strain and Fracture in Whisker Reinforced
Ceramics"; pp. 241-57 in Materials Research Society Symposia Proceedings, Vol.
78, Advanced Structural Ceramics, Ed. P.F. Becher, M.V. Swain, and S. Somiya.
Materials Research Society, Pittsburgh, PA, 1986.
13. Becher, P.P., Hsueh, C-H., Angelini, P., Tiegs,T.N., "Toughening Behavior in
Whisker-Reinforced Ceramic Matrix Composites," 1. Am. Ceram. Soc., 21[12],
pp.1050-61 (1988).
14. Wei, G.C., and Becher, P.F., "Development of SiC Whisker-Reinforced Ceramics,"
Am. Ceram. Soc. Bull., M [2], pp.298-304 (1985).
15. Majumdar, S., Kupperman, D., "Effect of Temperature and Whisker Volume Fraction
on Average Residual Thermal Strains in a SiC/A~03 Composite," J. Am. Ceram.
Soc., 72[2], pp.312-3 (1989).
16. Evans, AG., and Faber, K.T., "Toughening of Ceramics by Circumferential
Microcracking," J. Am. Ceram. Soc., 64[7], pp.394-8 (1981).
17. Evans, A.G., and Faber, K.T., "Crack-Growth Resistance of Microcracking Brittle
,Materials", J. Amer. Ceram. Soc. 67 [4] 225-260, (1984).
18. Faber, K.T., Evans, A.G., and Drory, M.D., "A Statistical Analysis of Crack
Deflection As a Toughening Mechanism in Ceramic Materials," Frac. Mech. of
Ceramics, Bradt, R.C., et. al. eds. v. 6, pp. 77-91 (1983).
19. Grimes, RE., Kelkar, G.P., Guazzone, L.and White, K.W., "Elevated Temperature R-
curve Behavior of a Polycrystalline Alumina," J. of Am. Ceram. Soc.,n[5],
pp.1399-404 (1990).
20. Jenkins, M.G., Kobayashi, A.S., White, K.W., and Bradt, RC., "A 3-D Finite
Element Analysis of the Chevron-notch, Three-Point Bend Fracture Specimen,"
Int'!. J. of Fract.,~, pp.281-95 (1987).
21. Bluhm, J.I., "Slice Synthesis of a Three Dimensional Work of Fracture," Eng. Frac.
Mech.7 [3] 593-604 (1975).

163
22. Knehans, R., and Steinbrech, R. "Memory Effect of Crack Resistance During Slow
Crack Growth in Notched A~a3 Bend Specimens," 1. Mat. Sci. Lett.,1[8],
pp.327-9 (1982).
23. Virkar, A.V., Gordon, R. L. "Fracture Properties of Polycrystalline Lithia-Stabilized
W' -Alumina," 1. of Am. Ceram. Soc.,60[l-2], pp.59-61 (1977).
24. Wyatt, a.H., and Dew-Hughes, D., Metals. Ceramics. and Polymers, Cambridge,
p.259, (1974).
25. Hsueh, C-H., Becher, P.P. & Angelini, P., "Effects of Interfacial Films on Thermal
Stresses in Whisker-Reinforced Ceramics," 1. Am. Ceram. Soc., 11[11], pp.929-
33 (1988).

164
MICROSTRUCTURES AND FRACTURE BEHAVIORS AT HIGH TEMPERATURES FOR

A120a-SiC NANOCOMPOSITES

Atsushi Nakahira and Koichi Niihara

The Institute of Scientific and Industrial Research

Osaka University, 8-1, Mihogaoka, Ibaraki, Osaka 567
Japan

ABSTRACT

Effects of nano-size SiC dispersions on the microstructures and mechan-

ical properties have been investigated for A1203 nanocomposites. These
A1203 nanocomposites were prepared by hot-pressing the mixtures of fine
A1203 and SiC powders. Transmission electron microscopic observations
indicated the fine SiC particulate less than O.2tJ.m were uniformly
dispersed predominantly wi thin A1203 matrix grains. The significant
increase of mechanical properties were achieved for A1203/SiC nanocom-
posites, comparable to Si3N4 and SiC. In special, the fracture
strength of A1203 was approximately 3 times increased by the SiC dis-
persions. Another interesting finding is that the high temperature
mechanical properties were effectively improved by dispersing the
second phase on nanometer. The rolls of the nanometer-size second
phase on the microstructure and fracture behaviors at high temperatures
will be discussed.

INTRODUCTION

A1203 is one of the most popular ceramics in the various engineer-

ing fields, because of its excellent physical and chemical properties
[1]. However, the use of A1203 ceramics in structural applications has
been limited by the relatively low fracture toughness and strength, low
reliabili ty, and rapid degradation of mechanical properties at high
temperatures[2]. Therefore, the incorporations of particulates (such
as, TiC, SiC and Zr02) and SiC whisker have been frequently attempted
to toughen and strengthen A1203 ceramics[3-5]. The dispersion of Zr02
particulate and SiC whisker, in special, were shown to be very effec-
tive for the improvement of mechanical properties of A1203[6]. Howev-
er, the transformation toughening mechanism diminishes as the tempera-
ture increase and in the moist atmosphere even at ambient
temperature[7,8]. The whisker reinforcement are not attractive because
of the high cost and much difficulties in fabrication processes. On
the other hand, the particulate reinforcement (oxide, carbide and
boride so on) are economically more advantageous as the simple process-
ing for mass production[9,10].

Fracture Mechanics o/Ceramics, Vol. 9

Edited by R.C. Bradt et aI., Plenum Press, New York, 1992 165
 Recently, there has been great interest in the development of
ceramic-based nanocomposites[11,12]. In special, the considerable
efforts have been made to develop the ultrafine (usually nanometer
size) ceramic mixed-powder through the chemical synthesis by many
investigations[13-15]. On the other hand, Niihara and his
colleagues[16-19] reported previously that A1203-based, MgO-based and
Si3N4-based nanocomposites were successfully fabricated by hot-pressing
the mixture of fine ceramic powders through the conventional powder
metallurgical technique. It was shown that these particulate-rein-
forced ceramic nanocomposites exhibited the excellent mechanical
properties, for instance, high fracture strength and toughness and high
reliability so on.
These nanocomposites are new kind of composites, as compared with
the usual ceramics composites, microcomposite, in which the micronmeter
size particles are dispersed at the grain boundaries of matrix. The
toughening and reinforcement mechanisms in these nanocomposites,
however, are not well understood because of lacking the sufficient
experimental data on the distribution of the second phase, the inter-
face between intragranular particle and matrix grain, and residual
stress effects. Therefore, more detailed know ledges of microstructures
are required for these ceramics nanocomposites.
Another important aspect is the understanding of fracture process
for these ceramics-based nanocomposites. For the high temperature
structural applications, the inhibition of high-temperature deformation
under various stress (creep) and high-temperature slow crack growth
(SCG) are indispensable [20] . Therefore, it is very important to
identify the difference of high-temperature fracture behaviors between
these ceramic nanocomposites and monolithic A1203, including some Al203
microcomposites, in order to tailor the new ceramic composites.
The main purpose of this work is to assess the microstructures of
A1203/SiC nanocomposites to evaluate their mechanical properties and to
clarify the high-temperature fracture and deformation behaviors of
these nanocomposites. Finally, the roles of the nanometer-size disper-
sions within matrix grains on the microstructure and mechanical proper-
ties will be also discussed for these A1203-SiC nanocomposites.

EXPERIMENTAL PROCEDURES

1. Fabrications

A1203 and SiC powders were selected as starting materials for the
matrix and reinforcing dispersions, respectively. A1203 powder was 'Y-
phase with the average particle size below 0.4 /.l. m from Asahi Chemical
Co. . SiC powder was .e
-phase with average particle below 0.3 /.l. m from
Ibiden Co .. The A1203/ 5-33vol%SiC powder were ball-milled with Al203
ball in ethanol for 12hr. These mixtures were hot-pressed in carbon
dies lined with graphite foil at pressure of 28MPa and temperature of
1600 to 1800 °c for Ih in N2 atmosphere. The hot-pressed specimens
were ground by the diamond wheel. The mechanical properties measure-
ments were made on bars cut from the ground specimens.

2. Characterizations

The phase compositions of the hot-pressed specimens were investi-

gated by X-ray diffraction. The density of these specimens was ob-
tained by Archimedes method in toluene. The microstructures of pol-
ished samples were observed by optical microscopy and scanning electron
microscopy. The more detailed microstructures were observed by the

166
transmission electron microscopy. The specimens were cut and ground to
150,um by the diamond wheel. These thin foils were dimpled. After the
dimpling procedures, the specimens were then ion-milled at 3kV with Ar
ion. The observations were performed using the JEOL 200CX.
The grain sizes were estimated on the thermal etched surfaces for
monoli thic A1203 and A1203/SiC nanocomposi tes by the line intercept
method [21] . The fracture or igins and fractography of ruptured speci-
mens were observed by scanning electron microscopy. Also, the interac-
tion of cracks with dispersed phase was examined on the indented sur-
face using scanning electron microscopy.

3.Mechanical properties

The hardness of these Al203/SiC nanocomposites was measured by

Vickers diamond indenter with applied load of 9. 8N. The fracture
strength was measured by three-point bending test. The bars were
approximately 3.0 by 4.0 by 36mm in size, where the span was 30mm. The
tensile faces were polished to below 1,um finish and the tensile edges
were beveled to eliminate edge flaws. The specimens were tested at a
cross head speed of 0.5mm/min. At least five samples were used for
each hot-pressed specimens. The fracture toughness was evaluated on
the same specimens using the indentation fracture technique[22] , for
which the specimens were polished to below 1,um by diamond paste.
High-temperature mechanical properties for these Al203/SiC nano-
composites and monolithic Al203 were measured by the hot-hardness test.
The hot-hardness test is simple and convenient for characterization of
fracture and deformation behavior at high temperatures and the hot-
hardness behaviors closely parallel the deformation and creep charac-
teristics for various materials as shown by Westbrook et al[23, 24].
However, the experimental difficulties are considerable to measure the
deformation and creep behaviors by the conventional technique, tensile
and bending creep[25]. Therefore, in this work the deformation, frac-
ture and creep behaviors were evaluated by the hot-hardness technique.
The deformation resistance at the high-temperature were evaluated by
the temperature dependence of hot-hardness ( short-time hot-hardness)
test and the loading time dependence of hot-hardness(hot-hardness creep
test) experiments[26]. The short-time hot-hardness was measured in
vacuum of 1x10- 5 to 5x10- 5 Torr using a Nikon high temperature micro-
hardness tester(QM type) for 15 sec at a lowering rate of O. 3mm/sec
with applied load of 4.9N up to 1400°C. Hot-hardness creep test was
performed at 1000, 1100, 1200, and 1300°C in vacuum using the same
tester. The loading time was changed from 1 to 400sec for hot-hardness
creep test. The deformation behaviors around indentation after creep
test were observed by optical microscopy, scanning electron microscopy,
and transmission electron microscopy.

RESULTS AND DISCUSSION

1. Microstructures

The results of X-ray diffraction analyses for A1203/SiC nanocom-

posi tes indicated that A1203/SiC nanocomposi tes were composed of only
a -Al2 03 and .B -SiC. Fig. 1 shows the typical transmission electron
micrograph of monolithic Al203 and Al203/17vol%SiC nanocomposite.
Monolithic Al203 was equi-axed grain with the average particle size of
2,um. The pores at grain boundaries and dislocations inside A1203
grain were scarcely observed. On the other hand, Al203/SiC nanocom-
posites indicated that SiC particles less than 200nm were predominantly

167
 Fig.! Typical transmission electron micrographs of monolithic
A1203(A) and A1203/17vol%SiC nanocomposite(B).

Fig.2 Typical high resolutional electron micrographs of A1203/SiC

nanocomposites.

168
dispersed wi thin the A120a matrix grains. These intragranular SiC
particles were uniformly dispersed wi thin Al20a grains and usually
contained the stacking faults. In addition, intragranular SiC parti-
cles were usually faceted but, in part, spherical within Al20a matrix
grains. Moreover, dislocations were sometimes observed around the
intragranular SiC particles wi thin A120a matrix grains for A120a/SiC
nanocomposites. From these observations, it was confirmed that the
AI20a/SiC nanocomposites were successfully prepared by the conventional
powder metallurgical technique.
Fig.2 shows the typical high resolutional electron micrographs of
these AI20a/SiC nanocomposites. Any reacting phases were not observed
at the interface between A120a and intragranular SiC wi thin the Al20a
grain for both faceted and spherical SiC particles. Similar faceted
interfaces were reported for A120a/Zr02 by Lanteri et al[27] and for
SiaN4/SiC by Suganuma et al[28]. They proposed that these faceted
particles implied the existence of low energy interfaces for their
composites. Therefore, the straight interface of Al20a/SiC are also
considered to be formed to lower the energy at interfaces for these
A120a /SiC nanocomposi tes. Furthermore, the Moires fringes were fre-
quently observed at the corner of intragranular SiC particles wi thin
Al20a matrix grains. This result revealed that the interface at the
corner SiC particles was semi-coherent or incoherent.

2. Density and grain size

Fig.3 shows the effects of hot-pressing temperature and SiC volume

content on the relative density of A120a/SiC nanocomposites. The
relati ve densities for these A120a /SiC nanocomposi tes were strongly
dependent on the SiC volume content. The fully dense(over 99% of
theoretical densities) specimens were hot-pressed at 1600·C for
AI20a/5vol%SiC, at 1700·C for AI20a/11vol%SiC and at 1800·C for
A120a/17-33vol%SiC nanocomposi tes. These results indicate that the
addition of SiC as the second phase inhibit the densification of Al20a
matrix for these A120a/SiC nanocomposites.
The etching studies indicated that these dense Al203/SiC nanocom-
posites hot-pressed at 1600-1800·C contained no residual porosity and
consisted of equi-axed Al20a grains and their average grain size ranged
from 1 to 15,um at hot-pressing temperatures of 1600-1800·C. The dense
AI20a/SiC nanocomposites prepared under each optimum hot-pressing
temperature were appeared to consist of a fine grain matrix with 1-
2,um. However, the hot-pressing over optimum fabrication temperature
for each Al20a/SiC nanocomposites resulted in the rapid growth of Al20a
matrix grains for each Al20a/SiC nanocomposites. In special, the
remarkable growth of A120a matrix were observed at A120a/5-11vol%SiC
nanocomposites. These results show that the pining effects of SiC

100 , • •
~ 98 • •
~
'iii 96
c
Q)
0 94
Q)
>
~ 92 e:16QQOC
Qi .. :1700°C
a: 90 .: 1800°C

88
0 10 20 30 40
SiC Content (vol%)

Fig.3 The effects of hot-pressing temperature and SiC volume content

on the relative density of Al203/SiC nanocomposites.

169
 particle on grain boundary during the densification process increased
with the volume fraction of SiC particles for these A120s/SiC nanocom-
posites, which are consistent with the dependence of second phase
fraction on the densification rate for many ceramics[29]. Neverthe-
less, it becomes evident that SiC particles apparently inhibited the
densification and grain growth of A120s for these A120s/SiC nanocompos-
ites.

26

<? 24
a..
~
en
en
Q)
22 {/
"E
c:
20 / ~
~
'"
I /
.:1600·C
18 ":1700'C
.: leOO'c
16
9
0 10 20 30 40
SiC Content (vol%)

Fig.4 The effects of hot-pressing temperature and SiC volume content

on the hardness for A120s/SiC nanocomposites.

3. Mechanical properties at room temperature

The hardness for these A120s/SiC nanocomposites at room tempera-

ture is shown in Fig.4. As apparent from this figure, the hardness
changed with the SiC content and hot-pressing temperatures. The hard-
ness for the fully dense A120s/SiC nanocomposites increased with the
content of SiC particles and were in good agreement with expectations
based on the linear mixed rules[30], as shown in Fig.4 by the solid
line. However, A120s/SiC nanocomposites, as shown by white marks in
Fig.4, indicated the lower hardness than values expected from linear
mixed rules due to the presence of residual porosities. Moreover, the
slight decrease in the hardness were observed for some A120s/Si~,nano­
composites prepared at higher hot-pressing temperatures. This decrease
in hardness were thought to be contributed to the coarse A120s matrix
grains. From these results, the hardness for A120s/SiC nanocomposites
were found to be strongly dependent on the SiC content, relative densi-
ty, and matrix grain size. Niihara et al[31] previously reported that
A120s/211mSiC microcomposites also showed the increase in hardness with
the content of 211m-SiC particles. A120s/SiC nanocomposites indicate
the slightly high hardness, compared with those of A12 Os /211 m-SiC
microcomposites. These high hardness may be accounted for the differ-
ence of microstructures between A120s/SiC micro and nanocomposites,

170
namely, the particle size of SiC and the location of SiC particles.
These results suggest that the dispersion of SiC particles within Al203
matrix grains are likely to inhibit the slip wi thin A1203 grains even
at room temperature.
Fig.5 shows the dependence of fracture toughness for A1203/SiC
nanocomposites with SiC content. The fracture toughness for A1203/SiC
nanocomposi tes increased with SiC additions as can be seen in figure.
The maximum fracture toughness of 4.7MPam 1 / 2 was achieved by the addi-
tion of only 5vol% SiC and kept almost constant value up to Ilvol% SiC
for these A1203/SiC nanocomposi tes. However, the fracture toughness
for A1203/11, 17vol%SiC nanocomposites slightly decreased. This de-
crease in fracture toughness was thought to be caused by the agglomera-
tion of SiC particles. Fig.6 shows the crack propagation around Vick-
ers indentation on polished surface for A1203 /5vol%SiC nanocomposites.
The crack was observed to propagate straightly with small deviation.

N 6
.:I600'C
-E .. :t700'C
ctl
a.. .: 1BOo-C
5 T
~
<I)
<I)
Q)
c 4
-<=
0>
:::J

f=.
3
:s
Q)

t3
~
u. 2
0 10 20 30 40
SiC Content (vol%)

Fig.5 The effects on hot-pressing temperature and SiC volume content

on the fracture toughness for A1203/SiC nanocomposites.

These deviation of crack were thought to be caused by the nanometer-

size SiC particles. These observations suggest that the operative
toughening mechanism is the crack deflection by SiC particles. As
reported previously[32], large residual stresses are generated by the
thermal expansion mismatch between Al203 and SiC during cooling down
from fabrication temperature to room temperature for A1203/SiC nanocom-
posites. The tangential and radial stress can be calculated to be
approximately 750MPa(tensile stress) and -1500MPa(compressive stress),
respectively, according to Selsing's equation[33]. This high tensile
stress will not induce the microcracking around SiC particles because
the particle size of SiC are much smaller than the critical particle
size for the spontaneous microcracking[34]. However, the microcrack-
ing toughening can not be ruled out because of the observed agglomera-
tion of SiC particles. Kobayashi et al[35] proposed the residual
stresses effect as toughening mechanism in particulate composite.
They reported that the advancing crack was attracted to the adjacent
particles due to the residual stresses and that their model was in
good agreement with the experiments for SiC/TiB2 composites. There-
fore, these residual stresses effect would also contribute to the

'71
 Fig.6 Scanning electron micrograph of crack propagation around Vick-
ers indentation on the polished surface for AI203/5vol%SiC nanocom
posite. The crack propagation was from the left.

observed toughening for these A1203/SiC nanocomposi tes. From these

results, it could be concluded that the main toughening mechanisms for
A1203/SiC nanocomposi tes are considered to be crack deflection by SiC
particles within Al203 matrix grains and residual stress effects.
The variation in fracture strength for A1203/SiC nanocomposites
with SiC content is shown in Fig.7. Fracture strength increase with
SiC content up to 11vol% and ranged from 350 to 1050 MPa. However, at
the larger volume fraction of SiC, the fracture strength a little
decreased and kept constant value of 850MPa. These decrease in frac-
ture strength was caused by the agglomeration of SiC particles. By
utilizing the Griffith's relationship[36], mean critical flaw sizes for
monoli thic A1203 and A1203/SiC nanocomposi te can be estimated. The
calculated critical flaw size for monolithic Al203 and A1203/5vol%SiC
nanocomposite was estimated to be 25J,Lm and 6J,Lm, respectively. Gener-
ally, the addition of second phase lead to the increase of flaw size.
However, these results for A1203/SiC nanocomposites shows the SiC
addi tion decreases the critical flaw size, conversely as expected. In
addi tion, the observed fracture strength for A1203/SiC nanocomposi tes
is not comparable to the relative increase in fracture toughness,
suggesting that another strengthening mechanism must be operative for
these A1203/SiC nanocomposites.
Scanning electron micrograph of fracture surfaces for monolithic
A1203 and A1203/SiC nanocomposites are shown in Fig.8. The fracture
mode of monolithic A1203 were mainly intergranular and in part intra-
granular. It is well-known that for monolithic A1203, the tensile
stresses are usually generated along the grain boundaries of A1203 by
the thermal expansion anisotropy between a-axis and c-axis of Al203 and
result in inducing grain boundary fracture[37]. The fracture behavior
for monolithic A1203 in this work is consistent with other results[38].
On the other hand, the observation of fracture surface by scanning
electron microscopy showed that the matrix fracture for A1203/SiC
nanocomposites was predominantly intragranular. This significant
change of fractography in Al203 matrix is thought to be contributed to
both the reinforcing at grain boundary caused by the radial compressive

172
 1200

t
C1l
~ 1000

OJ 800
~

r
c:

t
~ 600
U5 1
~
:=l
400
.:160O-C
U
C1l 200 .: 1700·C
u: .: 1800·C

0
0 10 20 30 40
SiC Content (vol%)

Fig.7 The effects on hot-pressing temperature and SiC volume content

on the fracture strength for Al203!SiC nanocomposites.

Fig.8 Scanning electron micrograph of fracture surfaces for monolith-

ic Al203(A) and Al203!5vol%SiC nanocomposites(B).

173
 stresses in matrix and the crack attraction due to the tangential
tensile residual stresses around the SiC particles in matrix for
A120a/SiC nanocomposi te. Therefore, it may be concluded that the
strengthening mechanisms for AlzOa/SiC nanocomposites are considered to
be the decrease in critical flaw size and the toughness increase asso-
ciated with the dispersion of SiC particles. The decrease in flaw
size are attributed to the refinement of microstructures due to the
uniform dispersion of nanometersize SiC particle wi thin A120a grains
and the effects of residual microstresses generated by the thermal
expansion mismatch between AlzOa and SiC.

4. Hot-hardness (short-time hot-hardness test)

The temperature dependence of hot-hardness for monolithic A120a

and AlzOa/5, 11, 17vol%SiC nanocomposite is shown in Fig.9. The hard-
ness for both monolithic AlzOa and A120a/SiC nanocomposi tes decrease
with increasing temperature. Honoli thic A120a, in special, exhibited
the marked fall in hardness over 800·C. On the contrary, the decrease
of hardness for AlzOa/SiC nanocomposites with temperature was found to
be lower from the ambient temperature up to 1350·C, comparing to those
for monolithic AlzOa. These results indicate that the degradation of
high temperature hardness were significantly improved by the SiC addi-
tion. Also, the degradations of hot-hardness were apparently depend-
ent on the SiC content for AlzOa/SiC nanocomposites. With increasing
the volume fraction of SiC particles these AlzOa/SiC nanocomposi tes
exhibited the furthermore smaller decrease in hardness up to 1300·C.
As shown in figure by arrow, the change of slope are observed at 800·C
for monolithic A120a and at 1200·C for A120a/5vol%SiC nanocomposites,
although AlzOa/11,17vol%SiC nanocomposites indicate linear behavior up
to 1300·C. These changes of slope must be related with the change of
the dominant mechanism of deformation. Above these critical tempera-
ture, the another slip systems in addition to basal slip system are
thought to be activated to increase the plastic flows[39].
The deformation and fracture behavior around indentation were
observed for monolithic AlzOa and AlzOa/SiC nanocomposites. The crack
at each corner of indentation diminished with increasing temperature
for both monolithic A1203 and A1203/SiC nanocomposites. In special,
for monolithic A120a, the brittle fracture was observed only below
600·C and the grain boundaries fracture were appeared over 600·C.
These grain boundary fractures were caused by the softening of grain
boundary phase and grain boundary sliding. On the contrary, clear
radial cracks were observed at indentation corner up to 1000·C for
AlzOa/5vol%SiC, at 1100·C for AlzOa/11vol%SiC, and at 1200·C for
AlzOa/17vol%SiC nanocomposites. These critical temperature, TB/D,
which are called to be transition temperature of brittle-ductile frac-
ture[40] , increased with the SiC content. Therefore, these results
suggest that SiC particles wi thin A120a matrix grain retain the high
temperature deformation due to the inhibition of grain boundary sliding
caused by softening and cavity formation. Hot hardness shows the
ability to withstand the elastic and plastic deformation and crack
growth(high-temperature fracture)[41]. However, only short-time
hardness test could not identify completely the deformation and creep
mechanism, although it yielded the useful data on the high-temperature
fracture behaviors by hot-hardness test.

5. Hot-hardness creep

The creep tests were performed by varying loading time under 4.9N
at a constant temperature at 1000 to 1300·C (above ~1/2Tm: Tm is the
melting point on the absolute scale) for monolithic AlzOa and

174
A1203/5vol%SiC nanocomposites. Fig.10 shows the variations of hardness
with loading time for monolithic Al203 and A1203/5vol%SiC nanocompos-
ites. The hardness for both monolithic Al203 and Al203/SiC nanocompos-
ites decrea~ed as the loading time was increased. Linear relationship
was obtained between hardness and loading time at 1000 to HOO·C,
al though the loading time dependence of hot-hardness consisted of two
regions (region I and II) for both monolithic A1203 and A1203/SiC
nanocomposi tes above 1200·C. However the region I were shifted to
longer loading time by the addition of SiC for A1203/SiC nanocompos-
ites, comparing to monolithic A1203. The change of slope in Fig.10
suggested that there exist two thermally activated process correspond-
ing to region I and II.

100.------,-----,----------,

<il [j
a..
Q. 10
~ e
• ~
Ul
Ul I • il e
..
Ql
C
'0 •
(ij
I •.. ,'Iono c •
S"""-SoC
•
'"
0
l1VO'%SC
l1vo'%SC
1
0 500 1000 1500
Temperature (.C)

Fig.9 The temperature dependence of hot-hardness for monolithic A1203

and Al203/5, 11, 17vol%SiC nanocomposite. Arrow shows the change
of the slope.

According to the analysis by Atkins et al[ 42], the hot-hardness

creep in the temperature range above 1/2Tm is consistent with a tran-
sient creep. The relation of the following form is given between the
hardness and loading time,

A/t=Hmexp(-Q/RT)

where H is hardness, t is loading time, Q is the activation energy for

creep, A and m are constants. Q value of activation energy and m value
in region I and II for hardness creep were calculated from the data at
1200 and 1300·C above O. 6Tm using above equation. Those results are
summarized in Table 1 for monolithic A1203 and A1203/SiC nanocompos-
ites. The value of Q was 78±17kcal/mole in region I and
110±10kcal/mole in region II for monolithic A1203, respectively. The
Q value in region I is close to that of obtained for basal, prismatic
and pyramidal slip system[43-45]. The Q value in region II was com-
parable with the aetivation energy for self diffusion, namely, grain

175
 boundary diffusion of A1 3+[46,47]. On the other hand, Q values for
A1203/5vol%SiC nanocomposites were 129t26kcal/mole in region I and
65±22kcal/mole in region II. Activation energy in region I and II for
A1203/SiC nanocomposi tes are not consistent with those for monolithic
Al203 in each creep region. These results suggest another creep mecha-
nism is operating in these nanocomposites. The activation energy in
region I for A1203/SiC nanocomposites are close to those of grain
boundary or lattice diffusion process. Therefore, the creep mechanism
in region I for A1203/SiC nanocomposites may be controlled by A13+ in
lattice or 0 2- diffusion at grain boundary. Although the detailed
analyses are too difficult for these composites, it is reasonable to
think that the slip deformation could be inhibi ted by intragranular
SiC within A1203 grains, for example, the prohibition of dislocation
climb and pile up. Nevertheless, it may be concluded that the SiC
dispersion wi thin A1203 matrix grains significantly improve the creep
resistance of A1203 due to the inhibition of slip deformation.

CONCLUSIONS

A1203/SiC nanocomposites were prepared by hot-pressing the mix-

tures of fine Al203 and SiC powder using the conventional powder metal-
lurgical technique. The microstructure and mechanical properties up to
high temperatures were examined for A1203/SiC nanocomposites.
1. The observation of transmission electron microscopy indicated
that A1203/SiC nanocomposi tes were composed of equi-axed A1203 matrix
grains and SiC particles were predominantly dispersed on nanometer

E 6

i rJ)
rJ)
Cl>
-E ell
5 O:1000'C O:I000·C
.:ll00·C 11/ .:1100·C
I
O:IZOO·C 0: 12OO"C
~ .:13OO"C .:13WC
.........--,---,---,_......J
4'---'---'---...L~""""""...J.......l_

-4 -2 0 2 4 6 -4 -2 0 2 4 6
log Time (sec) log Time (sec)

Fig.l0 The variations of hardness with loading time for monolithic

Al203 and AI203/5vol%SiC nanocomposites.

Table 1. The activation energy in region I and II for monolithic A1203

and A1203/5vol%SiC nanocomposites. (kcal/mol)

Region I Region II

Monolithic Al203 78±.17 llOilO

A1203/SiC nanocomposites 129±26 65±22

176
scale within Al203 matrix grains. These intragranular SiC were gener-
ally faceted and in part spherical. High resolutional electron micro-
scopic showed that the interface between A1203 and intragranular SiC
within A1203 matrix grains made direct bonding without any reaction
phases.
2. The grain size and relative density for A1203/SiC nanocompos-
ites were strongly dependent on the SiC volume fraction and hot-press-
ing temperature. The SiC particle was found to control the matrix
grain size and densification by the pinning effect of grain boundary
mobility during hot-pressing.
3. Hardness, fracture toughness and strength for A1203/SiC nano-
composi tes were significant improved by the dispersion of SiC parti-
cles. Hardness linearly increased with increasing SiC content up to
33vol%. The maximum fracture toughness of 4. 7MPam l / 2 was achieved by
the addition of only 5vol% SiC and slightly decreased above Ilvol% SiC.
The analysis of fractography and observation of crack propagation
indicated that the crack deflection and the residual stresses effects
generated by the therm~l expansion mismatch between Al203 and SiC would
be operative as the main toughening mechanism. Fracture strength were
increased from 350MPa for monolithic A1203 to 1050MPa for A1203/SiC
nanocomposites. The strengthening mechanisms for A1203/SiC nanocompos-
i tes were considered to be the decrease in critical flaw size and the
toughness increase associated with the dispersion of SiC particles.
4. A1203/SiC nanocomposites exhibited higher hardness at all test
temperatures and small decreasing rates in hardness with the increase
of temperature than those for monolithic A1203. These improvements of
hot-hardness is attributed to the prohibition of high temperature
deformation by the SiC particles wi thin Al203 matrix grain, which is
caused by the decrease of the grain boundary sliding associated with
the grain boundary softening and cavity formation.
5. The creep behaviors for A1203/SiC nanocomposites were evaluat-
ed by the time-dependence test of hot-hardness. This creep rate for
A1203/SiC nanocomposites were apparently reduced by SiC dispersion.
This improvement in creep is due to the dislocation pinning with hard
SiC particles.

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256-8(1986).
28. K. Niihara, K. Suganuma, A. Nakahira and K. lzaki, J. Mater. Sci.
Lett., 9 598-9(1990).
29. D.L. olgaard and B. Evans, J. Am. Ceram. Soc., 69 C272-7(1986).
30. W. Voigt, Lehrbuch der Kristallphysik, 739(1928).
31. A. Nakahira, K. Niihara and T. Hirai, J. Ceram. Soc. Japan 94 767-
72(1986).
32. K. Niihara, A. Nakahira, T. Uchiyama and T. Hirai, Fracture Meehan
ics of Ceramics 7, Ed. by R.C. Bradt, A.G. Evans, D.P.H. Hasselman
and F.F. Lange, Plenum Press pp.103-16(1986).
33. J. Selsing, J. Am. Ceram. Soc., 44 419-20(1961).
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D.P.H. Hasselman and F.F. Lange, Plenum Press pp.599-609(1974).
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91(1990).
36. D.W. Richerson Modern Ceramic Engineering, Marcel Dehher, N.Y.
(1982).
37. R.W. Rice, Proc. Brit. Ceram. Soc., 20 205-57(1972).
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741-50(1984) ..
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(1966).
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(1980).
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46. Y. Oishi and W.D. Kingery, J. Chem. Phys., 33 480-6(1960).
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46-53(1980).

178
FRACTURE TOUGHNESS OF SiC-WHISKER/ Zr02 / Al 20 3

TRIPLE PHASE COMPOSITES

Y. Kogo*, H. Hatta**, and Y. Kagawa***

* Mitsubishi Electric Corporation, 1-1-57 Miyashimo

Sagamihara, 229 Japan
** The Institute of Space and Astronautical Science. 3-1-
1 Yoshinodai, Sagamihara, 229 Japan
..* The University of Tokyo. 7-22-1 Roppongi, Minatoku
Tokyo. 106 Japan

ABSTRACT

An analytical model to predict fracture toughness of zirconia

composites is proposed. In this model, one of reinforcing phases is
high strength fibers and the other is transforming zirconia. The
analytical model for isotropic zirconia composites has already been
proposed by several authors. However, composite materials usually
possess anisotropic material properties. Thus in this paper an existing
isotropic solution was extended so as to be able to deal with anisotropic
composites. Then to demonstrate effectiveness of present formulation,
parametric study was carried out. wherein the material constants were
simulating SiC-whiskers / Zr02 particles / Al203 or glass matrix. The
numerical results suggested that the interaction effect between the
transforming zirconia particles and reinforcing fibers in the composites
was rather small. Hence improvement of fracture toughness by
transformation of zirconia particles can almost be considered to work
independently with such mechanisms as fiber bridging and interfacial
sliding.
INTRODUCTION
It is well known that dilatant deformation in the martensitic
transformation remarkably improves fracture toughness of the zirconia
ceramics. By virtue of this high fracture toughness, several goods, such
as scissors and kitchen knives, have been developed. The mechanism
of this improvement have been investigated enthusiastically by many
authors 1.2 because it has possibility to become key concept to
overcome the most serious shortcoming of ceramics, Le. low fracture
toughness. Among the investigators discussing the fracture toughness of
zirconia, Evans and Hutchinson et al appears to be the most successiing

FrOJ:/ure Mechanics afCeramics. Vol. 9

Edited by R.C. Bradt e/ al., Plenum Press, New York, 1992 179
group. They proposed 3,4 two kinds of analytical models, which
qualitatively explain well the toughening behavior of the zirconia
ceramic.
By the martensitic transformation, the critical stress intensity factor
KIC of zirconia certainly raises from the original material. The amount
of the improvement was estimated to be 1.5 to 3 times. However, KIc of
partially stabilized zirconia is about 6 to 10 MPam l / 2 and this value is
about 1 order smaller than the conventional metals. Thus toughness
improvement is still highly required to zirconia ceramics for easy
handling and their reliable structural use. Several measures have been
proposed to raise furthermore the fracture toughness of the zirconia
ceramicS. One of promising method appears to be to combine the
transformation toughening with other kind of toughening mechanism.
As a natural extension of this concept. we are now trying combination
of the fiber bridging and transformation toughening by intermingling
whiskers in the zirconia composite. Experimental results indicates the
fracture toughness increases by virtue of this combination and this
results is to appear in other Joumal6 .
In this paper, an analytical model to predict the fracture toughness
of an anisotropic composite with triple phases, I.e. reinforcing
whiskers, zirconia particles, and ceramic matrix, is developed to
discuss the fracture toughness behavior under the condition interacting
two kinds of toughening mechanisms. By use of the derived formula,
parametric study will be carried out by changing material and
geometrical constants to demonstraite the interaction effect between
the transformation and fiber bridging. Furthermore, the interaction
effect of the transformation toughening and microcrack toughening is
also examined by use of the same formula and by setting elastic moduli
of reinforcing phase equal to O.

ANALYfICAL MODEL
There are two kinds of analytical model dealing with fracture
toughness of materials accompanying martensitic transformation like
the partially stabilized zirconia. One of the approach is developed by
Budiansky et al. 4 They conSidered energy balance before and after crack
extension and obtain energy release rate. In the other approach, stress
intensity factor was calculated through stress analysis in the vicinity of
crack tip. Both of the models predict the same order of magnitude of
the transformation toughening and give individually plausible physical
explanations. These models, however, dealt with only isotropic
materials. On the other hand, composite materials intended to analyze
here, usually exhibits anisotropic material properties. Thus some
modification must be done in the existing solutions so as to deal with
anisotropic composite materials. Although both models appeared to be
able to extend to the anisotropic materials, we adopted stress approach
because this solution expected to give supplementally such valuable
information to fracture analysis as stress and displacement field as well
as the stress intensity factor.
McMeeking and Evans3 used eq. (1) to calculate increases of stress
intensity factor ilK of the zirconia ceramic:

ilK ={ T·h ds (1)

laST

180
where Sr denotes the boundary of the process zone in which the
martensitic transformation of zirconia is occurring and the line
integration ds is to be done along Sr. T denotes traction vector
originated due to the transfonnation of the zirconia and assumed to act
on Sr. T can be obtained from eq.(2) in terms of the mean value of the
transfonnation strain (eigen-strain 7) eT .
T =- n. C. eT (2)

where n and C are outward nonnal vector on Sr and elastic modulus

tensor. respectively, and the dot denotes inner products. In the case of
McMeeking et al.3. pure zirconia ceramic was analyzed. Thus the direct
value of the transformation strain of the zirconia can be utilized for
e T . On the other hand. the analytical model in this study is rather
complicated as shown in Fig.l where the domains of reinforcing fibers.
zirconia particle, and matrix are represented by WI. W2' and D-W I-W2,
respectively. Different elastic modulus between constituent materials
and anisotropic fiber distribution gives rise to anisotropic e T in the
composite. which is different from the simple mean value of
transformation strain of zirconia particle. eT in composite materials can
be rather easily calculated by use of equivalent inclusion method 7 even
in the case of those with fiber orientation distribution 8 and with two
kinds of reinforcing phase 9 as shown in Fig.I. In this study, the
orientations of reinforcing fibers and zirconia particle are assumed to
be distributed 2- or 3-dimensionally random to simulate actual
composite materials.

Fig. 1 An analytical model to calculate fracture toughness of a hybrid composite

accompanying martensitic transformation.
h in eq. (1) is the weight function, Bueckner lO defined. h for a semi-
infinite crack in an infinite isotropic body has been already obtained by
several authors. However. within our best knowledge, h for an
anisotropic body. convenient for present study. have not been given
explicitly. To obtain anisotropic h. Rice's formula ll given by eq.(3) is
useful:

h = r l /2[2(sin e)(dg/de)-(cos e)g]/4 (3)

181
where vector g is derived from any displacement field with same crack
geometry u. The relation between g and u are shown by eq.(4) 11

u =H-l K r 1/ 2 g(9) ( 4)

The several displacement fields for anisotropic body are given by Sih.
Paris. and Irwin 12.
By use of eq. (1-4), toughness change ~K can in principle be
calculated. However. we do not have data as for shape and size of the
process zone. This measurement is now under progress. Thus at the
present stage we assume that the shape of the process zone is the same
as McMeeking1 assumed and numerical results is shown by the form
~Kw-l/2. Here w stands for width of the process zone. Since ~K can be
shown to be proportional to w 1/ 2 like the case of McMeeking.
multiplying ~K by w- 1/ 2 to cancel the dimensional dependence to
numerical results.

NUMERICAL RESULTS
Material properties shown in Table 1 were used for numerical
calculation of fracture toughness by the use of eq.(I). Glass matrix
composite was afterward supplemented in order to illustrate the effect
of anisotroic properties on the fracture toughness. Since original Al20 3
matrix possesses the same order of magnitude of elastic modulus as
reinforcing materials. elastic properties of the alumina composite
does not exhibit intensive anisotropy. Besides the combination
of materials shown in Table 1. a composite replaced reinforcing SiC
whisker by microcrack was also calculated to discuss the interaction
effect between microcrack and transformation. This interaction is
frequently observed in the fracture process of zirconia ceramic.

Table 1 Properties of Constituent materials of hybrid composites.

Aspect
Materials E (GPa) lJ
ratio

SiC whisker 482 0.23 50

Zr02 Particle 373 0.23 --

AI203 275 0.22 --
Glass 70 0.22 --

Fig.2 shows the R-curve behavior of a zirconia composite as a

function of non-dimensionalized crack length a/w in which SiC
whiskers are assumed to be oriented randomly on the plane
perpendicular to the crack plane. Actually we calculated the R-curve
behavior. all the cases. In the follOwing. however. let us pay attention
only to equilibrium value. i.e. the maximum value in this figure.

182
 600

500
ro
c.
~
400
;\J

300 SiCw/Zr02/Glass
~
(2D-random)
:¥:: 200
<I Perpendicular to 2D plane
100

0
0 1 2 3 4 5 6
a/w

Fig. 2 R-cuNe behavior of an SiC-whisker/Zr02/Glass hybrid composite.

The effect of mixed whisker on the fracture toughness was shown

in Fig.3. It is obvious from the figure that toughness increases with
volume fraction of the whisker. Since toughening mechanisms other
than the transfonnation toughening is not included in this calculation,
this material should actually exhibit higher toughness than the values
in the figure due to the such effects as the crack bridging, crack
deflection, and crack bowing. Two kinds of curves in the figure are
intended to compare the effect of anisotropic material properties.

600
SiCw/Zr02/Glass
(2D-random)
~ 500
~ perpendicular 10 20 plane

400
~
:¥::
<I 300
Parallel 10 20 plane

200
o 0.1 0.2 0.3 0.4 0.5
Volume fraction of SiCw

Fig. 3 Effect of volume fraction of whisker and anisotropy of mechanical

properties on fracture toughness.

The solid and dashed lines correspond to 2D random orientation

composites in which the reinforcing fibers lie on the planes parallel
and normal to the main crack, respectively. Hence the composites of
solid and dashed lines possess the lowest and highest stiffness in the
direction normal to the crack plane. It can be concluded from the
figure that the anisotropic properties do not have profound effect on
the fracture toughness.

183
 Finally. the effects of microcrack and vOids on fracture toughness of
zirconia composites are shown in Fig.4 as a function of the volume
fraction of microcrack and voids. where the volume fraction of the
zirconia particle VZ r 02 was assumed to be constant 0.2. It was
anticipated before the calculation that these opening spaces
(microcracks or voids) must absorb dilatant deformation yielded by the
martensitic transformation. It is. however. obviouS from the figure that
the existence of the defects has only little effect on the
fracture toughness. It should be noted that the effect of so called
microcrack toughening is not included in present calculations. Thus
higher toughness can be actually expected for these material systems.

900
ro
a.. 850 Zr021AI2031Void
:E ( Vzr02 = 0.2 )
('II
800 aspect ratio
0.1 1.0
750
~
~ 700
<l
650

600
0 0.03 0.06 0.09 0.12
Volume fraction of Void
Fig. 4 Effect of volume fraction of microcracks on fracture toughness of a zirconia
composite.

CONCLUSIONS

An attempt was made to formulate the effect of martensitic

transformation in an anisotropic hybrid composite materials on fracture
toughness. The parametric studies based on derived equation yielded
the following conclusions.
(1) The derived formula expressing transformation toughening resulted
in reasonable numerical values and this analytical model was shown to
be quite effective to calculate fracture toughness in a wide range of
material systems.
(2) Mixing of whiskers in a zirconia composite raise the fracture
toughness even if the other kinds of toughening mechanisms are
excluded.
(3) Microcracks or vOids in zirconia composite slightly lower the
fracture toughness. Thus if the microcrack toughening is added to the
results. improvement of toughness can be expected for this system.

184
REFERENCES
1. Evans, A. G., Cannon, R M., 1986. Toughening of Brittle Solids by
Martesitic Transformations, Acta Metall., 34: 761.
2. Evans. A. G., Heuer. A. M.• 1980. Review-Transformation
Toughening in Ceramics : Martensitic Transformation in Crack-Tip
Stress Fields. J Amer. Ceram. Soc.. 63 : 241.
3. McMeeking. R M.• Evans. A. G., 1982. Mechanics of
Transformation Toughening in Brittle Materials, J. Amer. Ceram.
Soc.• 65 : 242.
4. Budiansky. B., Hutchinson, J. W.. Lambropoulos, J. C., 1983.
Continuum Theory of Dilatant Transformation Toughening in
Ceramics. Int. J. Solids Structures, 19 : 337.
5. Hori. S .. 1990, Kyoujinka Zirconia (in Japanese), Uchida
Roukakuho, Tokyo.
6. Kogo. Y., Hatta, H.. Kagawa, Y.. in preparation.
7. Eshelby. J. D.• 1957, The Determination of the Elastic Field of an
ellipsoidal Inclusion. and Related Problems. Proc. Roy. Soc. London.
A241 : 376.
8. Takao, Y.. Chou, T. W.• Taya, M.. 1982. Effective Longitudinal
Young's Modulus of Misoriented Short Fiber Composites. Trans.
ASME J. Appl. Mech., 49: 536.
9. Taya. M.. Chou, T. W., 1981, On Two Kinds of Ellipsoidal
Inhomogeneities in an Infinite Elastic Body : An Application to a
Hybrid Composite, Int. J. Solids Structures, 17 : 553.
10. Bueckner. H. F., 1970. A Novel Principle for the Computation of
Stress Intensity Factors, ZAMM. 9 : 529.
11. Rice. J. R 1972, Some Remarks on Elastic Crack-Tip Stress Fields,
Int. J. Solids Structures, 8 : 751.
12. Sih, G. C., Paris, P. C., Irwin, G. R, 1965, On Cracks in Rectilinear
Anisotropic Bodies, Int. J. Fracture Mech., 1 : 189.

185
R-CURVE BEHAVIOR OF CERAMICS

Rolf W. Steinbrech

Institut fOr Reaktorwerkstoffe

Forschungszentrum JOlich
Postfach 1913,5170 JOlich, FRG

ABSTRACT
The demand for ceramics with improved toughness and flaw tolerance has focused
attention in recent years on R-curve behavior which is characterized by an increase in crack
resistance (toughness) with crack extension. In a brief review, R-curves of various oxide and non-
oxide ceramics are shown in order to demonstrate the potential of the effect and to outline
underlying toughening mechanisms.

The results of R-curvestudies are presented in detail for long cracks in alumina where toughness
increases in some materials up to a factor of 3 after a few millimeters of crack extension. The
toughening in alumina originates from wake-controlled crack tip shielding due to crack surface
friction and interlocking grains. Thus, both crack surface roughness and crack opening behavior
play a key role in the R-curve effect. The influence of microstructure and the effect of crack
geometry on crack opening behavior are demonstrated.

Finally, the long crack R-curves are compared with those determined from stable crack propagation
of short "natural" surface flaws. The short crack R-curves start at a significantly lower toughness
level and do not reach the high ultimate toughness of long cracks. The R-curve results are
discussed with respect to a failure-relevant fracture characterization of ceramics.

1. INTRODUCTION

In the past decade considerable progress has been made to improve the mechanical
properties of structural ceramics /1/. Brittle fracture originates from material defects or processing-
induced flaws, which - upon loading - become unstable. From the materials point of view two
different guidelines are followed in tailoring better suited microstructures.

According to the Griffith instability criterion, which relates the critical fracture stress inversely to the
square root of the critical flaw size, the strength is increased by scaling down the microstructural
dimensions and thus reducing size and size distribution of failure- causing defects.

Frtuture Mechanics of Ceramics, Vol. 9

Edited by R.C. Bradt et ai., Plenum Press, New York, 1992 187
 On the other hand ceramics behave more toughly if stable crack growth prior to catastrophic failure
is achieved by utilizing specific microstructures which generate crack tip shielding. The toughness -
instead of being a constant material property - then increases with crack extension (R-curve
behavior).

The present paper describes the current understanding of the R-curve behavior of
monolithic ceramics in three parts.

First an overview of experimental R-eurves of various ceramics is given and the

underlying toughening mechanisms are outlined in principle.

The second part focuses on the R-curve behavior of alumina. From the large body of
experimental results and theoretical modeling available to date some of the important features are
described. The influence of both material and geometry effects on the increase of toughness (or
crack resistance) is demonstrated. The "waken-controlled origin of the R-curve effect is illustrated
and is analytically modeled in terms of the stress-separation behavior of friction-governed crack
bridging elements. Finally the implication of R-curve behavior on other crack-growth-related
properties of alumina is briefly outlined, by addressing the influence of R-curves on thermal shock
behavior, subcritical crack growth and cyclic fatigue.

The third part of the paper focuses on R-curves of short cracks. While most R-eurve
studies to date are based on crack propagation experiments from long artificially initiated cracks,
little attention has yet been given to the stable growth of failure-relevant short cracks and "natural"
flaws. Experimental measurements are presented for the latter and the R-curves are compared
with those from long cracks.

The results demonstrate that non-eonservative conclusions are usually drawn from long
crack studies with respect to maximum toughness and flaw tolerance.

2. TOUGHNESS BEHAVIOR
2.1 Resistance Curves

Crack propagation studies performed with long cracks in standard testing geometries of
fracture mechanics reveal that many ceramic materials exhibit a rising toughness with crack
extension. A selection of resistance curves, all determined from stable crack growth in compact
tension (CT) tests or similar short double cantilever beam (S-OCB) experiments, is plotted in Fig. 1.
Although the R-eurve behavior is not limited to a specific toughness regime the results tend to
indicate that high toughness of ceramics is a consequence of pronounced R-curve behavior.

Strong R-curve effects with increasing toughness over 1 mm or more of crack extension
can be observed in coarse-grained alumina /4-5/, Si3N4 with elongated grains /6/ and
transformation toughening zirconias like MgO partially stabilized zirconia (Mg-PSZ) /7,8/ and CeO
partially stabilized tetragonal zirconia (Ce-PSZ) /9/. On the other hand flat R-curves are often
measured for Y-TZP and non-oxide ceramics such as hot pressed Si3N4 and sintered SiC /10,11/.
How much the toughness rises with crack extension depends on microstructure, chemical
composition and precracking history, as is evident from the large body of experimental R-curve
results for zirconia-eontaining ceramics and alumina generated in recent years 17,12-14/. In the
case of Mg-PSZ, for example, changes in heat treatm'3nt cause variations in R-curve behavior from

188
flat curves (KR = 2 MPa ~m for overaged material) to strongly rising curves with a final plateau
value of Kp '" 18 MPa ~m 18/. Note that microstructure, composition and crack-geometry-related
changes in R-curve behavior of alumina will be addressed in more detail in Section 3.

In the low toughness regime the R-curves of two very coarse-grained materials are
included. Interestingly the cubic MgAI20 4 spinel 115,161, which is assumed to be free of residual
stresses (no anisotropy of thermal expansion), and microcracked graphite 1171 exhibit modest R-
curve behavior too.

J'
Yu & Shelly
- g-PSZ

_. Ce-TZP
E 12
co
c..
U & Yamanis - Si 3N4- B
~ Ii
(/)
(/) /'
/ ------- - Si3 4- A
UJ
Z /
/
-- y-rzp
I -r,:::'-'-'-,_._._'
(!)
::l • i ---- ..... AI103
o
.. ' .........
• • • • • • ,1 . . . . . . • . . . . • . . • • • • • • • • , • • • • • • • "

l- - SiC

:1.. ,,·,·"'·,·~'.·~~~---_u
,.. ,
I·~'~·~·~·~ ::.~
__ u_--------S-k-.-I~I·
? :. .~! .~
-- MgAl10<
.... GRAil ITE

~~ I I I I I i 1 i
.ii .5e Lee 1.58 1.ee 2.50 3.88 3.se U8

CRACK EXTENSION [mml

Fig. 1 Long crack R-curves of various ceramics tested in compact tension geometries.
(Li & Yamanis 16/, Yu & Shelly 19/, Sakai et a1/17/)

2.2 Toughening mechanisms

The mechanisms that have been recognized as causing toughening of ceramics can be
subsumed under crack deflection and crack tip shielding effects /18/. Microstructure-related crack
deflection occurs permanently in the case of intergranular fracture. The effect can be enhanced by
either tailoring ceramics with in situ grown grain anomalies (e.g. elongated grains in Si3N4 16/) or
by processing composites with localized stress concentrations and second phase crack deviators
(e.g. particles, whiskers, fibers) 11/.

However, microstructural crack deflection typically does not intensify with crack growth and
thus cannot explain long range crack resistance curves like those shown in Fig. 1 for Si3N4 and
A1 20 3. Indeed R-curve behavior fundamentally requires a mechanism which increases its
effectiveness with increasing crack extension.

The second general toughening mechanism, crack tip shielding, automatically satisfies this
condition if - in the absence of plastic deformation ahead of the crack tip - the underlying
microstructural effects are related to the growing crack wake. Shielding-based R-curve
mechanisms, which have been recently reviewed in detail by Evans 11/, may be subdivided into
zone and contact processes /18/.

189
 Zone shielding occurs when elements of a crack-surrounding process zone undergo a
stress strain hysteresis as the crack is passing by, e.g. due to transformation or microcracking. The
effect also may be rationalized by appreciating that a residual compressive stress field is created
within the process zone which inhibits crack opening and thus results in crack shielding. The
potential of transformation toughening for generating R-curve behavior is evident from the Mg-PSZ
curve in Fig. 1.

Contact shielding originates from interaction sites along the crack surfaces where intact
materials ligaments, e.g. grains, particles, whiskers, fibers, or serrated grains, form bridging
tractions which inhibit crack opening. Additional energy is required to overcome the bridging
stresses and to separate the crack surfaces. The R-curves of A1203' Si3N4 and MgAI204 spinel in
Fig. 1 are predominantly attributed to such contact shielding effects /6,16,19/. Details of the
bridging mechanism in AI203 will be addressed later.

However, it has to be emphasized that the above clear distinction between zone and
contact shielding often lacks unambiguous confirmation from experimental crack propagation
studies. This may explain the often controversial debates on the R-curve mechanisms of ceramics,
e.g. the respective roles of grain bridging and microcrack zones in AI 20 3 /20/.

It is also possible that process zone and bridging mechanisms operate simultaneously and
that the dominant mechanism changes as the microstructure is systematically varied. Furthermore
synergetic effects can generate a net toughness larger than that for the individual mechanism /1/.

3. R-CURVE BEHAVIOR OF AI 20 3

R-curve behavior of AI203 was first observed a decade ago in fracture mechanics
experiments unter conditions of slow quasi-static crack propagation /4/. Since then research has
been focused on the characterization of the effect and on a basic understanding of the underlying
microstructural mechanisms. Most crack propagation studies have been carried out with long
cracks in standard testing geometries of fracture mechanics but recently the R-curve behavior of
short failure-relevant cracks and surface flaws has gained major interest too. Following this
historical development the R-curve behavior of long cracks is first described and modeled. In
Section 4 then the short crack toughness behavior will be addressed.

3.1 Long crack experiments

By using notched or precracked specimens and stiff loading equipment quasi static
controlled crack growth can be achieved /21/ to study R-curve behavior. Commonly the single edge
notched (SENB), the double cantilever beam (DCB), the compact tension (CT) or the similar short
DCB (S-DCB) testing geometry are chosen. The stable crack growth response on loading is
measured and the load (P), load-point displacement (d) recorded. Finally, the crack resistance R as
a function of crack length a (crack extension M) can be evaluated from this.

The schematic P(d)-curve in Fig. 2 illustrates some of the important macroscopic

mechanical properties of coarse-grained A1203' After initial elastic increase the P(d)-curve deviates

190
from linearity and despite the onset of crack growth the load-bearing capacity of the specimen still
increases. Beyond the maximum a smoothly decreasing part then follows. Fig. 2 shows a P(d)-
curve where in addition at two different crack extensions unloadinglreloading cycles were run, each
following a previous load relaxation step. The unloading/reloading hystereses reveal an energy
dissipation which is subsequently attributed to frictionally interlocking crack surfaces. Furthermore
a residual displacement occurs, i.e. the crack does not fully close upon complete unloading.

To evaluate the crack resistance from a P(d)-curve the energy release rate (GI) concept
under the assumption of quasi-static crack growth GI = R is convenient. In the compliance (C)
notation this yields

2
p dC
R=G 1 = - ' - (1)
2B da

SENB
pL}
?

DeB E0 ,I

EJ
J

S-OCB
f
IncliJd ng residuial dlsplaccmern b,

0
df7
j
R = p2
2B
dC
da R = 28
p2 dC
da
p ~
B da

Fig. 2 R-curve evaluation from crack propagation experiments in alumina.

were B is the specimen width. Note that the crack length a can be measured in situ following stable
crack growth with a traveling microscope. Correlating a, P and d the crack resistance behavior can
be determined straightfowardly from equation (1). However, the observed hysteresis effects and
the occurring residual displacement have generated a controversial debate about the correct
compliance choice. Various energy-based concepts which consider the residual displacement
effect have been proposed in the past /22/. However a compliance which is related to the
unloading/reloading hysteresis becomes the shallower the further a crack is unloaded, Le. it is not
constant. On the other hand, the compliance through the origin (Fig. 2), tends to be tangent to the
very last part of the reloading curve and thus should represent the specimen stiffness immediately
prior to crack growth. The long crack R-curves shown in the next sections are all determined using
compliance values given by C =d / P.

191
3.2 Influence of microstructure and crack geometry

The R-curve behavior of AI203 is more pronounced in coarse-grained than in fine-grained

materials as illustrated by the SENB results in Fig. 3. Increases in crack resistance up to a factor of
5-10 can be observed in "pure" AI20 3 (99.7 %) with average grain sizes in the order of DA '"
20 Jlm. On the other hand fine- grained materials, which start at a higher initial resistance level
(R o)' do not experience a significant further increase. The resulting crossing of R-curves, also
confirmed by Lawn and coworkers /23,24/, gave rise in the past to some confusion about KIC
values determined with different testing geometries. Depending on the amount of crack extension
along the R-curve, opposite trends in the grain size dependence of KIC may result for different
testing geometries. Clearly, KIC values determined from double torsion (DT) tests after large
amounts of crack extension must show an opposite grain size dependence to those KIC values
determined in SENB tests without significant stable crack growth.

In addition to grain size effects the mode of microstructure strongly influences the R-curve
behavior of A1203' For materials with comparable average grain size the variant with
predominantly intergranular microfracture gives rise to the stronger R-curve effect.

Grain size and mode of microfracture can vary in a rather complex way with the chemical
composition. Fig. 4 shows the interrelationship between grain size, mode of microfracture, R-curve
effect and MgO content. Magnesia is known to supress grain growth of AI 20 3 and to support the
formation of homogeneous microstructures.

At very low MgO content, noting that the sintering procedure was kept the same for all
concentrations, AI203 exhibits elongated grain growth and fracture is predominantly transgranular.
However, with increasing MgO content the average grain size decreases and the percentage of
intergranular fracture increases. The strongest R-curve effect, represented by the increase of crack
resistance (R p), is observed at about 4· 10-2 wt% MgO. This concentration is close to the solubility
limit of MgO in AI 20 3 /25/ which obviously causes a big gradient in the microfracture and the grain
size behavior.

Besides these material-specific aspects the crack geometry has significance for the R-
curve results gained from a crack propagation test. A series of R-eurves determined from SENB
specimens with different notch depth is shown in Fig. 5. The starting crack resistance Ro is nearly
constant for all R-curves but the slopes are different and increase with notch depth. From this and
from different R-curves gained with various testing geometries (e.g. SENB, DCB, DT /26/) it is
evident that long-crack R-curve behavior is not a unique material property.

3.3 Mechanisms and modeling

The origin of the microfracture mechanisms which cause the R-curve effect of alumina has
been repeatedly localized in renotching experiments /27-29/. In such fracture tests first a crack is
propagated to generate the R-curve effect. Then the crack wake is partially or completely machined
away (renotched) and the crack propagation test continued. Steinbrech and coworkers /27,28/
demonstrated that the resistance is diminished upon removing the wake. Alternatively, if the
unbroken ligament is sawn away and the completely cracked but still not separated specimen is
subsequently loaded in tension crack bridging forces can be measured /29/.

192
 r
~..
..,:~
.. -)/;
.,
q , .

~/~
-~
.co
'"..

~
u
c
2
.
'"
iii
L
50

.....
.~
. e
\~ u o+-~-r~-,r-~..,-~---.~----.
05 06 0.7 08 09
crock length o/w

1: 100
-.
.CO

'".
u

...5 50

..
·iii
L

~
e
u 0 +---r--r~----.-~.--~...,~---.
0.5 0.6 0.7 08 09
crock length o/w

-~ 100 D.:4p.m
-.
.!:
'"..
u

...5
'iii
50

~
.>:

e
u

u 0 +---r--r~-,r-~.---r--r~---r-
0.5 0.6 0.7 0.8 0.9
crock length o/w

Fig.3 Grain size dependence of R-curve behavior in AI 2 0 3 (W = 7mm ).

~
100
IF
.c::: -'- -.-.-
!:= 80
\
~E I
\
....,
"- 60 I I

.c::: Ii
n.
ct: 40
I
I' I
\
E
:t 20
- - - -- - - -- - - -0"
c
<
0 0
2,10- 2 10- 1 2 4 10" 2
MgO in wl%

Fig.4 Influence of MgO contant on grain size (D A), percentage of intergranular fracture (IF) and
crack resistance Rp = R (L'.a = 2.1 mm) of AI 20 3

193
 100..._-----------------,
SE B
AI,:),.o.. 6;Jm

o +-~__r_--~-,...._~..._~__r_-_.,..,--r-...-------i
01 OJ O.S 0.& 01 0&
O/w

Fig. 5 Influence of notch depth on R-curve behavior of AI 20 3

Strong evidence for crack bridging also emanates from microscopic and SEM /30-32/ in
situ crack path observations. The two stages of crack extension in Fig. 6 reveal changes in the
main crack path and side cracking in the wake regime. Both effects can be attributed to serrated
grains which form bridging sites along the crack surfaces /19/. Also unbroken grains /33/ and
elastic ligaments /34/ have been observed. Note that crack path observation is restricted to the
specimen surface which only reveals part of the interlocking possibilities given if 3-dimensional
crack topography is considered.

While the crack bridging phenomena are well established only little experimental evidence
supports the additional existence of zone shielding effects in alumina. Assuming that as a
consequence of the anisotropy of thermal expansion polycrystalline alumina contains local residual
stresses the formation of a microcrack process zone surrounding a long crack is very likely /35,36/.
Indeed the existence of microcrack zones has been recently reported from small angle x-ray
scattering /37/ and acoustic microscope /38/ experiments. However, the shielding effect estimated
from this seems to be too small to contribute significantly to the R-curve effect /39/.

Thus it seems justified to consider bridging phenoma when modeling the R-curve behavior
of A1 20 3 . Various approaches have been reported /23,33,34,40/ which, although different in detail,
have in common that the increasing crack resistance of alumina is a consequence of increasing
contact shielding in the crack wake.

Assuming that the total resistance has two additive contributions, the crack-Iength-
dependent wake term (Rwake) and the constant crack tip resistance (Rtip = Ro), then the total
resistance is given by /19/

R = Rwake + Rtip (2)

The task of R-curve modeling is to evaluate an explicit formulation for Rwake which
considers both the material and geometry influences on the R-curve effect of A1 20 3 . The basic
situation can be illustrated with the aid of the schematic in Fig. 7.

Consider a crack which starts from the notch of a standard test specimen (e.g. DCB) and
which grows with intergranular microfracture to create local deflections from the general crack path
direction. The rough crack surfaces thus generated may be still in physical contact at some

194
 \. .-,. i." t'
l..
~

"
~;.

,
r

~,

,,'

Fig. 6 Microscopic crack path observation. Changes in crack path demonstrate wake effects.

IJJ
U
Z
<l:
~
ell
enW
a:
::.::
u
<l:
a:
U

CRACK LENGTH

Fig.7 Schematic model of R-curve behavior in A1 2 0 3 .

195
locations in the wake and contribute to the crack tip shielding. At first, the growth of the wake zone
is correlated with the distance between crack and notch tip, Le. an increase in macroscopic crack
resistance is measured with crack extension.

However, crack propagation is also accompanied by crack opening displacement which

also depends on crack and testing geometry. In consequence a maximum interlocking depth om of
the bridging sites exists beyond which no further interaction occurs. This limits the length of the
wake zone and gives rise to the plateau-like saturation behavior of R-curves.

The model suggests that crack surface roughness and crack opening behavior playa key
role with respect to the geometrical aspects of the R-curve behavior of A1203' Experimental crack
contour measurements indicate that a linear hinge model can be used to describe the crack
opening behavior. Furthermore, the maximum interlocking depth as determined from 0m-
measurements with aluminas of different grain sizes (DA) follows the relation /19/

(3)

Within these geometrical boundary conditions the energy dissipation in the crack wake is
governed by the stress-separation behavior cr(u) of the bridging elements (Fig. 8). The observed
friction effects during unloading/reloading cycles of precracked specimens strongly support a tail-
dominated cr(u) behavior as introduced by Mai and Lawn /41/

(4)

where crm is the maximum bridging stress and n considers the stress decrease with crack surface
separation u. The cr(u)-function descibes the separation behavior of a discrete bridging element
and thus represents a material property.

L . . - - - - - - ' ".... u

Fig. 8 Wake effect modeling. Tail dominated stress-separation function cr(u) considers the
observed friction effects.

In order to evaluate the total wake contribution exactly, a summation of the effects from all
bridging elements within the wake zone should be performed. To simplify this task the bridging
effects are conveniently considered to be smeared over the wake zone. Taking furthermore
non-steady-state crack opening behavior into account, Le. the crack opening angle changes with
crack extension, the wake contribution to crack resistance may be written / 20/

196
 Z
m

Rwake = 2 J a(u(z)) ~
da
dz
(5)
0

z
with a(z) am (1 - _ )n (6)
zm

Note that similar Rwake expressions can be derived using weight function methods 142/.

The analytical expressions for Rand Rwake allow in combination with the assumed
constant crack tip resistance (Rtip) the R-eurve behavior of alumina to be modeled. In Fig. 9 a the
R-curves of s-DCB experiments are simulated using am and n as fitting parameters.

As the model greatly simplifies the microstructure by only assuming one discrete grain size
rather than a grain size distribution it seems unreasonable to further elaborate the "best-fitting" set
of am and n values. Yet, it should be emphasized that future modeling has to include a a(u)
function derived from first principles.

The potential of this geometry-based R-curve model becomes evident by switching from
one testing geometry to another. Using the am and n values appropriate to the s-DCB geometry
(Fig. 9 a) the shape of SENB R-curves can be predicted correctly (Fig. 9 b). Obviously there are
differences in the "plateau" level of the two testing geometries, which are related with the non-
steady-state crack opening behavior, Le. the change in crack opening angle a with crack extension.
In the case of fixed a, which is given in specimens with large dimensions compared to the size of
the wake zone, the wake resistance becomes independent of the bridging zone size 141 1

urn
Rwake =2 J
o
a(u)du (7)

From equation (7) a plateau toughness of 65 J/m 2 is calculated for a DA = 16 11m material,
which is significantly lower than the upper resistance values measured in SENB. Note that similar
overestimations of resistance (toughness) are reported from R-curve measurements with
composites using too small specimen sizes 143/.

Despite the crude assumptions with respect to the averaging DA-values used the wake
model also describes the grain size dependence of R-curve behavior in reasonably good
agreement with experiments (Fig. 10).

3.4 Impact of R-curve behavior on other crack-growth-related phenomena

Besides the obvious toughening effect, the increase of crack resistance with crack
extension should also influence all other crack-growth-related damage mechanisms of ceramics.
Some aspects of the impact of R-curve behavior on thermal shock damage, subcritical crack
growth and cyclic fatigue are briefly addressed next. Note that more detailed studies are reported
by other authors in these proceedings 144-46/.

197
 100
s-DCB
o 0

E
......
Z
a:: so

_.- n : 2 a ~ = 33~Po
- n : 3 a ~ = 1.5 Po
----. n = I. a ~ : 60 Po

o+-r-~~--.-~-,-~.,..-,.-,........,-.,.-.--.~-r-.-.-r'
16 17 18 19 20
a [mmJ

Fig. 9 a)Simulation of experimental R-curves: s-DCS geometry.

150

100

E
......
z
a::
50

o+-'--'-~--.-~-r-~-r--""'-,---~-,---~-'---'--r'
0.2 0.6 0.8
o/w

Fig. 9 b)Simulation of experimental R-curves: SENS geometry.

100

E
......
z
a:: 50

O+-~-T, --. ,-- ..J

0.5 0.6 0.7 08 09

o/w

Fig. 10 Grain size dependence of R-curve behavior (theoretical

curves with crm=46 MPa, n=3).

198
3.4.1 Thermal shock behavior

In thermal shock situations local crack-driving forces are generated which exceed the
material toughness and thus cause preexisting flaws or defects to grow. The amount of possible
crack extension depends on i) the crack geometry and the time dependence of the crack-driving Gl
and on ii) the crack length geometry and temperature dependence of the material resistance R. As
a consequence a ceramic material with pronounced R-curve behavior is expected to be less
sensitive to a thermal shock damage. Two effects, both increasing the retained strength after
thermal shock, may originat" from R-curve behavior. Less crack extension will occur if thermal
shock cracks have to grow against a rising material resistance and higher stresses are necessary
to repropagate cracks which have generated bridging elements during previous thermal shock
growth.

Hasselmann 1471 introduced a thermal shock parameter which relates the retained strength
(modulus of rupture) to the fracture energy Ywof (work of fracture). However, as Ywof is a quantity
which averages the fracture process with respect to the fractured ligament size it seems not to be
adequate in the case of R-curve behavior. Only recently, concepts, which are based on fracture
mechanics approaches have attempted to overcome this problem by incorporating R-curve
behavior and considering exactly the shape of the R-curves 144,48/.

Although the non-unique nature of R-curves complicates such approaches a general

relationship between R-curve shape and retained strength can be expected. Experimentally water
quenching tests and crack propagation studies with aluminas of different grain size (all sintered
from the same starting powder) show that the slope of the measured R-curves can be directly
correlated with the retained strength (Fig. 11).

The correlation clearly illustrates the favorable influence of pronounced long-range R-curve
behavior in cases of severe thermal shock damage.

0.60
GRAIN SIZE
6-
b 0.50 ' " 181lm
o 171lm
I
I-
(9 0.40 o 10Ilm
Z 6.
o
•
W
a: 0.30
I-
(j)
0
w
Z 0.20
::i:
I-
W
a: 0.10

0.00
0 50 100 150 200 250 300
2
SLOPE OF R-CURVE [J/m ]
Fig. 11 Correlation between thermal shock and R-curve behavior for aluminas with different grain
size. «Jt 1 (Jj: normalized retained strength after thermal shock damage, m: slope of
R-curves)

199
3.4.2 Subcritical crack growth

For lifetime prediction of ceramic structures knowledge of the thermally activated and
environmentally assisted subcritical crack growth is essential. The increase of crack velocity (v)
with the energy release rate GI determines the time to failure of a ceramic material. Note that the
crack kinetics are often empirically described in terms of the relationship

(8)

where A and n are crack growth parameters. To convert stress intensity into energy release rate
GI = KI 2/E is used in this paper, E : Young's modulus.

In ceramics with R-curve behavior a strong increase of the material resistance with crack
extension can partially hinder subcritical crack growth. For example, in relaxation tests with coarse-
grained AI20 3 otten v-KI curves with negative slopes are measured /49/. This crack growth
behavior demonstrates that the increase of crack resistance from R-curve behavior is stronger than
the decrease of the crack-driVing force GI, related to the deceleration of crack velocity within the
relaxation experiment. It should be emphasized that GI is a macroscopic quantity which balances
both wake and crack tip resistance.

Evidence for the counteracting influence of R-eurve behavior on crack kinetics also
emanates from SENB crack growth studies under constant load. In such tests the crack velocity
exhibits a V-shape as a function of the macroscopic crack-driving force GI (Fig. 12). Initially the
R-curve effect dominates and the crack v'elocity decreases with crack growth despite the constant
load situation. Eventually the crack propagation is governed again by the typical positively rising
branch of subcritical crack growth. More detailed studies /45,49/ reveal that R-curve effect and
subcritical crack growth act independently and thus can be separated.

The practical implication of these long crack results has to be seen in an extended time to
failure in the case of a pronounced R-curve.

-3.0
-3.5
-4.0
~
E -4.5
E
.S -5.0
>
-5.5
>
.9 -6.0
-6.5
-7.0
20 30 40 50
GI [J/m 2]

Fig. 12 V-shaped subcritical crack growth in an SENB experiment under constant load.

200
3.4.3 Cyclic fatigue

The cyclic fatigue of ceramics has gained increasing interest in recent years because some
of the toughening mechanisms may disappear again by applying cyclic mechanical stresses. The
observed contact shielding of A1 20 3, which gives rise to the favourable R-curve behavior, is also
inherently prone to damage of the briding elements during cyclic fatigue. The macroscopic
mechanical situation is illustrated for a long crack in an SENB specimen in Fig. 13. After controlled
crack growth and load relaxation the specimen is cycled in tension with a maximum load significally
lower than the final load level at the end of the relaxation. After about 50 cycles the crack starts to
grow again indicating that the wake shielding is partially fatigued. Microscopic crack growth
observation reveals considerable side cracking in the reduction of bridging elements /49/.

The long crack results clearly demonstrate that a trade-off exists when AI203 is toughened
by contact shielding. However, it must be emphasized that the fatigue behavior was studied for well
developed wake zones and by changing the crack opening displacement largely. The situation may
be less severe for short cracks and small changes of the crack opening angle. Indeed no significant
fatigue effect was observed with short cracks under tension (R > 0 /54/). However, a decrease in
cyclic lifetime by a factor of about 10 - 100 was measured under alternating stresses ( R = -1 /55/) .

...,100
Z
L..J

-0
o
S 60

20

5 10 15 20 25 :so
Displacement [pm]

Fig. 13 Load displacement curve from SENB test with intermediate unloading/reloading cycles.
AI 20 3 material is prone to cyclic fatigue

4. R-CURVES OF SHORT CRACKS

The long-crack R-curve studies described in the previous sections are useful to gain insight
into the toughening behavior of alumina. Furthermore the ultimate toughening potential after
extended crack growth is recognized. The high toughness values cited for modern structural
ceramics often correspond to these plateau values of long-crack R-curves.

However, such toughnesses are not really relevant for most structural applications,
because the fracture of ceramic components is not determined by cracks of some millimeter length.
Typically crack instability already occurs at much shorter crack sizes. Thus failure-relevant crack
growth studies specifically must focus on the propagation and toughness behavior of natural flaws
and short cracks.

201
 The R-curve behavior Of short cracks, frequently introduced by indentation techniques, has
been studied in detail by Lawn and coworkers. The results are in qualitative agreement with the
long crack observations, i.e. the grain size dependence /23/ and the crack bridging effects /41/ also
hold for short cracks.

To characterize and to analyze beyond that the propagation and toughness behavior of
"natural" flaws, stable crack growth is required again. R-curve behavior satisfies this condition for a
limited amount of crack extension as can be demonstrated by an energy balance between
crack-driving force GI and crack-length-dependent R-curve /52/. The crack instability criteria

GI = Rand dGI / da = dR / da (9)

limit the range of stable crack growth which can be utilized for the measurement of R-curve
behavior with natural flaws. To date only few of these measurements have been reported /53-56/.
Fig. 14 shows a natural surface crack in coarse-grained alumina which was generated on the
tensile surface of bend bars by increasing the load stepwise. Note that the surface crack length is
monitored in situ by optical microscopy. To calculate the toughness using the equation

(10)

both the crack-geometry-dependent V-function and the crack depth a have to be known. With dye
penetrant techniques a semi-circular shape was traced for the surface cracks in alumina /53/.

100 fJm

Fig. 14 "Natural" surface flaw in AI2 0 3 (Note oblique microscopic illumination)

The resulting "natural" crack R-curves are plotted in Fig. 15 together with the respective
curves for the indentation and the long cracks from SENB geometry. The short crack R-curves start
at a considerably lower stress intensity level and crack instability occurs before the plateau
toughness is reached. The low crack initiation toughness of the "natural" flaws is presumably
related to localized microstructural heterogeneities. They either may weaken the material or induce
residual stess fields /57/. Often more than one crack forms. They can all grow but the one with the
shallowest R-curve becomes unstable first, which is in accordance with equation (9).

202
 Similar R-curve results are obtained with short cracks in Mg-PSZ (Fig. 16, 17). Again crack
initiation is observed at much lower stress intensities compared to those where long cracks start to
grow. Again the high plateau value. e.g. Kp = 15 MPa ,Jm, is not reached with "natural" surface
cracks.

90
AlA
80
70 5

5 EXTAAPOlA ED FA"" 'ONG

CRACKS (55'0:8) E
N
5
'>o
E
.....
-,
Q.
L
c5
3 INOE!'oITATION .. STRENG H
ES ILlwn.1 It) 3

10 SUAFACECRACKS ~ 2
..,v
0 500 1000 1500 2cxx)

CRACK LENGTH [.u. m

Fig. 15 R-behavior of short and long cracks. Indentation and strength in bending (ISB) results
from /23/

These differences between "natural" and long cracks are important from the application
point of view. Under technically relevant loading conditions specimens or components obviously
cannot utilize the full potential of the R-curve behavior of ceram!~s. Clearly toughness or resistance
data referring to the plateau value from long crack measurements overestimate the values
pertinent for service requirements.

Furthermore it must be emptlasized that the range of stable crack growth of natural flaws is not
easily recognized in standard loading situations. As the influence of short cracks on specimen
compliance is small macroscopically, despite R-eurve behavior the ceramic often behaves like a
linear elastic material.

5. CONCLUSIONS

The R-curve behavior of ceramics originates from an increasing crack tip shielding during
crack extension. Besides material properties, crack and testing geometry influence the shape of the
R-curve.

In the case of A1 20 3 , which may also serve as a model material for non-transforming monolithic
ceramics, the R-eurve behavior is wake-eontrolled, i.e. interlocking grains form bridging elements
which exhibit sliding friction during separation. The stress-separation function rather than the
macroscopic R-curve is seen as the important material property.

The R-curve behavior of alumina reduces thermal shock damage and hinders subcritical
crack growth but increases (after crack extension) the cyclic fatigue propensity.

203
 Fig. 16 "Natural" surface flaw in Mg-PSl

'<J '<J
'<J
12 '<J

"1
'<J
,........, '<J
:£:1 '<J
E
0
<>-
'<J
•• 0 •
:::0;:
•
.•
'<J
•#
• 0
@O
(}
'<J ,-DCB
• • •,dll0
•• f!T • after relolCotlon
•.f Ii • o during relooding

i~O.
• Jensen, Zelisko, Swain
• ~orsholl. Swoin

58 U8 158 2eg 258 388 358

Crock Length (IJm]

Fig. 17 R-curve behavior of "natural" surface flaws and long cracks in Mg-PSZ

204
Due to R-curve behavior monolithic ceramics are to a certain extent flaw tolerant which is manifest
in an increased load-bearing capacity. However, macroscopically a deviation from brittle fracture
can hardly be recognized because short cracks do not significantly change the overall compliance
of a component.

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1151 M.J. Readey and RW. Steinbrech, "R-Curve Behavior in Transparent MgAI203 Spinel
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205
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/18/ A.O. Ritchie, "Mechanisms of Fatigue Crack Propagation in Metals, Ceramics and
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/19/ A.W. Steinbrech, A. Reichl and W. Schaarwiichter, "R-Curve Behavior of Long Cracks in
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/21/ A.G. Atkins and Y.-W. Mai, "Elastic and Plastic Fracture: Metals, Polymers, Ceramics,
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/23/ P. Chantikul, S.J. Benninson and B.A. Lawn, "Role of Grain Size in the Strength and R-
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/25/ K.S. Roy and R.L. Coble, "Solubilities of Magnesia, Titania and Magnesium Titanate in
A1 20 3", J.Am. Ceram. Soc. 51,1 - 6 (1968)

/26/ F. Deuerler, A. Knehans and RW. Steinbrech, "Testing Methods and Crack Resistance
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/27/ A. Knehans and A.W. Steinbrech, "Memory Effect of Crack Resistance During Slow Crack
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/28/ A. Reichl and RW. Steinbrech, "Determination of Crack Bridging Forces in AI203", J. Am.
Ceram. Soc., 71, C-299-301 (1988)

/29/ KW. White, piivate communication

/30/ P.L. Swanson, "Crack-Interface Traction: A Fracture Resistance Mechanism in Brittle

Polycrystals" in Advances in Ceramics, 22, American Ceramic Society, Westerville, OH,
135 - 155 (1988)

/31/ J. ROdel, J.F. Kelly and B.R. Lawn, "In situ Measurements of Bridged Crack Interfaces in
the Scanning Electron Microscope", J. Am. Ceram. Soc. 73, 3313 - 3318 (1990)

/32/ S. Lathabai, J. ROde I and B.R. Lawn, "Cyclic Fatigue from Frictional Degradation at
Bridging Grains in Alumina", J. Am. Ceram. Soc., in print

/33/ MV. Swain, "R-Curve Behavior in Polycrystalline Alumina Material", J. Mater. Sci. Lett. 5,
1313-15 (1986)

/34/ G. Venkinis, M.F. Ashby and PW.R. Beaumout, "R-Curve Behavior of AI203 Ceramics",
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206
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Distribution, Density and Microcrack Interaction", pp. 835 - 47 in Fracture Mechanics of
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York (1975)

/36/ A.G. Evans and K.T. Faber, "Crack Growth Resistance of Microcracking Brittle Materials",
J. Am. Ceram. Soc. 67 [4], 255 - 60 (1984)

/37/ E. Babilon, K.K.O. Bar, G. Kleist and H. Nickel, "Investigation of Load Induced Microcracks
in Alumina with R-Curve Behavior", Proc. ECERS 1, Vol. 3, pp. 3247 - 3251 (1989)

/38/ A. Quinten and W. Arnold, "Measurement of Elastic Properties During Crack Growth in
AI203-Ceramics", Mal. Sci. Engng. A 122,15 - 19 (1989)

/39/ D. Gross and H. Wagner, "Microfracture" in reference /20/, pp. 90 - 107

/40/ B.S. Majumda, A.R. Rosenfield, W.H. Duckworth, "Analysis of R-curve Behavior of Non-
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Mechanism in Ceramics: II, A Model", J. Am. Ceram. Soc., 70, 289-294 (1987)
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Ceramics", J. Mat. Sci. Letters 9, 1403-1406 (1990)

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in Quasi-Brittle Materials, S.P. Shah (Ed), Kluwer Academic Publishers, Vol. 195 (1990)

/44/ H.E. Lutz and M.V. Swain, "Interrelation between Flaw Resistance, R-Curve Behavior and
Thermal Shock Degradation in Ceramics", these proceedings

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ibid

/46/ Y.-W. Mai, "Crack-Resistance Curve and Cyclic Fatigue in Ceramic Materials", ibid

/47/ D.P.H. Hasselman, "Unified Theory of Thermal Shock Fracture Initiation and Crack
Propagation of Brittle Ceramics", J. Amer. Cer. Soc., 52, 2716-2720 (1986)
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Strip Caused by Thermal Shock," Theorectical and Appl. Fracture Mechanics, 10, 219-226
(1988)

/49/ F. Deuerler, "Influence of Microstructure, Testing Geometry and Environment on the

Fracture Behavior of Polycrystalline Alumina", Ph.D. Thesis, University of Dortmund (1986)
(in German)

/50/ S. Lathabai, Y.-W. Mai and B.R. Lawn, "Cyclic Fatigue Behavior of an Alumina Ceramic
with Crack-Resistance Characteristics", J. Am. Ceram. Soc. 72 [9], 1760-63 (1989)
/51/ T. Fett and D. Munz, "Static and Cyclic Fatigue of Ceramic Materials", Proc. 7th CIMTEC
(1990)

/52/ D. Broek, "Elementary Engineering Fracture Mechanics", Noordhoff, Leyden (1974)

/53/ RW. Steinbrech and 0. Schmenkel, "Crack Resistance Curves of Surface Cracks in
Alumina", J. Am. Ceram. Soc. C 271-273 (1988)

207
/54/ 0.8. Marshall and M.V. Swain, "Crack Resistance Curves in Magnesia Partially Stabilized
Zirconia", J. Am. Ceram. Soc. 71 [6],399-407 (1988)

/55/ G. Dransmann and R.W. Steinbrech, "Toughness of Surface Cracks in MgO Partially
Stabilized Zirconia", Fortschriltsberichte DKG, 5 [1] (1990) (in German)

/56/ 0.8. Jensen, V. Zelizko, M.V. Swain, "Small Flaw Static Fatigue Crack Growth in Mg-PSZ",
J. Mat. Sci. Leiters 8,1154-57 (1989)

/57/ 1. FeU and D. Munz, "A Theory of R-curve Effects for Small Cracks in Ceramic Materials",
to be published

208
UNIVERSAL R-CURVE OF CRACK PROPAGATION

RESISTANCE IN CERAMIC COMPOSITES

Sergej M. Barinov and Vladimir Va. Shevchenko

High Tech Ceramics Scientific Research Centre

Academy of Sciences of the USSR
Ozernaya 48, Moscow, 119361, USSR

ABSTRACT

An analysis of a shape of KR-curves of subcritical crack

propagation resistance in ceramic composites is performed on
the basis of energy concept of fracture mechanics. Two cases of
a broadening of frontal process zone and of crack bridging zone
are considered. The existence of "universal KR-curve" is proved
which is generally described with l' = F(K') relationship, where
l' = liB is the dimensionless crack increment; F(K') is a cer-
tain function of dimensionless increment of stress intensity
factor K'; B is a factor depending on the structure and proper-
ties of a material and characterizing the extent of a subcriti-
cal crack growth. An analytical expression for F(K') function
have been derived and it is shown that as first approximation
"universal KR-curve" can be approximated with parabolic law.
Examples are given for the composites alumina - silicon carbibe
whiskers and lanthanium chromite - chromium as well as for po-
,ous zirconia ceramics.

INTRODUCTION
The toughening of ceramic materials is associated generally
with the increasing R-curves of crack propagation resistance. A
problem that has been already resolved to a considerable degree
is that of predicting the limits of the toughening in composites
with various structures. A review of the level of appropriate
developments is given in 1 . However, the problem of forecasting
shapes of R-curves is also important because it influences the
energy consumption during fracture process and, consequently,
the reliability of a ceramic material. Energy consumption, A,
of material's fracture which shows subcritical crack growth be-
fore the beginning of catastrophic failure is defined as follows
1
A = A
e
+ r c K2 (1)dl/E
J
(1)

o
where Ae is the stored elastic energy; 1 c is the subcritical

Fracture Mechanics olCeramics, Vol. 9

Edited by R.C. Bradt et al., Plenum Press. New York, 1992 209
crack increment; K(ll is the KR-curve; E is the elasticity mo-
dulus. It is evident that at equal values of fracture toughness
K of greater survivability, i.e. of capability to sustain over-
l8ads, will be the material which has greater fracture energy
consumption. The aim of this work is simulation of K -curves
for ceramic composites based on the energy concept o~ fracture
mechanics which has been widely used both for phenomenological
analys~s30f regularities of brittle materials nonlinear defor-
mation' and for simulations of structure influence on brittle
fracture resistance.

MODEL
According to generally adopted opinion,1 increasing R-cur-
ves are conditioned by evolution of .the energy dissipation zone
(process zonel at the crack tip. There are two known basic ty-
pes of dissipative zone: (il a frontal zone which in the pro-
cess of crack propagation turns into a wake zone which shields
a crack tip from external load, and (iil a planar zone of brid-
ges between the surfaces of crack. The first type of a dissipa-
tive zone is inherent to such processes as phase transformati-
ons or microcracking in the applied stress field. A dissipative
zone of second type appears as a result of grain boundary fric-
tion between crack edges, pulling-out fibers or whiskers from
matrix, plastic deformation of metal particles in ceramic matrix
composites. 167
One can assume, according to ' , , that R-curves are con-
ditioned by an increase of dissipative zone size in a process
of subcritical crack propagation. This assumption seems not to
be discrepant for a zone of polymorphous transformations in
such composites as alumina - tetragonal zirconia as well as
for planar zones of crack bridging. For the frontal zone of
microcracking as the other factor determining an increase in
crack propagation resistance can be an increase of energy dis-
sipation density within the pr~cess zone with an increase of
intensity of applied stresses. However, problem consideration
in this work is limited only with approximation of change in
process zone dimensions and constant density of energy dissi-
pation within this zone.
Another assumption is that infinitely small increment of
crack length is conditioned by a change, dK, of stress inten-
sity factor, by its momentary value and depends on the history
of crack propagation. It is also supposed that fracture goes
by way of normal tearing off in conditions of plane deformation.
An energy balance at an increase, dl, of a crack length in
a unit thickness specimen is considered as
dW = dW + dW ( 21
e d
where dW = Gdl is the change in the work of external forces;
G is the work of deformation release rate;

( 31

is the change of elastic stored energy; E is the modulus of

elasticity; v is Poisson's ratio, and dWdcis the irreversible
change of work in the dissipative process.
For the case of the frontal zone one can assume the simp-
lest approximation of a cylindrical shape of this zone, although
a real structure of the zone depends on deformation tensor com-

210
 1
ponents which initiate dissipative processes. In such a case it
can be written that

dW d = wdrddr d (4 )

where w is the density of energy dissipation; r is the linear

size of d the dissipative zone. d
For the planar zone of crack bridging similar relationship
is
( 5)

where h is some characteristic distance in the direction of

action of stresses normal to a crack surface.
From (2) and (3) follows an expression which relates the
stress intensity factor to crack increment:

G = K2 (1 -v 2)/E + dW/dl (6 )
c
Concrete definition of w in the expressions (4) and (5),
d
their substitution into (6) and integration permit to obtain an
analytic description of KR-curves for various dissipative pro-
cesses in the region near the crack tip.

Frontal Process Zone

For a transformation process zone it can be put down:

w = Vs e (7)
d c c
8
and according to
r = (3(1+v )2 /12n )(K/s )2 (8 )
d c
where V is the volume content of a second phase particles which
undergoes phase transformation; sand e are the critical stress
and deformation correspondingly iMducingCphase transformation.
The simil~r structure has also an expression for a micro-
cracking zone. The most important is the fact that substitu-
tion of (7) and (8) into (4) and differentiation gives power
dependence of dW d on a current value of the stress intensity
factor:
(9 )

where c is a coefficient which includes parameters of the ex-

1
press ions (7) and (8).
Substitution of (9) into (6) and integration of the obtai-
ned equation with the aS1umpt~on of invariance G in relation to
crack length (G = G = K (1-v )/E , where K is the critical
stress intensity faBtor)c lead to ~he followIng relationship:

1 = -B ((K 2 _K 2 )/K 2 + In((K 2 -K 2 )I(K 2 _K 2 ))) (10)

1 0 c c c 0
where B is the coefficient depending on parameters of (6), (7)
and (8) 1 and for the case of a transformation process zone is
equal to
2 3
B = c E K /s ( 11 )
1 2 c c c
where c is a coefficient.
2

211
 Expression (10) can be rewritten in a dimensionless form:

l'=F(K') ( 12)
1
where l' = l/B is the dimensionless increment of crack; F(K')
is the function1 of relative change of the stress intensity fac-
tor corresponding to an expression in the rigth part of the ex-
pression (10).
Equation (12) can be considered as a description of "uni-
versal K -curve" of crack propagation resistance in the mate-
rial wit~ an expanding frontal process zone. Plot interpreta-
tion of (12) when K =0 is given in Fig.1.
o

K'

0.5

o 1'
Fig. 1. Universal KR-curve.

According to (10), KR-curves can be described with the use

of only three parameters: B , K and K • So, brittle ceramic ma-
1
terials can be classified not oRl y acc8rding to their threshold
and critical values of the stress intensity factor, but to the
extent of stage of subcritical crack growth which is characte-
rized with parameter B .
Relationship (10) 1 can be simplificated by the way of ex-
pansion into a power series when K-K IK <1. An expression got
" t apprOX1ma
as a f 1rs " t lon
" "1S: 0 c

1 = B ((K-K )/K )2 ( 13 )
2 a c
According to (13), coefficient B has the meaning of a
2
maximum value of subcritical crack increment.

Crack Bridging Zone

For the case of a planar zone of crack bridging it can also

be assumed that

w
d
= Vs e
c c
where V is the density of bridging ligaments in the crack pla-
ne; sand e are the critical stress and deformation correspon-
ding19 in th~ boundaries of this zone. The extent of a crack 9
bridging zone can be evaluated on the basis of Dugdale's model
as:

212
 r = (n/ 16 )(K/s )2 ( 14)
d c
Differentiation of (14) and substitution of the result into
the relationship (5) give

dW = c 3 KdK ( 15)
d
where the coefficient c 3 includes parameters incorporated into
expression (14). Substitution of (15) into equation (6) and in-
tegration lead to the relationship
( 16 )

or in a dimensionless form:
l' = F (K') ( 17)
2
where l' = 1/B and F (K') is a function of dimensionless in-
3
crement of the stress 2 intensity factor. Expansion of a loga-
rithmic function in the right part of (16) into power series
gives approximate relationship
1 = B ((K/K )2_(K IK )2) ( 1B )
3 c 0 c
i.e. a simple parabolic approximation of KR-curve.
To verify nondiscrepancy of the obtained results an analy-
sis of KR-curves for some ceramic materials was performed.

SOME EXPERIMENTAL DATA

Experiments with R-curves for some ceramic materials have

shown that in coordinates R - 1 dependencies can be approxima-
ted with straight lines which is confirmed a parabolic relation
between K an901. A well illustration of this fact are, for
example, §ata where R-curves of alumina ceramics having dif-
ferent grain size were investigated. It is known that increasing
of R-curves in alumina ceramics is due to crack bridging as a
result of action of grain boundary friction forces which prevent
crack opening.
Another interesting example is growing R-curves in alumt~a
- silicon carbide whiskers composites with various porosity.
For such materials an increment of the work, dW d , carried out
while pulling-out whi1~ers from matrix can be expressed taking
into account the data in the following way
( 1 9)

where N is the number of whiskers per area unit of the crack

surface; Idh is the length of debonding of whiskers when pulling
out from matrix; E is the elasticity modulus of whiskers, and
T is the shear str~ngth for whisker/matrix boundary. Substitu-
ti 0 n 0 f (1 9) in t 0 (6) and in t e g ra t ion g i v e

1 = -(n 2 Nl 3 E /6(1- v 2 )EW)(T/S ) 2 F (K') (20)

db c C 2
Fig. 2 shows KR-curves for al~~ina - silicon carbide com-
posites according to data given in in the logarithmic coordi-
nates. Inclination of log K - log 1 lines corresponds to para-
bolic dependence with the exponent of a power near to two. The

213
 0.3

0.0

-0.3
-0.9 -0.6 -0.3 log 1 ( mm )
Fig. 2. The R-curves for composites
alumina - silicon carbide whiskers
with19ifferent porosity (after
Ref. ).

value of the coefficient of the logarithmic expression in equa-

tion (20) corresponds to maximum subcritical crack increment.
As it can be seen from the given data, this crack incre-
ment does not depend on material porosity systematically, and
amounts to 0.12 - 0.99 mm. From the other side evaluation of
the initial size of crack bridging zone with eq~~tion (14) con-
sidering K data and those of strength given in shows values
in the ran~e of 18 - 29 ~m. For a composite with porosity 0.6%
change in the length of crack bridging zone in the process of
5ubcritical crack propagation which can be estimated as ratio
K /K is equal to 1.7. Thus, with the crack length increment
f¥om 0 60 to 500 ~m a size of the crnck bridging zone changes
from 18 to 30 ~m approximately.
To study KR-curves in 60%LaCr0 3 - 40%Cr ceramic/metal com-
posites experiments were performed with three-point bending of
SENB specimens having a thin side notch (curvature radius of
the notch tip was 50 ~m)'1§pecimens were obtained according to
two technological schemes : (i) by high speed (explosive) com-
paction of powder mixtures of components with following high-
temperature sintering, and (ii) by conventional method of cold
pressing with subsequent sintering. The first technology pro-
vided formation of strong bonding between components of compo-
site and a higher level of the mechanical properties.
The tests of notched bars were performed using a rigid
testing Instron type machine with displacement control being
supplied with a high-temperature vacuum furnace.
0
The range of
testing temperatures was from 25 to 1400 C. Diagrams of load
P - deflection d were registered. It was supposed that non-
linearity of P - d diagrams was conditioned by subcritical crack
propagation. In this case the crack increment is interconnec-
ted ~~th the change of specimen compliance in the following
way,

214
where c is a coefficient. Because accord~ng to (13) and (18)
4
the crack increment is propo~~~~nal to~ K , and load change,
~ P, is proportional to ~ K I , then in the case of parabolic
dependence of I on K the following relationship should be ful-
filled

( 21)

Fig. 3 shows in logarithmic coordinates relationships bet-

ween deflection increment ~d = d - d and relative load incre-
ment, ~P'= (P - P )/(P - P ), on th~ stage of subcritical crack
extension, where ~ an§ d ~re the load and deflection at the
moment of crack pr8 pagati8n beginning; P is the load correspon-
ding to transition from stable to unstable crack propagation.
From the data given in Fig. 3 it follows that a slope angle
tangent of diagrams log ~P' - log ~d nearly equals to two. How-
ever, location of the point of diagrams crossing with log d-
axis essentially depends on the technological history and test
temperature of specimens. In particular, from the data of Fig. 3
it follows that for specimens obtained by explosive compacting
higher values of B factor are characteristic.
Fig. 4 shows the results of investigation of cra9§ propa-
gation in SENB-specimens of porous zirconia ceramics. SEM
studies showed that subcritical crack growth is associated with
the process of microcracking. From the data of Fig. 4 it follows
that the slope of the lines corresponds to a parabolic depen-
dence with exponent from 1.5 to 2. Values of B decrease with
the ~ncreasing of test temperature in the range from 1100 to
1300 C due to decreasing of the grain boundary phase viscosity
and macroscopic "embrittlement" of specimens.

log ~ P'
o

-0.5

-5 -4.5 log I::> d

Fig. 3. The dependence of 10~P' on log~d

for cermets LacrOt-Cr. Testing tem-
peratures: 1 -20 o , 2 -1000 0 C, 3 -
0 0
1200 C, 4 -1400 C. Lines 1,4 for
explosive compacted specimen, lines
2,3 for sintered specimen without
explosive treatment.

215
 log liP'
o1------------,,-------,
I /]/.
#
-1

- 6.0 - 5 .0 log r::, d

Fig. 4. The dependence of logll P' on logr::,d

for porous zirconia ceramics.0
Testing temperatures:
0
1 -20 C,
0
2 -1100 C, 3 -1300 C.

Thus, a value of B factor in expressions (10) and (18)

characterizes the extent of the subcritical crack propagation:
at B - 0 the material fails catastrophically at the critical
loading, and at B fracture take place in a fully stable
_0:>

way. One can assume that combination of K and B parameters

characterizes energy consumption during ffacture process.
Transformation of the second term in the right part of
expression (1) considering that dl = Bdl' and K = K K' leads
to the following relationship c

J
1
A = (K B/2E) (K,)2 dl , (22)
F c
o
According to equation (12), integral in the right part of
(22) is a certain constant value A' = const. So,
A = A'BK 2 /2E (23 )
F c
Thus, optimization of composition, structure and technolo-
gy of ceramic materials can be carried out using additional
fracture resistance criteria taking into account the stage of
subcritical crack propagation.

CONCLUSION

An energy approach has been developed as applied to descri-

ption of KR-curves for ceramic materials. In the framework of
this approach it is shown that KR-curves can be approximated
wit h the "u n i v e r sal KR- c urv e " i nth e form

216
 I' = F (K ' )

where l' = liB is the dimensionless crack increment; K' is the

dimensionless increment of stress intensity factor; B is a
structure sensitive parameter characterizing a degree of sub-
critical crack increment. As a first approximation function
F(K') can be approximated with power dependence for the cases
of both a frontal process zone and planar zone of crack brid-
ging. Nondiscrepancy of the results has been confirmed by ex-
perimental data for some ceramic composites.

REFERENCES

1. A. G. Evans, Prospective on the Development of High-Tough-

ness Ceramics, J. Am. Ceram. Soc. 73:187 (1990).
2. M. Sakai, K. Urashima, and M. Inagaki, Energy Principle of
Elastic-Plastic Fracture and Its Application to the Fracture
Mechanics of a Polycrystalline Graphite, J. Am. Ceram, Soc.
66:868 (1983).
3. G. P. Cherepanov, "Mechanics of Brittle Fracture", Nauka
Press, Moscow (1974).
4. B. Budiansky, J. W. Hutchinson, and J. C. Lambropolous,
Continuum Theory of Dilatant Transformation Toughening in
Ceramics, Int. J. Solids Struct. 19:337 (1983).
5. L. S. Sigl, P. Mataga, B. J. Dagleish, R. M. McMeeking, and
A. G. Evans, On the Toughness of Brittle Materials Reinfor-
ced with a Ductile Phase, Acta Metallo 36:517 (1988).
6. S. M. Barinov, Yu. L. Krassulin, Subcritical Crack Growth in
Microcracking Brittle Materials, Strength Problems (USSR)
9:B4 (1982).
7. s. M. Barinov, V. Va. Shevchenko, Crack Bridging and R-Curve
Behavior in Whisker-Reinforced Ceramics, J. Mater. Sci. Lett.
10 (1991) in press.
8. R. M. McMeeking, A. G. Evans, Mechanics of Transformation-
Toughening in Brittle Materials, J. Am. Ceram, Soc. 65:242
(1982) .
9. J. F. Knott, "Fundamentals of Fracture Mechanics," Metallurgy
It Press, Moscow (1978).
10. R. Steinbrech, R. Khehans, and W. Schaarwaechter, Increase
of Crack Resistance During Slow Crack Growth in A1 2 D3 Bend
Specimens, J. Mater. Sci. 18:265 (1983).
11. R. F. Krause, E. R. Fuller, and J. F. Rhodes, Fracture Re-
sistance Behavior of Silicon Carbide Whisker Reinforced Alu-
mina Composites with Different Porosities, J. Am. Ceram, Soc.
73:559 (1990).
12. P. F. Becher, C.-H. Hsueh, P. Angelini, and 1. N. Tiegs,
Toughening Behavior in Whisker-Reinforced Ceramic Matrix
Composites, J. Am. Ceram. Soc. 71:1050 (1988).
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particle Welding, Mechanical Properties and Fracture Beha-
viour of LaCrD -Cr Cermets, J. Mater. Sci. 21 :3901 (1986).
3
14. J. E. Srawley, Plane Strain Fracture Toughness, in: "Frac-
ture, Vol. 4. An Advanced Treatise", ed. by H. Liebowitz,
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ramics", Metallurgy Press, Moscow (1980).

217
SUBCRITICAL CRACK GROWTH OF MACRO- AND MICROCRACKS IN CERAMICS

T. Fett and D. Munz

Universitat Karlsruhe, Institut fOr Zuverlassigkeit und Schadenskunde im

Maschinenbau, and
Kernforschungszentrum Karlsruhe, Institut fOr Materialforschul1g II
Postfach 3640, 75 Karlsruhe 1, FRG

ABSTRACT

The determination of subcritical crack growth data is necessary for lifetime predictions of
ceramic components. In this context, the problem of measuring subcritical crack growth with
natural cracks and macro-cracks is considered. v - K,.curves of subcritical crack growth for
natural small cracks were obtained by a statistical method based on strength and lifetime
measurements in static tests, and for macro-cracks by displacement measurements as well as
observations under the microscope performed on SENB-specimens. It can be stated that the
crack growth law for small natural cracks cannot be derived from measurements of macro-
cracks.

1. INTRODUCTION

Delayed failure of ceramic materials at moderate temperatures can be caused either by

subcritical crack growth governed by the actual stress intensity factor K, or by crack propagation
under cyclic load governed by the stress intensity factor range t:.K Under static or moderately
changing stresses crack growth rate is a function of the stress intensity factor K,
da
(jf= v(K,) (1)

In order to allow correct lifetime predictions to be made the relation (1) has to be known,
especially for extremely low crack growth rates. Different methods of determining the v-K,
curves have been described in the literature dealing with macroscopic cracks on the order of
several mm as well as with procedures relating to small natural cracks. It was shown by several
authors H that the crack growth law for natural cracks is in contradiction with macro-crack
results. It was found that the exponents of the well-known power law relation between v and K,
are lower for natural cracks than the exponents for macro-cracks. Consequently, the lifetimes
of components with small natural cracks cannot be predicted satisfactorily from v-K, curves
obtained with specimens containing large cracks. This holds especially for materials with a
strong R-curve effect. Therefore, it is indispensable to determine the subcritical crack growth
behaviour by reference to small cracks. Especially lifetime methods allow the determination of
crack growth rates down to 1 . 10~12m/s 5.

2 v-K,-CURVE FOR NATURAL CRACKS

All lifetime procedures are based on the general lifetime relation between lifetime t, and
static stress (J

Frat:lure Mechanics oj Ceramics, Vol. 9

Edited by R.C. Bradt el aI., Plenum Press. New York, 1992 219
 (2)

where K,c is the fracture toughness and Kfi is the initial value of the stress intensity factor given
by
(3)

(a; = initial crack size, Y = geometric function). The lifetime relation, eq.(2), allows the v - K,
curve to be determined without special assumptions made on the type of subcritical crack
growth law 5. By differentiating eq.(2) with respect to the initial stress intensity factor K,; one
obtains the crack growth rate at the onset of crack extension

(4)

The necessary variation of Kfi can be generated either by introducing uniform small surface
cracks (for instance by Knoop-indentations) and varying the stress applied or by use of a fixed
stress and making use of the scatter of the natural cracks. For a material with negligible R-curve
behaviour the scatter of the initial crack size is related to the scatter of the inert strength a c by

(5)

leading to

(6)

The procedure of evaluation v(K,) is relatively simple. In a first series of tests N samples
are tested in dynamic tests carried out at high stress rates in an inert environment to give the
distribution of the inert strength a c . The N values of strength are arranged in an increasing
order. In a second series, also involving N specimens, the lifetimes tf have to be measured.
The results are also arranged in increasing order and the lifetime and inert strength for identical
failure probabilities have to be introduced in eq.(4), i.e. log(ala cv ) is plotted versus log(tfv a 2) ,
where \I is the ranking number of the results. Then v(K fi ) is obtained from the slope of this curve.

To be able to apply the procedure it has to be ensured that failure-relevant cracks belong
to the same crack population for inert strength and delayed failure measurements. To satisfy
this condition, the crack origins should be detected with a microscope after the test. This is
difficult especially for A/20 S and other white ceramics. There are two ways to avoid these prob-
lems:

1. Introducing artificial small cracks, for instance cracks created by Knoop indentations,
which are of the same order of magnitude as the natural cracks.

2. A surface treatment involving only rough grinding produces surface cracks. With such a
surface state it can be ensured that all specimens will fail at the surface.

In fig.1 the procedure is illustrated for a coarse-grained hipped 99.6%-A/2 0 S with a mean
grain size of 3.2JLm. This material shows an inhomogeneous grain size distribution with maxi-
mum grains of ~25JLm. Figure 1a represents the inert strength data in a_Weibull plot and fig.1b
shows the lifetimes in static bending tests carried out with several stresses. The auxiliary dia-
gram, fig.1c, where log(ala c ) is plotted versus log(tf a 2) provides the differential quotient neces-
sary in eq.(4). The resulting v - K,-curve is finally represented in fig.1d. The relation between the
crack growth rate and stress intensity factor for these microcracks can be described by

~=AK,n=A",(~)n (7)
dt K/ c

with A· = 6 . 10- m/s, n = 19 and K,c =4MPa.jm (SENB-specimens).

4

220
 217MPa 17310CPa 15510CPa
o 0 0
a b 0
0
o 0

I
0
o 0 0
o 0
eo o
o
o
0 gO o 0
0
0 0
1 o 0 o 0
'-"
'- o
o 0 o 00
0 0
'-" o -1
0
o 0
.E o 00 0
.E 0
0
0 0
-2 0 -2 0
0 0
0 140loCPa
0
0
~
2.40 2.50 2.60 -3 1 100
0.01
log (strength) lifetime (h)
0.0
c d 0

.......
... -6
...... 0
0
cP
00

...
0
.}:

---- ~
0
So
...
-,;J

.!:!
q.. 000 >
oo~ 0

;:
0 0
q, 01 0
C 0
..2 0
E...
0
:...~
,
0
0
.......
c:
o~ -10
O~
01 0
.2 0

-0.5
2 4 6 -.40 .20 .00
log (normalized lifetime) log ( K I / K Ie )

Fig. 1 Procedure of determining v - Krcurves for 99.6%A/20 3 .

(normalized stress = a/a e , normalized lifetime = t f ( 2)

3. CRACK GROWTH BEHAVIOUR OF MACROSCOPIC CRACKS

In order to compare the subcritical crack growth behaviour of small cracks with v-Krcurves
obtained for large cracks, tests were carried out with edge-notched specimens containing
50/Lm saw cuts of 2.25mm depth. The investigation was performed with 3.5x4.5x50mm speci-
mens made of the same hipped 99.6%-A/20 3 as used in fig.1. In a 3-point bending arrangement
the specimens were statically loaded (with a load less than necessary for spontaneous failure)
and the displacement was measured in the center of the supporting roller span by an LVDT.
Due to subcritical crack propagation, the displacement increases with time. The displacement
increments can be recorded with a high resolution, and the change of the compliance then gives
a measure of the crack length increment da. In addition to the calculation of crack length from
compliance, the crack length was measured directly using a travelling microscope. By direct
observation of the crack tip location in longer time steps together with the continuously
recorded displacements in the load line all information is provided which is necessary to
determine v-K-curves. The determination of the crack length is described in more detail for the

221
tests performed with zirconia. Knowledge of the crack depth a allows the actual stress intensity
factor to be computed, and the v-K/ curve is obtained by taking the time derivative of the crack
length 6. In fig.2 macrocrack v - K/ apprcurves for different stresses applied are plotted. In addi-
tion the data of fig.1 are included which describe the micro-crack behaviour. At the beginning
of the static bending test the high crack rates· expected from the natural cracks - occur in all
tests. Then the curves show at first a decrease of the subcritical crack growth rate with
increasing crack length. After little crack extension the crack growth rate drops by several
orders of magnitude. Following a large range with constant crack growth rate the crack exten-
sion accelerates continuously until failure occurs. This behaviour can be explained by the
existence of an increase in the crack growth resistance with increasing crack extension, com-
monly described as R-curve behaviour.

'";) -5
-4.,----------------,
.·w
....... o
E

....
.~ -6 z.~
.& 0 tI

-8
\h~o
~ -9 ~
.......
-0

o
~-10
2'
-11

3 4
K,oPP' (foIPo m'I')

Fig. 2 v-K,-curves for macro-cracks in static bending tests (A/ 20 3) ,

(triangles and dash-dotted line: results of fig.1d).

In materials with R-curve the crack tip is shielded by the shielding stress intensity factor
K/" and the real stress intensity factor at the crack tip deviates from the applied stress intensity
factor K, app/ according to

(8)

The shielding stress intensity factor K/, increases with crack extension, i.e. K/, = f(tla). The
well-known power law of subcritical crack growth can then be written

v = A(K1,tip) n = A[ K{ appl - K{sJ

n (9)

The shielding stress intensity factor as a function of the crack extension can be obtained,
if the crack growth relation without an influence of the R-curve is known. For a first evaluation
it is assumed that the microcrack-curve (triangles in fig.2) is not influenced by the R-curve.

In the schematic fig.3 two K/ apprvalues can be related to one crack growth rate (points A,
and A2 in fig.3) for one specimen. The corresponding K"tfp value is given by point B in fig,3 and
according to eq,(7)

222
 - ~cro croc
-5
- macro-crocI( I
~ -6

-8
//1 /
/. .
//B AI A2
2-10
/
-It /
I

Fig. 3 Determination of the R-curve under subcritical

crack growth conditions (schematical).

DO
,,-.., It.
N
"-
-E 2 DO ,.", ••
DO •
o •• # •
••• ••
0
a..
~
M
• •
:><:
•
.20 .40 .60
0-0, (mm)

Fig.4 R-curves in static bending tests (AI 20 3)

(same symbols as in fig.2).

223
 daldt )1/n
K"tiP = K/ c( ~ (10)

Then K,s corresponding to the crack extension at point A is given by

1/n
dajdt )
K/s = K/ app'- K/ c( A* (11)

Thus, for each macrocrack v - K, apprcurve a K's-t.a-curve can be obtained. Under the assump-
tion that eq.(7) is a correct description of the crack-tip relevant subcritical crack growth law, one
obtains the K's-t.a-curves shown in fig.4. An increase in K,s with increasing crack extension is
observed. The initial Kii has an effect on the shape of the curve. For small values of Kii first a
rapid increase in K,s is observed. For larger values of Kii this first increase is smaller. It should
be kept in mind, however, that K"I;P is not constant for one curve. As a tendency one observes
that the R-curves corresponding to the lower crack growth rates exhibit higher values of K,s.

0.50
---.
Q)
tJ

.~0.40
Q.
E
1 0 .30
<:
o
.~ 0.20
x
Q)

Q)

7i 0.10
E'tJ
0.0~:::"-_-,lLO""--~.2l...0---.3"J..O""---.4'-=O-----:!.
50
crack extension (microscope)

Fig. 5 Crack length determined from compliance and microscope measurements 7 •

3.2 Determination of v-K,-curves for zirconia

A second evaluation procedure is based on curve-fitting and will be demonstrated for a

measurement on a ZrOz-ceramic. Tests were performed with specimens made of a PSZ-cer-
amic: (ZN40, ZrOz-MgO, Feldmilhle AG, Plochingen, FRG). Bending bars of thickness W=4.5mm,
width B = 3.5mm and length L = 50mm, containing a saw cut of 50Jlm width and a;::<2.2mm depth
were statically loaded in a 3-point bending arrangement. From the time-dependent displace-
ments measured in the center of the supporting roller span the time-dependent compliance was
determined. The change in compliance gives a measure of the crack extension. Additionally, the
actual crack depth has been determined using an optical microscope. The compliance method
is not restricted to the specimen surfaces and yields a mean value of the crack length which is
representative of the whole specimen thickness. A further advantage is that the compliance can
be determined with a very high resolution and results in a continuous curve which is appropri-
ate for taking the time derivative.

224
 The procedure used combines the two methods. Direct observation of the crack tip location
together with the continuously recorded displacements in the load line results in a calibration
curve (fig.S) where the crack extension ~a obtained with the compliance method is plotted
versus the optically measured crack extension. The dotted lines are used to calculate the real
crack depths from the results obtained with the compliance method.

In order to provide a large number of optical crack length measurements it is recommended

to apply a preload for some hours. Under this preload no crack can be observed but time-de-
pendent phase transformations 8 become partially saturated. For the measurements represented
in figs.S and 6 about 90% of the envisaged main load was applied in the preload phase. During
the main test conducted under full load it was possible to follow the crack tip very easily with
the microscope. In contrast, tests without preloading exhibited spontaneous crack increments,
and only a few optically measured crack length data were obtained. In fig.6 the crack length is
represented as a function of time, and the v - K, app' -curve - resulting from the time derivative
- is shown in fig.? This curve exhibits the same features as the v - K,apprcurves obtained for
Alz0 3 (fig.2).

0.60

E
E
'-"040
c
o
'in
.,c
x
.: 0.20
<.>
o
'-
<.>

0.0~----:-2----4.L------c!6:------!8

time (h)

Fig.6 Time-dependent crack propagation in a static 3-point bending test '.

In order to obtain the v - K"tip"relation as well as the R-curve K,s = f(~a). two different set-
ups were made for K,s. A first possibility to describe the R-curve is given by
K/ s = K,s,max[1 - exp( - C~a)] (12)

An additional relation was used as proposed in 6

K _ {Kls,maX[2c~a - (C~a)2J for ~a:s: 1/C}

(13)
Is - K,s max for ~a > 1/C

In principle, one single v - K,apprcurve as shown in fig.? contains sufficient information to

determine a set of parameters (A,n.K's,max,C) by a least-squares procedure. Figure 8 shows once
more the v - K,app, data for ZrOz together with the fitting curves according to eqs.(9),(12) and
(13). The solid line is obtained by application of eq.(12) and the dotted line by use of eq.(13).

225
 -5.----------------,
Z
E -6 ZrO:! •••
.= • •
....
:. . .
•

-8
... It;
• •
a•
•

Fig. 7 Crack growth rates obtained from fig.5.

-5,r------.-------,--
Z
E -6

a-:u"" -7
.:;!.

-8

-10'--------'----'---::,-------'
4

Fig. 8 Crack growth rates compared with least-squares fits

(solid line: eq.(12), dotted line: eq.(13))

226
 2.50

--.2.00
~
-E
o 1.50
a..
3
1.00

0.50

. ..J.40=-----."!-60=--
0.0~=-0----.~2=-0----

a-a j (mm)

Fig. 9 R-curves according to the set-ups eq(12)

(solid line) and eq.(13) (dotted line)

The two straight lines describe the relations v - K',tip. As can be seen, the subcritical crack
growth curves depend on the prescribed R-curve formulation. From this point of view a single
static test cannot provide enough information for a complete characterisation of subcritical
crack growth in materials with R-curve behaviour. Figure 9 finally represents the two R-curves
obtained by the least-squares procedure.

4. INFLUENCE OF R-CURVE ON THE v-K,-CURVE FOR NATURAL CRACKS

The method of determining the v-Krcurve by lifetime measurements (Section 2) works

without problems for materials without R-curve behaviour. For materials with a rising R-curve
the lifetime t, as well as the inert strength (Jc may be influenced in principle. Therefore, one has
to check how much R-curve effects will distort the v-K-curves resulting from the procedure
described before. In order to study the influence of R-curve effects on the v-K,-procedure, the
R-curves of figA were abstracted by the straight lines shown in fig.10 that represent the "mean
R-curve". A change of the R-curve with initially applied stress intensity factor will be neglected
below. The dependency of fig.10 can be described by the three equations

12.5 MP~~ ~a for ~a < O.08mm }

K/s = MPajrn r=- (14)
2.875 mm ~a + O. 17M Pa-v m for O.08mm < ~a < O.6mm
{
2.495MPajrn for ~a > O.6mm

The v - K,-curve is obtained from lifetime and strength measurements by use of eqs.(4) and (6).
In order to demonstrate a possible influence of the R-curve, it is necessary to calculate the
lifetimes and strengths for macro-crack R-curves.

Strength: The critical crack size in case of stable crack growth ac and, consequently, the critical
stress (Jc (the strength) result from the two conditions

(15)

resulting in

(16)

227
 ---..
2.50~ ~
S 2.00- ••
to
~ 1.50
•
~

•
'-'

•
•
.20 .40 .60 .Be
0-0·I (mm)
Fig. 10 "Mean R-curve" from fig.4.

1000
..
t
:>
0
I
0::
I
£
"i I I
0'
n..
~
..<:
100
H
0>
l:
...
CD

ii;

10
10 100 1000
strength (MPo) without R-curve

Fig. 11 Influence of the R-curve eq.(14) on the strength (K fC =4MPaJiTI).

228
 In fig.11 the strength in the presence of an R-curve effect - described by eq.(14) - is plotted
as a function of the strength which results in the absence of any R-curve behaviour. It becomes
evident that low strength values increase due to the R-curve effect. For the special R-curve of
eq.(14) strength values less than 260MPa are affected. A somewhat stronger R-curve effect
would have an influence on the strength data reported in fig.1a.

Lifetime: The lifetime t, in a static test performed with the stress a results in

(17)

where ai is the initial value of the crack length a and ac is the crack length at failure. Under
subcritical crack growth conditions the crack size at failure ac can be derived from the failure
condition Kf=KfO(=Kfc) resulting in

(18)

Using the mean R-curve for subcritical crack growth, eq.(14), the lifetimes were calculated
with n = 19 for a mean strength of ac = 360MPa as measured for A/20 3 (fig.1a). The results are
shown in fig.12. Due to the R-curve behaviour of the macro-cracks the lifetimes deviate signif-
icantly from the values obtained under the assumption that subcritical crack growth of natural
cracks is free of R-curve effects. Crack arrest occurs at a = 75MPa. Within the range of exper-
imentally applied stresses the slope of the lifetime curve is obviously reduced which leads to
an apparent exponent n'~28. On the other hand, if we assume that the measured n-value of 19
is already influenced by an R-curve effect, we obtain for the uninfluenced law an n-value of
n' = 13.
The computations - leading to fig.12 - were repeated once more with a power law exponent
n = 13. Within the range of applied stresses the apparent n-value then becomes n'~19. Figure
13 represents the auxiliary plot log(a!acl VS. log(t,a 2) with strength data in the experimentally
obtained range of 265-425MPa. Whilst each single curve (approXimately described by a straight
line) yields an n-value of about n = 13 the regression of all data again yields an n-value n'~19.
In both cases - namely occurrence of an R-curve effect or absence of such an effect - the same
overall n-value would be obtained for the two representations, fig.12 and fig.13. An indication
of an R-curve effect may be the deviating n-values for a single-curve evaluation (fig.13) and a
total evaluation of all curves.

strength
2.50

... wi hout R-curve

2.00

crock arrest

-20 -10 o 10 20 30
log(lifetimejA)

Fig. 12 Influence of the R-curve, eq.(14J, on the lifetimes in static tests (n = 19).

229
 0.00,-----------·------------,
217MPa
,.....
1Il 73MPa
...'"
<l>
iii -0.20 --- 155 Pa
-0
<l>
N - 140 iPa
o
E
...
0-0.40
-S
0>
!2

-0.6Q.L,,6-----_-L.,------....i_"'"2-------;0
4
log(normalized lifetime/A)

Fig. 13 Auxiliary diagram according to fig.1 computed with n = 13.

+ [median valuesl
250
o CXJDl 0 (Q)
0'
0....
200
::::l':
........ 00 0>
1Il

'"
~ 150
o 00 <Em
000
'"

100 ' - - - _ - - - L_ _- ' -_ _- ' -_ _--'-_ _- ' - - - _ - - '

0.01 100

Fig. 14 Experimental data according to fig.12.

230
 O.OOr----------------------,
o 140 MPo

,..... o 155 IPo

1Il
1Il
Q)
• 173 MPo
I..

iii -0.20 • 217 MPo

"'0
Q)
N

o o
E
I..
o

~o
C
'(;; -0.40
o

2 4 6
log ( normalized lifetime)

Fig. 15 Experimental data according to fig.13

(normalized stress = (1/(1e, normalized lifetime = (,(12).

Table 1.
Exponents of the power law, eq.(7).

(1 (MPa) n
217 14.6
173 11.9
155 15.6
all data 19.2

231
 ..
•
-6- ••
•
J
0>
o
···0• ·
o
o~<1
-10 .f"-"
o~

.40 .20 .OC

log ( K I / K Ie )

Fig. 16 V - K,-curve of fig.1d, separate for different stresses applied.

The experimental data entered in fig.1 may now be analysed once more in detail. In fig.14
the mean lifetimes resulting from fig.1 b are plotted in a 10g(l1) vs. 10g(t,I1 Z) diagram according
to fig.12. Due to the well-known proportionality t, ex: l1- n , the regression line yields an n-value
n=19.5.

Figure 15 shows once more the auxiliary diagram from which the derivative for eq.(4) is
obtained. The n-value can be determined from the slope that is proportional to -1/(n - 2). A
least-squares fit of the single curves as well as of all the data yields the exponents entered in
table 1. This result is an indication of the occurrence of curves like those plotted in fig.13. But
a number of 12-16 specimens in each test series does not seem to be sufficient.

5. OUTLOOK

As shown in Section 4, there are indications that in coarse-grained A/z0 3 • exhibiting a

strong R-curve effect in specimens with macrocracks - also lhe natural cracks are influenced.
The aim of future work will be to determine the R-curve effect and the v-K,-relation for natural
cracks. In principle, the experimental data of fig.1a,b contain all information which is necessary
to determine both the R-curve and the v-K,-curve. One possibility of evaluation will be proposed
below:

1. At the beginning of the procedure a least-squares routine provides a set of parameters

A,n for a power law description of subcritical crack growth and S,C for a two-parametric
R-curve description (for example eqs.(12,13)).

2. For each strength value I1 cv of fig.1a the related initial crack size aiv is determined from the
failure conditions in strength tests

K,app/=l1cvYJB;; =KIO+K/sl acv -aIV

OK/ apPI ) = dK/ s (19)

( aacv d a cv
cr=const

3. a. Calculation of the final crack length ac in a constant load test analogous to the first
of eqs.(19).
b. The initial crack sizes are introduced in the lifetime relation

l
ac
1 da
tf calculated = A r::: n
[I1Y -va - Kts ]
ai

232
4. The calculated lifetimes are then compared with the measured ones and the sum of
squares is determined as
2 2
5 = L( log t, calculated - log t'measured) (20)

5. In the next step the parameter set is changed systematically and the procedure starts
again from point 1 with these new parameters.

6. The procedure is repeated as long as the squares 5 z get minimum.

The result is the best parameter set for description of the v-K{-curve and R-curve, depending
on the chosen type of relations. An appropriate least-squares computer subroutine is, for
instance, the Harwell routine VA02A.

6. CONCLUSIONS

The main topic of the report is the comparison of subcritical crack growth data determined
with natural cracks and macroscopic cracks for materials with R-curve effects. Measurements
on bending specimens of a 99.6%A/zOs-ceramic with natural and macroscopic cracks and with
a ZrOz-ceramic were carried out in static bending tests. The main results are:

• The macro-v-K-curves v = f(K, ""p{) initially show a decreasing subcritical crack growth rate
with increasing stress intensity factor applied. For large crack extensions the crack growth
rate then increases and the specimen subsequently undergoes failure.

• For A/zOs the R-curves were determined as K{,=f(6a). Monotonically increasing curves
were found.

• Modelling the R-curve by simple expressions allows the related parameters and the
v=f(K{)-relation to be determined.

• The comparison of the small crack v-K-curves with the macro-crack results shows that it
is not sufficient to characterise the crack-growth behaviour of a ceramic material by
macro-crack data. Besides, also lifetime measurements obtained with natural cracks in
A/zOs indicate an influence of R-curve effects.

• A useful treatment to determine subcritical crack growth behaviour should combine

• a small number of static tests with macrocracks in order to prove the existence of an
R-curve behaviour with

• a large number of static lifetime tests with natural cracks in order to determine the
natural crack v-K{-curve and the natural crack R-curve.

• Finally a procedure is proposed that allows the small crack v-K{-curves to be determined.

7. REFERENCES

1. T.E. Adams, D.J. Landini, C.A. Schumacher, B.C. Bradt, Ceramic Bulletin 60:713 (1981).
2. B.J. Pletka, S.M. Wiederhorn, J. Mater. Sci. 17:1247 (1982).
3. K. Chen, Y. Ko, Amer. Ceram. Soc. Bull. 67:1228 (1988).
4. T. Fett, D. Munz, J. of the European Ceram. Soc. 6:67 (1990).
5. T. Fett, D. Munz, Commun. of the Amer. Ceram Soc. 68:C213 (1985).
6. T. Fett, D. Munz, Subcritical crack growth of macro-cracks in alumina with R-curve-beha-
viour, submitted to J. Amer. Ceram. Soc.
7. T. Butz, Measurement of crack growth in zirconia (in German), Internal Report, Karlsruhe
1991.
8. R. Steinbrech, these Proceedings.

233
R-ClJRVE AND FATIGUE BEHAVIOR OF
GAS PRESSURE SINTERED SILICON NITRIDE

Kazuhiro Urashima, Yo Tajima and Masakazu Watanabe

R&D Center, NTK Technical Ceramics
NGK Spark Plug Co., Ltd.
2808 Iwasaki, Komaki, Aichi, 485 Japan

ABSTRACT
Fracture resistance and fatigue behavior of two kinds of gas
pressure sintered silicon nitride ceramics were studied.
Indentation fracture, indentation strength and indentation and
crack growth measurements, that are very useful to evaluate
fractures from small cracks, were carried out to characterize
crack growth resistance. The results indicated that the crack
propagation resistance (R-curve behavior) is distinctively
different between the two materials. From the observation of
crack extension path, it was considered that the R-curve behavior
is due to the grain bridging of elongated p-Si 3N4 grains.
Fatigue behavior of the two materials was also investigated
under cyclic loading by 3-point bending for the specimens with
Vickers indentation-induced flaws. The relationship between
maximum stress intensity factor and crack velocity, i.e. Khu-V
diagram, was obtained by measuring crack lengths as a function of
numbers of cycles. The fatigue behavior of the two materials was
also different. A material that exhibited pronounced R-curve was
more susceptible to the fatigue crack growth as K1max approached
KIT' It was observed that the damage by the cyclic loading was
caused by the fracture of the grain bridging behind a crack tip.

INTRODUCTION
Recently silicon nitride ceramics with high fracture
toughness in excess of 6MPamO. 5 have been developed. These
materials are expected to exhibit high reliability and flaw
tolerance and to be used as structural components such as heat
engine and gas turbine engine parts. 1,2 In the recent studies, it
has been reported that some ceramic materials exhibit an
increasing crack extension resistance, i.e. R-curve behavior.~12
Maniette et al. 7 studied the R-curve behavior of a gas pressure
sintered silicon nitride and observed a marked increasing R-curve
for a straight through crack. They concluded that the toughness
improvem~nt of the silicon nitride ceramics arises from the crack
bridging of the intact grains.

Frocture Mechanics o/Ceramics, Vol. 9

Edited by R.C. Bradt et al., Plenum Press, New York, 1992 235
 Indentation strength method has been used to e\Taluate the R-
curve behavior for small cracks. 8-11 Since stress intensity factor
due to residual stress around the indentation-induced crack has
a tendency to decrease wi th increasing crack length, a steady-
state crack growth is possible to take place. Krause et al. 1Z have
reported the R-curve behavior of silicon carbide whisker
reinforced alumina using the indentation-strength method and they
conclude that the toughening is results of aggregate interlock and
whisker pullout which develop in the wake of the crack tip.
On the other hand, it has been known that some s i l f con
ni tride ceramics undergo the damage by cyclic loading .13-15 The
authors have investigated the fatigue behavior of a gas pressur~
sintered silicon nitride using the specimens wi th and wi thout
artificial flaws under cyclic loading. As the results, it is
revealed that the specimens with precracks showed enhanced fatigue
behavior by cyclic loading compared with the specimens with
natural flaws .16,17
In the present study, the R-curve and fatigue behavior of two
kinds of gas pressure sintered silicon nitride wlth different
fracture toughness were evaluated to elucidate whether the
correlation between them does exist.

EXPERIMENTAL PROCEDURE AND ANALYSIS

Materials

Two kinds of gas pressure sintered silicon ni tride designated

as A and B were used in this
with the additions of MgO and
with the same amounts of MgO
the further addition of Al z0 3 •
materials are listed in Table
between the two materials but
study. Material A was fabricated
ZrO z, and material B was fabricated
and ZrO z as in the material A with
Some mechanical properties of the
1. Fracture toughness is different
other properties are almost same.

Table 1 Mechanical properties of the materials

Material Density Vickers Young's Bending Fracture

Hardness Modulus Strength Toughness
( g/cm 3 ) (GPa) (GPa) (MPa) (MPa. mO. 5 )
A 3.26 14.0 320 750 6.0
B 3.25 14.5 320 770 4.1

Microstructure Evaluation

Microstructure evaluation was carried out in an attempt to

quanti ta ti vely compare the two materials. Specimens were polished
and etched with phosphoric acid, and the scanning electron
micrographs were used to measure the size of each grain. 18

236
R-curve Measurements

Three measurement methods described in the followings were

carried out to characterize the R-curve behavior for specimens
with indentation-induced cracks.

Indentation fracture method(IF). In this test, indentation

was made onto the polished surface with indentation loads, P
ranging from 1 to 294N for 15 sec in air using a commercial
Vickers hardness tester. The indentation-induced crack lengths,
2c were measured with the precision of ±l p m using optical
microscope of 400 magnification. The fracture toughness Kc was
calculated using the following expression proposed by Anstis et
al. ,9

(1)

where E and H are the Young's modulus and the Vickers hardness,
respecti vely, and §v is a material- independent constant for
Vickers-produced radial cracks and §v=O. 016 was used in the
present study.

Indentation and crack growth method (ICG) . Specimens for this

test were cut off from a 40 by 40 by 15mm block and ground to
rectangular bars in dimensions of 3 by 4 by 40mm with a 140-grit
diamond grinding wheel. The tensile surface was polished to
remove a residual stress due to machining and to produce a finish
for optical microscopic examination. A Vickers indentation with
a load of 49N was made at the center of prospective tensile
surface of eaeh test piece. The test was conducted in 3-point
bending wi th a span of 30mm. The specimens were applied a
specific stress with the cross head speeds of 0.05 mm/min, and
then were unloaded after keeping 5 minutes. The crack length was
measured by optical microscope.
The crack growth resistance parameter, KR, was calculated by
modifying the method proposed by Krause et al. 12 Suppose the
equilibrium condition for crack extension is that K=K R• The net
stress intensity factor K for this system is

(2)

where Kb and Kr are a bending stress intensity factor and residual

stress intensity factor due to the indentation, respectively. The
two stress intensity factors are expressed by the following
equations:

(3)

and

(4)

237
where Y is the shape factor and o. is the applied stress.
In this system, stable crack extension is possible to occur as
long as the following condition is satisfied.

dK dK
- < -R (5)
dc dc

Therefore, if the crack length are measured for different applied

stresses in an iterative loading. the R-curve as a function of
crack length is possible to be obtained. Typical changes of
stress intensity factor according to this theory are shown in Fig.
1.

.
E 9,-------------------,
'"
~8 ,, , fI.MlI
~ 7 , ....... - ... - 300
<56
~~~:::::::::==----
_~~=~=~~~=======~_ 250
,;:<::--=:---- ------------------
U 5 ,:::;,,,, ... '_ ... _ --- 200

ii
$
~4
K., 150
.~ 3

.s 2
(l)

<, "';;;;;;;;,jf;;;:::;;;;::=;;=;
~ 1
~o
en 100 150 200 250 300
Crack length c p. m

Fig.1 Stress intensity factor as a function of crack length.

Dashed lines are calculated K according to Eq.(2) for
various o. shown right. A solid line is an example of KR
curve obtainable by the ICG method between the initial
crack length (c r ) and the crack length at the
instability point (c T ).

Indentation strength method(IS). Indentation strength

measurements were made using the same specimens as in the ICG
method wi th indentation loads in the range of 1-294N. The
strength of the indented specimens was measured by 3-point bending
with the cross head speed of 0.5 mm/min. The strength data of
specimens that fractured from the indented sites were used for the
subsequent R-curve analysis 12 described as follows. In this
analysis. it is assumed that KR is given by an equation of the
power law model expressed as:

(6)

where Ko • Co and m are constants. Then, the relation between the

strength 0 and the indentation load P is given by:

238
 (7)

where

(8)

(9)

Details of the analytical procedure to obtain the constants are

described by Krause et al. 12

Cyclic Fatigue Test

Cyclic fatigue tests were also conducted using the same
specimens for the ICG method. All the testing were conducted in
3-point bending at room temperature in ambient air using an
electrohydraulic testing machine. In the cyclic test, the
specimens were subjected to a sinusoidal cyclic stress wi th a
frequency of 10Hz and a stress ratio of 0.1. An iterative process
of loading and measurement of surface crack length by optical
microscope of 400 magnification was made to estimate the crack
propagation velocity. The crack configurations were determined
for the fractured specimens which had been treated by a dye
penetrant.

RESULTS AND DISCUSSION

Microstructural Evaluation

The SEM photographs of microstructure are shown in Fig. 2.

The quantitative evaluation of microstructure was made by
measuring the thickness, d and length, I of each grain on the
micrographs and by calculating the two-dimensional aspect ratio,
lid. The average thickness of the material A and B was calculated
to be 0.431!m and 0.33l-lm. respectively. Distributions of the
thickness and aspect ratio are shown in Fig. 3. These results
indicate that the microstructures of the two materials are
similar.
R-curve Behavior

Indentation fracture. The fracture toughness of each

indentation load was calculated according to Eq. (1). and the
results are shown as a function of crack length in Fig. 4. For
large crack length, the toughness of the material A is higher than
that of the material B. The toughness becomes lower as the crack
length gets smaller. and the two materials would exhibit a similar
toughness value when the crack length is extrapolated to zero.

239
 Fig.2 Microstructure of materials A and B etched by
phosphoric acid.

-
50
.t-
~A
40
DB
>-
g 30
QI
~

g-... 20
ll..
10

<.1 -.2 -.3 -.4 -.5 -.6 -.7 -.8 -.9 - 1 1 >
Thickness I urn

o 6 0 . - - - - - - - - - - - - - - - - -.....
~
~A
- 50
DB
~ 40
c
QI
~ 30
CJ
ell
It 20

1-2 2-3 3-4 4-5 5-6 6-7 7-8 8-9 9-1010>

Aspect ratio

Fig. 3 Distribution of thickness and aspect ratio.

240
It must be noted, however, that the crack has to be a radial crack
when applying Eq. (1) in this method. Although observation of the
fracture surfaces was conducted by using scanning electron
microscope, it was not possible to determine the crack
configuration for the smaller cracks.

7,------------------,
~
d
6 A
~ 5 ••••••• ------e------.
~ e •• '
~ 4
~ 3
.
~
~

y'~.--.---------- .. ----------~---------.
B

100 200 300 400

Crack length c Jl m

Fig.4 Fracture toughness as a function of crack length

measured by the indentation fracture method.

Indentation and erack growth. By the indentation and crack

growth method, it is possible to obtain the stable crack growth
wi thout fai lure. In order to calculate the crack extension
resistance, KR , using Eqs. (2), (3) and (4), the crack depth, a
needs to be obtained. As it was not possible to measure the crack
depth non-destructively, the crack dimensions, a and c, were
measured for the fractured specimens. The results are shown in
Fig. 5. These results suggest that an aspect ratio of crack, a/c,
is independent of the crack length wi thin the measured range
between 80 and 140~m, being about 0.8. Therefore the crack depth,
a, was estimated by multiplying the surface crack length c by the
aspect ratio. The value of Y was then calculated according to the
Raju-Newman's equation 19 for semi -ellipsoidal crack in the bar
bending. As the variation of the calculated Y values was
small(Y=1.24-1.28), Y was set to be a constant, Y=1.25, in this
study. The calculated crack resistance, KR , as a function of the
crack length, c, for the two materials is shown in Fig. 6. It
shows that the material A exhibits more pronounced R-curve
behavior and higher KR value and that the KR values for large
cracks are in agreement with the Krc values by the SEPB method.
Indentation strength. Fig. 7 shows plots of the logarithm
of the strength vs the logarithm of indentation load for the two
materials. The strength data of specimens fractured from natural
flaws are indicated by a bar at left side of the figure. The
dashed lines are drawn by the least square method, according to
Eq.(7). The slopes of these lines for the materials A and Bare
-0.228 and -0.293, respectively.
Fig.8 shows plots of c vs. P which were used to obtajn the
constants, Co and Po· The other constants, Ko and x' were also
calculated according to the analysis reported by Krause et al. 12 ,
and the obtained constants are summarized in Table 2.
The R-curves for the two materials were then obtained by
using Eq. (6) with the calculated parameters and are shown in Fig.
9. The results are similar to those by the IF and leG methods;
more pronounced R-curve behavior and higher KR value for the
material A.

241
 200 . - - - - - - - - - - - - - ,
E
::s.
150
o
.c
'5c>
.3 100
:£
o
e!
u 50
~
~
:J
en
o0~------::50':---1~00-:--...,1c:::50-:---=2OC
Crack Depth a fJ m

Fig.5 Relationship between indentation surface crack length,

c, and crack depth, a. The dashed line is the least
square fit.

~
d
6 ...; .
.-.--y--- •
A

E 5 -
til
CL 4
-.- - -,.-
...... - ...
- .... - _
B
~
II: 3
.... '
_
..
~
2 -

80 100 120 140 160

Crack length c fJ m

Fig.6 Crack resistance curves by the ICG method.

242
 Table 2 Values of constants for the IS method

Material Po Co Ko X m
A 1.365 8.07 4.30 0.085 0.129
8 1.147 9.52 5.38 0.13 0.047

l,ooor------------,
800 .
......... A
.
8!. 600
'I •
::;; ...............

..
-5 400
Ol ... t: .......
C
0> " ,
~ 200

'lMb., 1 5 10 50100 SOIl

Indentation Load N
1,000,-----------,
600
B
8!.600

....
::;;400
-5 ,
Ol
c
~200 't ...
(f)
',.
100 l..------'----:'-:":----:::cc-::-:----=-=-=...J
0.1 1 5 10 50100 SOIl
Indentation Load N

Fig.7 Indentation load vs bending strength plot for the

materials A and B. The dashed lines are the least
square fits and the solid lines indicate the slope
of -1/3.

Comparison of the three methods. SEM photographs of the

indentation-induced crack paths are shown in Fig. 10. The crack
path of material A is very tortuous and many grain bridgings were
observed as shown by arrows. On the other hand, the erack path
of the material B is relatively straight. From these reslll ts, the
toughening mechanism of the material A is thought to be the grain
bridging.
The three methods indicate the similar R-curve behavior for
the two materials; the material A has more pronounced R-curve than
the material B. However, the KR values are different among these
methods. In the indentation method, the fracture toughness was

243
 3
B
2.5 , ......
~.

A
2

.. .,-
~ .'
e 1.5
OJ '
.2

0.5

0
-1 o 2 3

Fig.8 Indentation crack length, c, as a function of

indentation load, P, for the two materials. The
lines are the least squares fit for the data.

8,------------------,
A

8
4

3 L-----:-:l00:=----:2~OO::----~300:=----:4~OO::----'

Crack Length 11 m

Fig.9 Calculated R-curves from the indentation strength

measurements.

244
lower than that of others. The indentation crack is introduced
by a specific stress field and it has relatively fast crack
extension velocity. It is considered that the crack shielding of
the indentation crack is less than that of others. The
indentation strength method resulted in the highest value of KR
among the three. Although the magnitude of KR is very sensitive
to the constants. Co and Ko • it seems difficult to accurately
estimate the constants since these constants are very much
dependent on the strength data. The KR value of ICG method was in
a good agreement with the SEPB method. This method has an
advantage that the R-curve is characterized with fewer specimens
and in shorter time compared to other methods.

Fig.l0 SEM photographs of indentation crack paths.

Crack Propagation Behavior

The crack propagation behavior under cyclic loading for the

materials A and B is shown in Fig. 11. The applied stresses were
about 80% of the fracture stress at first. and then changed to a
lower stress for material A and to a higher stress for the
material B. The results show that the crack propagation behavior
are different between the materials. The material A is shown to
be more fatigue susceptible under cyclic loading. To study the
effect of static loading, a test under static loading and
subsequent cyclic loading was carried out for the material A. The
result is shown in Fig. 12. The stress was 279MPa for the static
loading and the maximum stress was 266MPa for the cyclic loading.
The crack stagnated during the static loading, and propagated
under the cyclic loading even though the maximum stress of the
cyclic loading was lower than the stress for the static loading.
The result clearly indicates that the material A is damaged by the
cyclic loading more than by the static loading.
The crack propagation velocities was estimated from slopes
of the curve obtained by smoothing the data points. zo The stress
intensity factor at the surface crack tip (K hu ) was calculated by
the same method as in the ICG test. The value of Y was calculated
according to the Raju-Newman' s equation 19 for semi-ell ipsoidal
crack in the bar bending. The aspect ratios of cracks were
0.7 and 0.8 for materials A and B. respectively. According to the
above mentioned method, the K1oax-V diagram for the two materials
was obtained as shown in Fig. 13. It shows that al though the
material A has higher fracture toughness than the material B, it
exhibits the enhanced crack propagation under the cyclic loading
in the higher Krm • x region. This resul t suggests that the fatigue
behavior under cyclic loading is closely related with the R-curve

245
 1,000,.-------------,
e 900 111M?' IllM?, I A
~ 800

-= 700
g' 600
~ 500
-4-1~ ;
~ 400
o 300
200L_-"--
100
o0L..-----'20---4Q-'::-----:60:---a:':0:----::100
Number of cycles x10'

500 , . - - - - - - - - - - - - - - - ,
e B
.. 400
.s::
c;,
! 300 I~IIIII_IIP'
~200
U ",. ..
100 po- ...

20 40 60 80 100
Number of cycles x1 0 4

Fig.ll Crack propagation curves under cyclic loading for the

two materials. The tests were conducted under two step
loading. The values in the figure show the applied
stresses.

246
 500 , - - - - - - - - - - - - , - - - - - - - - - ,
Static loading Cyclic loading
279MPa max266MPa
400
E
::t

_....--~I
.r: 300
"6l
c
.3 200
13 ......
~ 100
u
o LO-----'-2--4--J....S---a--.l..o--J....20-----'4-0--'SO

Time x10 4 sec Number of cycles x10 4

fig.12 Crack propagation curve under static loading and

subsequent cyclic loading for the material A.

lE-oS

Cl>
A
"5 lE-07
>-
.g
E
lE-08
>
~
·u lE-09
0
Q)
>
""u<1l... lE·lO !'"
U

B
lE·ll
•
lE·12
3 4 5 S 7 8
K Imax MPa· rTf I

fig.13 Khu-V diagram under cyclic loading.

247
behavior and the toughening mechanism. It was pointed out in the
previous section that the crack propagation resistance would be
enhanced by the crack bridging by the elongated Si 3N4 grains. In
turn, it is likely that the damage for the material A by the
cyclic loading was caused by the fracture of the grain bridging
behind a crack tip.

SUMMARY
(1) The R-curve behavior of the two kinds of gas pressure sintered
silicon nitride was characterized by three indentation methods.
One material exhibited more pronounced increasing R-curve than
another. From the observation of crack path, the R-curve behavior
was thought to be due to the grain bridging of elongated p-Si 3N4
grains.
(2) Cyclic fatigue behavior was also evaluated for the materials
at room temperature. As the results, it is concluded that the
improvement of toughness gives rise to fatigue with cyclic
loading. It was considered that the fatigue was caused by the
fracture of the grain bridging.
(3) The indentation and crack growth method which is based on the
indentation fracture mechanics was utilized to determine fracture
resistance curve. The results were in good agreement wi th the
SEPB method.

REFERENCES
1. Chien-Wei Li and J. Yamanis, Super-Tough Silicon Nitride with
R-Curve Behavior, Ceram Eng- Sci proc., 10, 7-8: 632
(1989).
2. Y. Hattori, Y. Tajima, K. Yabuta, Y. Matsuo, M. Kawamura and
T. Watanabe, Gas Pressure Sintered Silicon Nitride Ceramics
for Turbocharger Application, in: "Ceramic Materials and
Components for Engines", W. Bunk and H. Hausner, ed., Deutshe
Keramische Gesellschaft, Honnef (1986).
3. R. W. Steinbrech, A. Reichl and W. Schaarwachter, "R-curve
Behavior of Long Cracks in Alumina", J Am Ceram Soc, 73,
7: 2009 (1990).
4. M. V. Swain and R. H. J. Hannink, R-curve behavior in
zi rconia ceramics, in: "Advances in Ceramics, vol. 12,
Science and Technology of Zirconia II", N. Claussen, ed., The
American Ceramic Society, Inc., Ohio (1984).
5. R. F. Cook, B. R. Lawn and C. J. Fairbanks, Microstructure-
Strength Properties in Ceramics: I, Effect of Crack Size on
Toughness, J. Am. Ceram. Soc., 68: 604 (1985).
6. A. G. Evans, New Opportunities in The Processing of IUgh
Reliability Structural Ceramics, in: "Ceramic Transactions,
Vol. 1," G. L. Messing, E. R. Fuller, Jr, and H. Hausner,
ed., The American Ceramic Society, Inc. Ohio (1988).
7. Y. Maniette, M. Inagaki and M. Sakai, Fracture Toughness and
Crack Bridging of a Silicon Nitride Ceramic,.I Europ Ceram
~, 7: 255 (1991).
8. B. R. Lawn, A. G. Evans and D. B. Marshall, Elastic/Plastic
Indentation Damage in Ceramics: The Median/Radial Crack
System, .I. Am Ceram. Soc., 63: 576 (1980).
9. G. R. Anstis, P. Chantikul, B. R. Lawn and D. B. Marshall,
A Cri tical Evaluation of Indentation Techniques for Measuring
Fracture Toughness: I, Direct Crack Measurements. .I Am
Ceram Soc, 64: 533 (1981).

248
10. P. Chantikul, G. R. Anstis, B. R. Lawn and D. B. Marshall,
A Cri tical Evaluation of Indentation Techniques for Measuring
Fracture Toughness: II, Strength Method. JAm. Ccram Soc,
64: 539 (1981).
11. s. R. Choi, J. E. Ritter and K. Jakus, Failure of Glass with
Subthreshold Flaws, J. Am Ceram. Soc. 73 (1990).
12. R. F. Krause, E. R. Fuller and J. F. Rhodes, fracture
Resistance Behavior of Silicon Carbide Whisker-Reinforced
Alumina Composites with Different Porosities, J. Am. Ceram
~, 73, 3: 559 (1990).
13. T. Kawakubo and K. Komeya, Static and Cyclic Fatigue Behavior
of a Sintered Silicon Nitride at Room Temperature, J. Am.
Ceram. Soc., 70: 400 (1987).
14. H. Kishimoto, A. Ueno and H. Kawamoto, Crack Propagation
Characteristics of Sintered Si 3N4 under Static and Cyclic
Loads, J Soc Mat Sci Japan 36: 1122 (1987).
15. R. O. Ritchie, Mechanisms of fatigue Crack Propagation in
Metal, Ceramics and Composites: Role of Crack Tip Shielding,
Mater. Sci. and Eng. A, 103 (1988).
16. Y. Tajima, K. Urashima, M. Watanabe and Y. Matsuo, Static,
Cyclic, and Dynamic Fatigue Behavior of SUicon Ni trlde. in:
Ceramic Materials and Components for Engines, V.J. Tennery,
ed., The American Ceramic Society Inc., Ohio (1989).
17. T. Niwa, K. Urashima, Y. Tajima and M. Watanabe,
Effects of Crack Size on Fatigue Behavior in Silicon
Nitride, Nippon SeramikkllslI Kyokai Gaklljlltll Ronbllnshi.
99: 296 (1991).
18. Y. Tajima, K. Urashima, M. Watanabe and Y. Matsuo, fracture
Toughness and Microstructure Evaluation of Silicon Nitride
Ceramics, in: "Ceramic Transactions, Vol. 1," G. L. Messing,
E. R. Fuller, Jr, and H. Hausner, ed., The American Ceramic
Society Inc., Ohio (1988).
19. I. S. Raju and J. C. Newman Jr., En~. Fract Mech Vol. 11
817 (1979).
20. S. Horibe, Cyclic Fatigue Crack Growth from Indentation flaw
in Si 3N4 , J Mater Sci Lett 7, 725 (1988).

249
INVESTIGATION OF R-CURVE BEHAVIOR AND ITS EFFECT ON STRENGTH

FOR ADVANCED CERAMICS

Hideyoshi Tsuruta and Yutaka Furuse

Engineering Research Center
Tokyo Electric Power Co., Inc.
2-4-1 Nishi-Tsutsujigaoka Chofu-shi Tokyo, Japan

ABSTRACT

Three kinds of tests, including compact tension (CT)

test, SEPB test and indentation flaw resistance test, were
carried out on advanced ceramics for gas turbine components
in order to investigate R-curve behavior and its effect on
strength. Rising R-curve behaviors were observed not only in
ceramic matrix composite but also in monoli thic ceramics.
KRmax value of each sample was nearly equal to its KIC value
that was obtained by SEPB method. This was related to the
large pre-crack used in SEPB method in which process zone
would grow up sufficiently. Indentation flaw resistance of
composite was higher than that of monolithic materials. The
KIC value obtained by indentation induced flaw (IIF) method
increased wi th increasing the length of flaw introduced by
Vickers indentation. This result indicates that the KIC
value can be related to the pre-crack length and its process
zone length growing with extension crack. Distr ibution of
strength was simulated by Monte Carlo method in both flat and
rising R-curve cases using the same flaw distribution. It
was found that the Weibull modulus of rising R-curve case was
higher than that of flat R-curve case.

INTRODUCTION

Many works have been conducted to develop a highly

efficient gas turbine which can be operated at turbine inlet
temperatures higher than present level. Requi rements for
increase in turbine inlet temperature can be met ei ther by
introducing improved superalloys such as directionally
solidified superalloys, single crystals and oxide-dispersion-

Fracture Mechanics a/Ceramics, Vol. 9

Edited by R.e. Bradt et aI., Plenum Press. New York, 1992 251
strengthened superalloys along with advanced turbine cooling
techniques or by the utilization of ceramic components
without using cooling air. Since there is an increasing
penalty in efficiency by providing progressively larger
amounts of cooling air, to maintain the surface temperature
of metallic components below their usable temperature, there
is a strong drive towards the introduction of ceramic
components into gas turbine. Because of the reason mentioned
above, Tokyo Electric Power Co. (TEPCO) has been conducting a
research program for the application of ceramics to hot parts
of power generating gas turbines such as combuster, nozzle
vane and rotor blade. (1) Since the catastrophic feature of
the ceramics is the most serious problem in using as the
bri ttle materials, fracture mechanism of ceramics must be
clarified to achieve high reliability of ceramic components.
Recently, many works have been reported on R-curve behavior
of ceramics and its effect on mechanical properties. Most of
those reports deal with limited materials such as alumina,
TZP and their composite. (2)-(5) However it is very difficult
to use those materials for gas turbine components because of
their poor strength at elevated temperature and thermal shock
resistance.

In this study, compact tension tests have been conducted

to examine R-curve behaviors of candidate ceramic materials
for gas turbine components such as monoli thic sintered
silicon nitride, sintered silicon carbide and SiC platelet
reinforced silicon nitride composite. To measure the R-
curve, the crack stabilizer was used for stable crack growth
and traveling microscope was used to measure the extending
crack length. It will be discussed how R-curve behavior
affects other mechanical properties such as fracture
toughness, indentation strength and Weibull modulus.

EXPERIMENT

Sample Preparation

Table 1 shows material properties used in this study.

Silicon nitride and silicon carbide are commercialized
monoli thic ceramics and SiC platelet reinforced Si 3 N4
composite was developed by us and coresearcher. (6) These
were machined for CT test and bending test specimens. The
configuration of CT specimen is shown in Fig. 1. The shape
of the CT specimen was of specified in ASTM E-399 but
thickness of it is rather thinner than specified. The crack
tip was polished by SiC powder to make the radius of the
crack front less than 20um. The dimension of bending
specimen is 3mmX4mmX40mm and one of 4mmX40mm surfaces was

252
 Table 1. Material properties.

Strength(MPa) Young's modulus(GPa)

at RT at 1400C
Composite 500 450 300
Si 3 N4 800 700 300
SiC 700 500 400

o E
E

o
o
I't'l

\. 30mm
.I
3mm

Fig. 1. Configuration of CT specimen.

polished. The bending specimen was used for fracture

toughness measurement by SEPB method and for evaluating
strength degradation caused by indentation flaw.

CT Test

CT tests were conducted with the crack stabilizer which

was set as to seize top and bottom faces of the center line
of loading hole of the CT specimen. The crack stabilizer can
cancel the strain energy stored in the testing apparatus, and
stable crack growth will be obtained. (7) The strain gage was
put on the inside corner of crack stabilizer to measure the
load shared by crack stabilizer. The traveling microscope
consists of the X40 optical microscope, the sliding component
and the digital dial gage. The accuracy of digital dial gage
is 0.002mm. The schematic diagram of testing apparatus is
shown in Fig. 2. The crosshead speed was set O. 005mm/min
during crack extension. The load applied to the CT specimen
was obtained by subtracting the load subjected to the value
of crack stabilizer from the value of load cell. Fracture
resistance KR was calculated by the following equations:

253
 optical
microscope
~

traveling

\
CT specimen

digital dial gage

sliding component
Fig. 2. Schematic diagram of testing apparatus.

KR = P/BW 1 / 2 f(a/W) (1)

f(a/W) = {(2+a/W)(O.886+4.64a/W-13.32a 2 /W 2 +14.72a 3 /W 3

-5.64a 4 /W 4 )}/(1-a/W)3/2 (2)

where P is the load, B is the thickness of the specimen,

W is the specimen width and a is the crack length. Both Wand
a are the lengths from the centerline of the loading holes.

SEPB Test

Fracture toughness was measured by the single edge

precracked beam (SEPB) method using bending specimen.
Precrack was introduced by bridge indenta tion method.
Vickers indentation was used as a crack starter. The
fracture tests were conducted by 3-point bending using the
precracked specimen with the span length of 16mm. The length
of the crack was meqsured along with ASTM E399 after the
fracture test. The toughness was calculated by following
equations:

254
 (P SiB W3 / 2 ) f(a/W) (3)

f(a/W) [3(a/W)1/2{1.99-(a/W)(1-a/W)(2.l5-3.92a/W+
2.7a7W2)}]/{2(1+2a/W)(1-a/w)3/2 (4)

where P is the load, B is the specimen thickness, S is

span length (in this study l6mm) , W is the specimen depth
(width) and a is the crack length determined in ASTM E 399
8.21.

Resistance for Indentation Crack

Indentation strength test was carried out by 4-point

bending with the upper span of 10mm and lower span of 30mm
using the Vickers indentation specimen to evaluate the
resistance for indentation. The Vickers indentation was
introduced at the center of one of the 4mmX40mm surfaces of
the bending specimen. The load level of Vickers indentation
were 5kg, 20kg and 50kg. The crack length was measured by
using scanning electron microscope before the fracture test.
The fracture toughness was calculated using the following
equation of IIF method:

(5 )

where a is the fracture stress, a is the radius of

semicircular flaw, M is the geometric factor and ¢ is the
elliptic factor. In this study, the value of M and ¢ were
assumed to be 1.0 and 1.5 respectively.

RESULTS and DISCUSSION

CT Test

The R-curves measured by the CT specimen are shown in

Fig. 3. The rising R-curve was obtained in all samples.
KRmax value of composite, silicon nitride and silicon carbide
was 10.8, 7.0 and 6.0 MN/m 3 / 2 respectively. The
microstructures of samples used in this study are shown in
Fig. 4. The representative lengths of relatively large
grains of the composite, silicon nitride and silicon carbide
are about 50 11m, 20l1m and l5/lm respectively. Fig. 5 shows
the stable crack extension. Crack defrection was observed
in all materials. During the crack extension, the go and
stop motion of the crack extension was observed. This
phenomenon was observed especially significant in composi te
material and could be related to the debonding of grain
boundary aT large grain at crack front. neTore debonding,

255
the crack extension would be not extend until the shear ing
stress at grain boundary of large grain reaches critical
value and this large grain could act as the crack pinning.
After debonding, the friction at the grain boundary of the
large grain would act as the crack bridging and construct the
process zone with the crack extension. These effects would
contribute to the rising R-curve.

r-.,
N

"'"a
'-.. 10
Z
:::::;;
'-"
Cl:
::.:::
a)
u
c::
.....
c<:l
SiC
Cfl

Cfl 5
Q.)
0:::
Q.)
.....
.....
::l

U
c<:l
.....
I:L.

0 2 3 4

6a (mm)

Fig. 3. Fracture resistance of composite,

Si 3 N4 and SiC obtained by
CT specimen.

SEPB Test

The fracture toughness (K rc ) was measured by SEPB method

to make a comparison with the KRmax obtained by CT test. The
fracture toughness value of the composite, monolithic silicon
nitride and monolithic silicon carbide were 10.5, 7.0 and 5.8
MN/m 3 / 2 respectively, and those values are nearly equal to
the KRmax values obtained by CT tests. As the precrack used
in SEPB method sufficiently large (about 2mm), it was
considered that the Krc value obtained by this method would
approach the KRmax value, if process zone would be formed

256
 10llm
I-------t

Fig. 4. SEM photograph of fracture surface.

(a):composite, (b):Si N ,
3 4
(c) : SiC.

257
 1 QjJm

F.i.g. 5. Typical crack extension. (a):composite,

(b) :Si 3 N4 , (c) :S.i.C.

258
sufficiently during the precracking. According to this
observation, it is important to consider the R-curve behavior
of the material when the KIC value obtained by SEPB method is
used in designing and/or evaluating the reliability of the
ceramic component.

Resistance for Indentation Crack

Resistance for indentation crack is shown in Fig. 6.

Strength degradation of monolithic materials was greater than
that of composi te material. The normalized residual
strengths of the monolithic materials at the indentation load
of 50kg were about 0.2 and that of composite material was
0.5. Figure 7 shows the relationship between the crack length
and residual strength. The residual strength increases with
increasing reciprocal of the root of the crack length. The
increasing curve of the monolithic materials was linear
although that of the composite material was non-linear.
Figure 8 presents relationship between crack length
introduced by the Vickers indentation and the fracture
toughness value calculated by Eq. 5. In thi s study the
surfaces on which Vickers indentation was introduced were not
removed by machining, so that residual stress would affect on
the KIC value a little. The fracture toughness values of
monolithic materials are nearly constant and independent of
the crack length, although that of the composite material is
increased with increasing the crack length. This behavior
will be related to the R-curve behavior. Process zone would
be formed when the crack was introduced by Vickers
inden ta t ion. However in the case of compos i te, the
indentation crack was so small at low indentation load that
process zone would not be formed sufficiently.

Effect of R-curve Behavior on the Distribution of Strength

The strength distribution was simulated by Monte Carlo

method to evaluate the effect of R-curve behavior on the
distribution of strength. At first, 100 flaw sizes were
generated by random numbers, so as to follow the Weibull
distribution. The strength of different R-curve cases as a
function of flaw size can be explained using the model
described in Fig.9. The slope of the 0.1 straight line
means the value which is proportional to the square of the
applied stress. In the case of flat R-curve, unstable
fracture occurs when the straight line reaches the point A.
On the other hands, in the case of rising R-curve, stable
fracture occurs when the straight line reaches the point A
and the crack extends until the straight line reaches the
contact point I3 where unstable fracture takes place. The

259
 o composite
~ 10
bO°
c: ~O L::,. Si3N4
Q)
.....
+->
o SiC

0
C/)

cd
::l
-0
0
~ 0.5 -
0:::

-0
Ej
Q)
N

cd
E
.....
0
t1
:z:
0
0 10 20 30 40 50
Indent Load (kg)
Fig. 6. Indentation flaw resistance of
composite, Si 3N4 and SiC.
Strength is normalized by initial
strength.

0
10
Q..
400 f-
6 0
.J::.
+J
CI
C
QI 0 Ch
.....
+J
VI
(ij
:J
"U
'V;
200 - D.
E
QI
0::

0 o composite
L Si3N4
o SiC
I I
0 0.05 0.10

.j1i2; (lim -1/2)

Fig. 7. Relationship between ..jl/2a and

Residual strength. The a is the
radius of semicircular flaw
introduced by Vickers indentator.

260
 10
r---

o
N

"-
'"'a
:z:
-----
:::;;
'-'
0
u
::.::
0
en 5- D
<fJ
Q.)
c:::
L6. L6. o
.c
bO
::l
0
......
Q.)
.....
o composite
....,
::l
6, Si3N4
U

'"
.....
CL.
o SiC
I
0 500 1000
2a (I'm)

Fig. 8. Relationship between fracture toughness

and the radius of semicircular flaw.

rising R-curve

flat R-cu rve

a
ao

Fig. 9. Strength calculation model using

different R-curve cases.

261
strength in each case was calculated by the slope of the
straight line of which the unstable fracture occurs. The
Weibull modulus was calculated by using the strength
distribution which was obtained based on above-mentioned
method for each R-curve. This Monte Carlo trials was
repeated 1000 times and mean Weibull modulus was obtained.
Following rising R-curve equation was used for calculation
which was approximately determined from the R-curve obtained
by CT test.

(6 )

In this equation, the units of KR and a are

(MN/m 3 / 2 ) and (10- 6 m) respectively. The calculated Wei bull
moduli of the flat R-curve, rising R-curve (Eq.6) are 15 and
18 respectively. It would be concluded that materials with
rising R-curve behavior have higher Weibull modulus than
materials with flat R-curve behavior when they have the same
initial flaw size distribution.

SUMMARY

Rising R-curve behaviors were observed in both

monolithic ceramics and ceramic matrix composite. The KRmax
value of each sample was nearly equal to the KIC value that
was obtained by SEPB method. This relationship would be
obtained by the large pre-crack induced in the SEPB specimen
in which process zone would grow up sufficien tly. The
indentation resistance was increased with increasing the
KRmax value and the KIC value obtained by IIF method was
increased with increasing the flaw length that was introduced
by Vickers indentation. And these results indicate that the
KIC value will be related to the precrack length and process
zone length growing with extending crack. The distribution
of strength was simulated in both flat and rising R-curve
cases. The Weibull modulus of rising R-curve resulted
higher value than that of flat R-curve.

REFERENCES

1. Y. Hara et aI, "Development of ceramic component for a

power generating gas turbine", ASME paper, No.91-GT-319,
(1991)
2. M.V.Swain, "R-curve behavior and thermal shock resistance
of ceramics", J.Am.Ceram.Soc .. 73[31. 621-28. 1990
3. R. Knehans and R. Steinbrech, "Effect of grain size on the
crack resistance curves of A1 20 3 bend specimen",
Science of Ceramics 12-Ceramurjica s.r.l., Faenza, Italy

262
4. E.H.Lutz, N.Claussen and M.V.Swain, "KR-curve behavior of
duplex ceramics", J.Am.Ceram.Soc., 74[1], 11-18, 1991
5. J. Homeny and W.L.Vaughn, "R-Curve behavior in a silicon
carbide whisker/alumina matrix composite", J.Am.Ceram.
Soc., 73[7], 2060-62, 1990
6. H.Sakai, K.Matsuhiro and Y.Furuse, "Mechanical properties
of SiC platelet reinforced ceramic composite", Ceramic
engineering and science proceedings, vol.11 No. 11-12,
1990
7. M. Sakai and M, Inagaki, "Dimensionless load-di splacemen t
relation and its application to crack propagation
problems", J.Am.Ceram.Soc., 72[3], 388-94, 1989

263
CRACK FACE BRIOOING TRACTIONS IN MONOLITHIC SPINEL

Jack C. Hay and Kenneth W. White

College of Engineering
University of Houston
Houston, Texas, 77204-4792

ABSTRACT

T!le strongly rising R-curve behavior, typical of coarse grain sized spinels, has
been ascri:ed to crack face tractions in the following wake zone which reduce the crack tip
stresses. JI novel experimental approach is presented which isolates these tractions for
direct chmacterization in pure tension. With this method, a detailed study of the crack face
separation ~vents has identified the toughening contributions from the active microstructural
constituen I s. A critical wake stress of about 7 MPa is estimated for this high purity spinel,
containing only minor quantities of a crystalline grain boundary phase. The post fracture
tensile tesl results are validated through a simple model to reconstruct the experimentally
determine<' R-curve.

INTRODlICTION

Fni ;ture mechanisms in ceramic material systems have been the center of interest
over the la!t two decades. The rising crack growth resistance curve behavior fIrst observed
in Aha:, t-:r Buresch and Pabst 1, suggested the existence of a cumulative toughening
mechanisr' in brittle materials. It was six years later when Hubner and Jillek 2 provided
the fIrst in:;ight into the role of the following wake region in the fracture toughening
process, where the R-curve behavior of sharp cracks was compared with similar specimens
containing blunt cracks. Knehans, et al. 3 showed that the removal of the crack face

FroclUTe Mechanics of Ceramics. Vol. 9

Edited by R.C. Bradt el aI., Plenum Press, New York, 1992 265
material immediately following the primary sharp crack lowered the crack growth resistance
to that value characteristic of initial conditions, prior to crack growth. Microscopic
observation of the bridging microstructural features in the following wake region was
published independently by Swanson 4 and Sakai, et al. 5, who studied monolithic Ah03
and MgAh04, respectively.

The renotching experiments of Knehans, et aI. 3 and Grimes, et al. 6 clearly

determined the importance of the wake region in the toughening of monolithic ceramics,
however, their experiments offer no direct assessment of the load path in the vicinity of the
crack tip. With the goal of directly proving the existence of crack bridging loads in the
wake zone of coarse-grained alumina, Reichl and Steinbrech 7 implemented the short
double cantilevered beam (DeB) specimen, modified with a short backnoteh prior to
testing. This specimen continued to support a finite load after passage of the main crack tip
through the test ligament and into the machined back notch. Optical verification of the grain
bridging mechanism on the specimen surface identified discrete traction sites along the
crack face. The authors arrive at a value of 29 MPa for an estimation of wake stresses in
the modified specimen.

An in situ SEM study of fracture of alumina using a double torsion specimen was
recently presented by Vekinis, et al. 8. Although no direct measurement of wake loads was
attempted, this study provided the first mechanistic correlation between the microstructure
and the fracture phenomenon. Three proposed micro-mechanisms include bending of
elastic bridging ligaments, frictional energy consumed through grains which were wedged
or pinched as a result of thermal expansion anisotropy, and finally, bridging grains forced
to rotate in fixed sockets in the mating crack faces. Each of these proposed mechanisms
occur only in the wake region and are consistent with the existing body of
phenomenological data appearing in the literature. In a study conducted by White and
Kelkar, crack face bridging mechanisms were evaluated. The nonlinear fracture behavior
identified by renotch tests of MgAIZ04 spinel 9, prove the existence of grain crack face
tractions in the wake zone. The absence of thermal expansion anisotropy in this cubic
spinel system, however, excludes TEA-activated wedging as a valid toughening
mechanism.

The fracture mechanism studies to date provide an excellent phenomenological basis

for the toughening process, however, fall short of directly identifying the components of
the fracture event. It is clear from this existing data that the following wake region plays a
significant role in the fracture process for most monolithic, non-transforming structural
systems. Also apparent, is the absence of an accepted mechanism, or mechanisms,
universally responsible for the two essential components of the fracture behavior; the crack
initiation resistance associated with the crack tip, and the cumulative toughening.

266
 Central to the difficulties precluding the direct identification of these mechanisms is
the task of isolating the components of the microstructure which are active in the load
sharing event. Reichl, et. al. 7 have elegantly demonstrated the load-supporting capability
in the wake region. Although these results agree very well with the theoretical treatment of
Mai, et al. lO, no microstructure-specific analysis emerges from this approach. Their stress
computation assumes that all the grains contribute equally toward the wake effect,
regardless of their size, morphology or fracture mode. A detailed consideration of the
microstructure, in conjunction with the fracture behavior, would elucidate critical aspects
which must be included in the wake analysis. The present study introduces a direct method
for the evaluation of closure stresses in the following wake region. The analysis examines
the microstructural features of a high-purity, polycrystalline MgA1204,consisting of grains
ranging in size from 50 to 500 11m. As a means of validating these experimental methods,
microstructural features and the measured crack closure stress are incorporated into a model
for the reconstruction of the R-curve.

EXPER~ENTALPROCEDURES

A coarse grain sized magnesium aluminate spinel, MgA1204' , characterized by a

bimodal grain size distribution, was selected for this study largely in consideration of two
characteristics: a strongly rising R-curve behavior in combination with optical transparency
comparable with that of window glasses 9. A majority of the grains are observed to fall
between 50 to 200 11m, with a few remaining grains distributed in the 200 to 500 11m
range. The average grain size is approximately 150 11m. The room temperature elastic
modulus of 275 GPa was determined by both flexural MOR tests and ultrasonic
techniques. The material processing has been designed to produce a high purity and low
porosity ceramic for optimum optical properties. Constituent powders and a crystalline hot
pressing aid, LiF, are blended and processed according to reference 11.

Referring to Figure la and Ib, typical specimen dimensions are S=40 mm, W=7
mm, B=6 mm and aoJW=O.45. As a control, two specimen geometries permit alternate
approaches to obtain equivalent data. In the first, a single edge notched beam specimen is
loaded in three point bending at a crosshead speed of 1.3 11m/min. The crack length is
observed optically and allowed to propagate to a predetermined length, where it is arrested
by removal of the load. Details of this technique appear elsewhere 6. The partially
fractured specimen is removed from the load frame to be backnotched, carefully removing
all uncracked material, including the crack tip. The success of this step may be verified
through optical methods, both from the root of the back notch and the side of the crack, as

• Alpha Optical Systems, Inc., Ocean Springs, MS 39584 (A Coors Ceramics Co.)

267
 t A
P P

~ S
P/2
P/2
(a)

A
,~12 ~Bj4

-'-~
~P/2
s
P/2
~ao
P
(b)
(c)

Figure 1. Geometry for (a) Straight Notch, Single Edge Notch Beam, and (b)
Straight Notch, Double Edge Notch Beam with a wedge.

Figure 2. Optical view of post fracture tensile specimen, confmning location of

backnotch.

268
 5

4
-----
C':I
0.

6 3

'"'" 2
nOlching Technique

....
~
t-
IJ)

0
0 10 20 30 40 50
Displacement (11m)

Figure 3. Comparison of Post Fracture Tensile Test results using

two methods of specimen fracture evidencing consistent results
through both techniques.

shown in Figure 2. The fractured specimen, attached only by the wake zone, is now
prepared for the post fracture tensile (PFf) experiment shown schematically in Figure lc.

A second technique (Figure Ib), developed to obtain equivalent data from a similar
crack length and crack opening displacement (COD), will provide an indication of the
significance of any detrimental influence from the mechanical backnotching step. This
approach, derivative from that of Reichl, et al. 7, incorporates a flexure specimen,
machined to the same adW used in the single edge notched beam of Figure la, is
backnotched prior to crack growth. A stiff alumina wedge, inserted into the backnotch,
provides support throughout a four point flexure test. A unique inflection point on the
load-displacement record, clearly identifies the test conditions coincident with entry of the
crack tip into the backnotch. The PFT experiment may now be continued as described
below.

After mounting attachment fixtures to the ends of the specimen, a tensile load is
applied along the specimen length and normal to the crack faces at a crosshead speed of 1.3
11m/min. The load measured by this method represents the tensile component of the crack
face tractions, which contribute toward the cumulative toughening behavior. In Figure 3,
the stress displacement curves for PFT tests of the backnotching method and wedge
method are compared. The relevance of the differing stress levels, arising from each
respective initial COD profile, will be considered in detail below, however, the strong
agreement between the trailing curves validates the backnotching procedure.

A necessary condition ensuring meaningful results of the tensile test is that the
unloading procedure following the flexure tests does not produce significant damage to the

269
bridging microstructure in the wake zone. A simple load and reload experiment identifies
losses in the wake zone following reloading to be consistently below 5% of the last
measured load before unloading. This degree of wake zone damage is small with respect to
the measured wake zone loads of the current study and is consistent with recent
observations of Lathabai, et al. 12 involving cyclic fatigue of bridging grains in alumina.

RESULTS AND DISCUSSION

Previous detailed treatments of the rising R-curve behavior, characteristic of these

spinels 9,13, confIrms the presence of a cumulative component of crack growth resistance.
The post fracture tensile (PFf) test will be implemented here to study the cumulative
component of this behavior, existing in the following wake region. The result of a PFr
test, shown in Figure 4, displays four distinctive behavioral regions, each representing a
signifIcant component of the crack face separation event. The linear region extends to
about 65% of maximum load (point A), suggesting that non-recoverable grain activities are
delayed to some threshold loading level. Unloading within this region was found to follow
the same trace back to the origin of the PFr test. At the onset of the non-linear behavior,
the load continues to rise to a maximum (point B), characterizing the full development of a
displacement controlled deformation mechanism which supports a maximum load only at
full maturity. Beyond PMAX, increasing crack face separation monotonically diminishes
the load supporting capacity of the active region, eventually reaching a regime characterized
by a very small load with only a modest dependency upon crack face separation (point C).
This fInal regime suggests a virtually constant load-supporting mechanism over the range
of measured displacements.

50
B
40
'""'
Z
....... 30
"C
~
0 20
,.J

10

0
0 10 20 30 40 50
Displacement (j.lm)

Figure 4. Load-Displacement results of Post Fracture Tensile

Experiment.

270
 Figure 5. SEM Fractograph after complete separation, showing
transgranular fracture of large grains.

To effectively link this behavior to the microstructure, two critical characteristics of

this spinel are evaluated. The postmortem fracture topography, represented in Figure 5,
indicates the high fraction of transgranular fracture, typical of these ceramics. As expected,
these fractured grains fall predominantly in the larger sizes; typically the largest grains
failing intergranularly fall between 80 and 100 11m. Since effective grain bridging requires
adequate physical communication across the crack faces, these two criteria are critical in
identifying the possible roles of the various microstructural components in the fracture
event. Accordingly, the crack opening displacement will now be compared with these
microstructural dimensions to assess the capacity for crack face bridging.

The COD profile in the wake zone of a bend bar specimen ranges from zero at the
crack tip to a maximum at the crack mouth. The maximum COD associated with the load
carrying event has been reported to fall between 0.25 7 and 0.50 14 of the active grain size.
Because of the inability of smaller grains to bridge large COD's, bridging is expected to
vary from a maximum at the crack tip to a minimum at the trailing extreme of the wake
zone. The linear model for the COD offered by Steinbrech 15, will be adopted here for
analysis of the bridging zone length.

Various COD profiles are produced by allowing a crack to propagate to various

crack extensions. In a series of PFT experiments, predetermined COD profiles were
obtained from specimens of various crack lengths, as shown in Figure 6, where the greater

271
 Figure 6. Backnotched Single Edge Notched Beam specimens of
different COD profiles prepared for Post Fracture Tensile test.

os

4
.~
IQ.
;~ 3

-..
ell
....
ell 2
,rrJ

0
0 10 20 30 40 50
!!j~Vl~~~.~~!!! ~It!!!)
Figure 7. Post Fracture Tensile test stress displacement family of
curves.

272
 8~------------"

10 20 30 40 SO
Displacement (~m)

Figure 8. Curve fit and extrapolation of experimental data,

approximating stress displacement curve for a flat crack.

backnotch depth of the right-hand specimen accommodates the shorter crack length (and
therefore smaller COD) resulting from the flexure test. After nonnalizing the tensile loads
with the wake zone area, three such results fonn the characteristic family of tensile stress-
displacement curves shown in Figure 7. The lower curve, corresponding to the largest
COD profile, illustrates the lower stresses expected from the smaller population of bridging
grains in the wake zone. Accordingly, the lower bridging grain population reduces both
the tensile elastic stiffness and the peak stress, but does not alter the advanced stages of the
separation event, as all three curves agree within experimental error for equivalent COD's.

Neglecting the elastic displacement component, the stress required to open a crack
of zero COD may be estimated from the y-axis intercept of Figure 8. For this spinel, this
method yields a critical stress of 7.35 MPa. A curve fit of the trailing side of the
experimental curves, extrapolated to zero COD, describes the complete stress-crack
opening displacement relationship for the trailing wake zone of a fracture test. This
relationship between crack closure stress and COD is used in the next section to
characterize a crack growth resistance curve.

RESISTANCE CURVE MODELING

The microstructure-dependent relationship between the crack face tractions and the
crack opening will provide the basis for modeling of a crack growth residence curve for
validation of this experimental approach. As shown by several earlier R-curve studies
involving notched bend bar specimens 3,6, the slope of the resistance curves dR/<Ma is
dependent not only upon microstructure, but also specimen geometry. The DCB specimen
has been shown to be immune to this influence, as illustrated by the renotch results shown
in Figure 9 9. Here, dR/dAa remains virtually unaffected by the crack location, despite the
wake removal at a crack length of about 4 mm. Therefore, to avoid the artifacts of the

273
 J

E
-.;

/
Q. 2
~
~
tl:
/
I
0 2 4 6 8 10
t.a

Figure 9. Renotch test for Magnesium Aluminate using a DCB

configuration. 9

flexure specimens, the present OR-curve modeling results are compared to experimental
spinel results obtained from the DCB configuration.

OR values are obtained from instantaneous elements of fracture surface energy and
crack extension, and represented as 16:

where Oi is the fracture surface energy at initial conditions. The assembly of subsequent
values of OR will comprise the OR-curve.

Since the toughening mechanisms for this material have previously been shown to
exist only in the wake zone 9, the present analysis assumes equality between the energy
dissipated in the wake zone and the strain energy release rate. This is justified by the
experimentally derived expression for stress, which includes all wake mechanisms, and
excludes only that frontal zone material which is inactive in the toughening process. The
reversion to an original stress intensity factor following wake zone removal, shown in
Figure 9, indicates that any strain energy which may be dissipated in this zone is
negligible.

Analysis of the ~O component is determined using a model offered by Kannen. 17

The work per unit area required to close the crack is given by

~O:=; ~f U dx
ao

274
 60
Range or
SO Experimental
Rcsulls
N 40
<
E
;:;
'-' 30
C-'
20

10
0 2 4 6 8 10 12 14
Crack Extension (mm)

Figure 10. Comparison between crack growth resistance curves using the model
presented here and conventional calculations.

where U is the work done by the crack face tractions in closing the crack by an amount
equal to the COD, defined by the area under the stress-COD curve. After substitution for
U,

+JJ
a V(x)

L1G = cr(V) dV dx
ao 0

where cr(V) is the closure stress and V(x) is the COD. The quantity l/a relates to the
energy release rate for the crack extension a.

For this study a simple linear approximation of the COD is adopted 15,
_ 8 (a-x)
V( x)- a
where 8 is the loadpoint displacement, a is the crack length and x is the location along the
crack plane such that a > x > ao. A more rigorous approach for the COD approximation
would implement the results of Yu, et al. 18, who report a parabolic profile.

Evaluation of .1G at several crack lengths yields the PFT-derived resistance curve
shown in Figure 10. The relatively good agreement with the experimentally determined
OR-curves of White and Kelkar 9 establishes the validity of the present approach to wake
zone evaluation.

CONCLUSIONS

A novel experimental approach has been presented which isolates the following
wake component of the cumulative toughening from the crack tip resistance. Post-fracture
tensile load measurements represent the residual strength of this microstructural region as a

275
function of crack face separation distance, pennitting the development of a proposed model
for toughening in monolithic, nontransfonning ceramics. The true microstructural features,
including grain size distribution and fracture mode are consistent with the proposed model.
Using this approach, crack face tractions are estimated at a level near 7 MPa.

REFERENCES

1. F.E. Buresch, R. Pabst, "Bestimmung von Festigkeitseigenschaften Keramischer

Stoffe Unter Verwendung Bruchmechnischer Methoden," Science of Ceramics,
Vol. 6 XVI 3-17, (1973).
2. H. Hubner, W. Jillek, "Subcritical Crack Extension and Crack Resistance in
Polycrystalline Alumina," J. Mater. Sci., 12 [1], 117-25 (1977).
3. R Knehans, R Steinbrech, "Memory Effect of Crack Resistance During Slow Crack
Growth in Notched Al203 Bend Specimens," 1. Mat. Sci. Let., 1 [8], 327-29
(1982).
4. P. Swanson, CJ. Fairbanks, B.R. Lawn, Y.W. Mai, BJ. Hockey, "Crack-Interface
Grain Bridging as a Fracture Resistance Mechanism in Ceramics: I, Experimental
Study on Alumina," J. Am. Ceram. Soc., 70 [4] 279-289 (1987).
5. M. Sakai, RC Bradt, A.S. Kobayashi, "The Toughness of Polycrystalline MgAb04,
"Journal of Japanese Ceramics Society, 96 [5], 525-31 (1988).
6. RE. Grimes, G.P.Kelkar, L. Guazzone, KW. White, "Elevated-Temperature R-
Curve Behavior of a Polycrystalline Alumina," J. Am. Ceram. Soc., 73 [5] 1399-
404 (1990).
7. A. Reichl, R W. Steinbrech, "Determination of Crack Bridging Forces in Alumina," 1.
Am. Ceram. Soc., 71 [6], C299-301 (1988).
8. B. Veninis, M.G. Ashby and P.W.R. Beaumont, "R-curve Behavior of Alz03
Ceramics," Acta Metall. Mater., 38 [6], 1151-62, (1990).
9. KW. White, G.P. Kelkar, "Evaluation of the Crack Face Bridging Mechanisms In a
MgAb04 Spinel," J. Am. Ceram. Soc., 74 [7] 1732 (1991).
10. Y.W. Mai, B.R Lawn, "Crack Interface Grain Bridging as a Fracture Resistance
Mechanism in Ceramics: II, Theoretical Fracture Mechanics Model," J. Am.
Ceram. Soc., 70 289-294 (1987).
11. D.W.Roy, J.L. Hastert, "Application of Transparent Polycrystalline Body with High
Ultraviolet Transmittance," U.S. Patent no. 4,983,555: Jan. 18, 1991.
12. S. Lathabai, 1. Rodel, B.R Lawn, "Cyclic Fatigue from Frictional Degradation at
Bridging Grains in Alumina," 74 [6], 1340-48, (1991).
13. G.P. Kelkar, "Fracture Behavior of Monolithic Alumina and Magnesium Aluminate
Spinel," M.S. Thesis, University of Houston, 1989.
14. G.P. Kelkar, KW. White, "Effect of Microstructure on R-Curve Behavior of
Monolithic Ceramics Using DCB Specimens," Paper 2-BP-90, 92nd Annual
Meeting of the Amer. Ceram. Soc., Dallas, TX, April 23-26, 1990.
15. R.W. Steinbrech, F.Deuerler, A.Reichl, W. Schaarwachter, "Correlation of Crack
Opening Displacement and Crack Resistance Curve of Alumina," Science of
Ceramics, Vol. 14,659-664 (1988).
16. P.F. Becher, CH. Hsueh, P. Angelini, T.N. Tiegs, "Toughening Behavior in
Whisker-Reinforced Ceramic Matrix Composites," 1. Am. Ceram. Soc., 71 [12],
1050-61 (1988).
17. M.F. Kanninen and CH. Popelar, Advanced Fracture Mechanics, Oxford University
Press, New York, 1985.
18. CT. Yu, A.S. Kobayashi, "Fracture Process Zone In Ceramics and Ceramic
Composites," Proceedings and Abstract AMD-Vol 130, Experiments in
Micromechanics of Failure Resistance Materials, ed. KS. Kim, pp. 79-83 ASME
1991.

276
R-CURVE PROPERTIES OF ALUMINA

MEASURED BY STABLE FRACTURE TEST IN BENDING

Toshihiko Nishida and Ichiro Kameyama

Kyoto Institute of technology

Matsugasaki, Sakyo-ku, Kyoto, 606 Japan

INTRODUCTION

The single edge precracked beam (SEPB) method 1-3) and the inden-
tation fracture (IF) method 4 - 6) are well known procedures now employed
for measuring fracture toughness (KIc) of high performance ceramics.
These methods have been also objected of standardization by the Japan
Industrial Standard enS). Keeping steps with the standardization of
these method, we investigated further about the problems related to the
SEPB method 7- 9). On employing the SEPB method, a sharp pop-in pre-
crack is introduced in a rectangular specimen by using a precracker, and
then, this specimen is fractured in bending. As well as this method
provides a pop-in crack whose tip atomically sharp, over estimation of
KIC (danger-side evaluation usual by sawed notch) 10,11) can be avoided
and the scattering of the experimental (the number of measurements) can
be significantly reduced. JIS states that the SEPB method is only ad-
dressed to "fine ceramics" which are dense after sintering and in the
state of polycrystals composed of small grains as called "KIC constant"
materials.

Because the brittle nature of ceramics still prevents their full

applications for structural and engineering use, new fabrication processes
of toughened ceramics has been investigated actively 12,13) along with the
standardization of evaluating KIC values. As a result of these efforts, it
has become clear that the resistance against crack extension is affected
both by the stress-shielding effect due to the process zone formed at the
crack tip, and that due to wake formed along the fracture surface and to
the interaction between the two fracture surfaces. When the latter ef-
fects are not negligible, KIC will be considerably increasing with the
increase in crack length; a phenomenon known as R-curve behavior.

It is expected that the KIC values for R-curve materials measured

by the SEPB method will be affected by the history in preparing the
precrack. Therefore, in the JIS procedure, it is clearly notified that the
SEPB method is applicable only for KIC constant materials. As discussed
in the next section, it is difficult to classify a priori if a ceramics materi-
al belongs to the category of KIC constant materials or not. Thus, only
possible way is to investigate case by case about the effect of the ceram-
ic microstructure on the KIC values obtained by SEPB method.

Fracture Mechanics a/Ceramics, Vol. 9

Edited by R.C. Bradt et ai.• Plenum Press, New York, 1992 277
 With this in mind, in the present paper, we measured the KIC
values of several kinds of alumina polycrystals by the SEPB method, and
discussed about their validity.

THEORY - CRACK EXTENSION RESISTANCE OF POLYCRYSTALLINE CERAMICS

KIC values of polycrystalline ceramics strongly depend on micro-

structure. it is also well known that the KIC values for polycrystals are
fairly higher than those of single crystals. To simplify the discussion in
this paper, we assume that a brittle material with a very sharp straight-
through crack is loaded in mode J ((a) in Fig. 1). Because the KIC of a
single crystal is relatively smaller than that of polycrystals, crack will
initiate the propagation 'llong the cleavage planes inside of a crystal
grain or along th(~ grain boundary at relatively low loading stage. The
crack extension in such initial stage be most. likely affected by clack
deflection, because of the random orientation of crystallographic planes in
the po)ycrystal ((b) in Fig. 1). The degree of the deflection becomes
constant after a comparatively short crack extension am in the figure (at
a length a few times the average grain size). Crack extension resistance
will be increased by the resultant crack deflection, crack bowing, crack
branching, etc. In the present discussion, we treat this deflection ef-
fects as §.tre§:;L..§hieldjJ!.K__effQ.cl ..of A.l?-rOC~~~LZOIl~L..9!'-'!_~TIl_G-Ii._.tiJ2 (Rfront
in the figure) as a whole.

In a next step, we will treat the case in which a crack continues to

pxtend on continuous loading ((c) in Fig. 1). In addition to the continu-
ous shielding effect at the crack tip, similar effects behind the tip (i.e.
§. birJqLDg.j Lt.. tbQ.__~/:l,k~L.9,Jl<UO r .~fj£~LJ).J!__ J!:<M;l!JJ:~_._§.tJx.fuce _JIi!cl!QD ) may
become (~ffective (Rt",hind in the figure). Those effects will increase
gradually during a comparatively long period of the crack extension,
compared to am defined before. Fracture resistance of polycrystalline
ceramics (Rtotal) is considered to be improved over that of single crys-
tals by the cooperation of those kinds of stress shielding effect (Rfront +
RIJChind). When the latter effect (Rbehind) can be negligible compared to
the former (Rfl<llJd or am is much shorter than the precrack and liga-

OL

Fig. 1 A simple model for crack extension and their change

of resistancf!.

278
ment length, a polyerystalline body can be considered as a "KIC con-
stant" material, not exhibiting R-curve material.

The fracture toughness defined by the stress at which an ideally

sharp crack with no historical damage begins to propagate is expected to
coincide exactly with the point KIO in Fig. l. However, at the pl'(~sent
time, we do not have a technique able to detect the crack initiation exact-
Iy. Gerwrally, KIC is determined by Uw load at the onset of unstable
fract.ure, because crack initiation .in brittle materials directly leads to
catastrophic fracture. The critical condition for t.his unstable fracture is
expressed by the point wher'e the energy release ratio (dG/da) exceeds
th(·~ crack extension resistance (dR/da), and it corresponds to the point of
a contact of the stress gradient ]j[](~ with the ({-curve. If the' initial
crack length is sufficiently larger than am (al. in Fig .1), Klc evaluated
from the onset load of brittle fracture is close to the KIm value, defined
in fracture mechanics d(~aling with large continuous plastic ',;ldy. On the
other hand, the size of defects such as intrinsic flaws and surface
damages in high strength ceramics have the same order'-ol'-magnitude size
of their microstructure (as in Fig. 1). Thus, KIC obtained from the onset
load of brittle fracture will be lowm' than KIm. Then' hav!' been sevpral
studies reporting on the tendency or KIC to decrease with ttl(' decrease
in size of the crack originating fracture 14, L5). This phenomenon can be
explained simply by considering both t.he energy condition of britLle
fracture and the transit.ion from macro-crack to micro-crack. Klc values
measured by using a crack or notch with long size are useful for the
comparison of crack extension resistance among mater·ials. However, these
values are sometimes useless to predict the strength of smooth specimens
with small crack size.

EXPERIMENTAL

Four kinds of polycrystalline alumina from Nikkato Co. were used in

this work. Their microstruct.m·al features arp shown in Fig. 2 and Table
1. They wen~ designated as A-D in the orclPr of de(;n~asing maximum
grain size. The alumina content in them were above 99.9%. Preparation
of t.he SEPB specimen, measurement and calculation of KIC were carried
out as described in .JlS R 1607. Ten to fifteen nwasurelllents in one
condition were carried out at a room tempel'ature in air. The single edge
V-shape notched beam (SEVNB) method 16) in which V-shaped notch with
very small tip radius was introduced was also employed in or'der t.o duci-
dat.e the effect between the two fracture surfaces of pop-in crack on KlC.
Only five measurements in one condition were done because the scatter of
the obtained data was very small.

Stable fracture test.s for' obtaining R-c:urve characteristic of Hw

specimens were also mad!:). However, it was very difficult to attain stable
fracturp in bending. Actually, the R-curve behavior could be obtained
only from tests carried out with applying a stabilizer (see Appendix) and
also a very slow cross-head speed (0.002 10m/min.) has to be adopted.
The stable fract.ure test.s were done in dried toluene to keep humidity
away.

RESULTS AND DISCUSSION

KIC values measured by .JIS R 1607 and bending strength measured

by JJS R 1601 of specimens A - D are listed in Table 2. An important

279
 Fig. 2 SEM photographs of polished and thermally etched surface of
alumina poly crystals used in this experiment.

Table 1. Grain size of alumina polycrystals.

Sample Grain size

Max.{j" m) Mean(.u m)

A :lO 8.1
R 15 5.4
C 10 6.3
D 2 1.0

Table 2. Fracture toughness and strength of alumina

polycrystals.

Sample Fracture toughness Strength**

SEPB* IF* SEVNB

(MPam l / 2) (MPa)

A 5.2 ± 0.2 3.9 ± 0.5 3.4 ± 0.1 278 ± 17

B 4.8 ± 0.3 4.3 ± 0.6 363 ± 16
C 3.6 ± 0.1 3.7 ± 0.1 346 ± 18
D 3.2 ± 0.1 2.8 ± 0.1 3.3 ± 0.1 467 ± 58
* JIS R 1607, ** JIS R 1601

280
 1001:
11

150um
15 11 IT

Fig. 3 SEM photographs of fracture surface of alumina polycrystals and

thei r slll"face profi les.

281
peculiarity of the specimen A with largest grain size was its high K,c by
SEPB method. Several researchers have already reported that rising R-
curve characteristic was observed for alumina polycrystals with large
grain size, and have suggested rising R-curve would be caused by stress
shielding effect such as grain bridging mechanism behind the crack
tip 18,19>. As a consequence of the fact that the precrack in SEPB speci-
men is introduced by pop-in method, the fracture surface would be
smoother than in the case of the stable fracture. Roughness of the
fracture surface was measured by a roughness tf?ster on the pop-in
precrack region, on the brittle fracture region, and on the stable frac-
ture region. SEN photographs and their surface profiles of the pop-in
precrack surface are shown in Fig. 3.

Surface profiles for the br'itUe fracture and fOl' the stable fracture
were almost t.he same as that of the precrack surface. A good correlation
was also observed between roughness and maximum grain size, and pro-
trudes with about 20-30 /1. m were observed on the surface of specimen A.
As discussed in a previous paperS), displacement of the crack mouth
opening of the SEPB specimen at the onset of brittle fracture of ceramics
was a few 11 m at the longest. This suggest that there is much possibili-
ty for SOmf? stress shielding dfect such as fracture surface traction to
operate.

The pop-in crack was cut off by saw notch leaving only its front
portion, and then Klc values were measured by J1S R 1607 method as
shown in Fig. 4 (Double notch test). The relation bPlween KIC and the
remaining precrack length (6 a, in Fig. 4) is shown in Fig. 5. The Klc of
specimen A clearly decreased with decreasing 6a,. However, there was
no effect of the double notch test on KJ(: for specimen 0 with small grain
size. This suggests that the Klc for specimen A with large grain size
measured by SEPB method is influf~nced by some actions behind the crack
tip, and their effects operate in the range of a few mm from the tip.

(Al

(8)
Sow notch

Fig. 4 Schematic drawing of double notch test before (A) and

after double notch (B)

282
 In the previous section, it was suggested that some stress shield-
ing effects behind the crack tip operate in SEPB test of alumina poly-
crystal specimens with large grain size. Then, we attempted to obtain
the R-curve by using both SEPB and SEVN B specimens. In the latter
case, the possibility of surface traction at the crack initiation was avoid-
ed for definition.

-5
'"
Specimen: A
0
- 5.2
d
E CO
d
~4 Ql ~~o
zLJ

Il:1dJ 0- 3.2
3 [jJ

Specimen: 0

0 0.5 1.0 1.5

liar (mm)

Fig. 5 Relation between KIC and .6 ar shown in Fig. 4 for specimen

A and D.

Typical load - displacement curves of specimen A during stable

fracture in bending are shown in Fig. 6. Compliance of SEPB specimen
on loading did not change up to the maximum load. On the otlwr hand,
compliance of SEVNB specimen on loading changed before the maximum
load; a phenomenon accompanied by AE. Load - displac(~menl relation
during stable fracture for the SEPB specimen was also theoretically calcu-
lated on the assu mption that a linear fraclu 1'e mechanics of KIC constant
material is applicable. The agreement between theoretical line and exper-
imental data was good for SEPB specimen. This suggests that even if the
fracture surface traction such as grain bridging does exist, the fracture
behavior can be analyzed based on the assumption of perfect elastic body
(negligible plasticity in the mechanism). Thus, the crack extension .6 a
was calculated from Uw change in the compliance of the specimen by
using the assumption of perfect elastic body, and KR was also calculated
from the theoretical crack length and fracture loads.

Typical R-curves for SEPB and SEVNB specimens of A are shown in

Fig. 7. A flat characteristics of 5.2 MPam l / 2 was obtained for SEPB
specimen. On the other hand, crack extension resistance increased for
SEVNB sp<lcimen from 2.7 MPam I / 2 to 5.2 MPam l / 2 which is exactly the
saturated value by SEPB specimen, with crack extension length of about
0.1 mm. This result suggests that KIC values by SEPB method may be
overestimated in the case of R-curve materials because of large traction
effects in the precI'acked surfaces.

283
 60 r-----------,
SEPB

z 40 •••• Experimental

----- Th~ti(ol

10 2.0 3.0 4.0

Displacement (lO~m)

Fig. 6 Typical stable fracture curves of specimen A measured by using

SEPB and SEVNB.

284
 6 SEPB
I a..-
~5
E 0
d:4
L
\
SEVNB

o OS 1.0 1.5
Me (mm)

Fig. 7 R-curve of specimen A measured by using SEPB and SEVNB.

SUMMARY

Fracture toughness (Klc) and crack extension l"esistance (R-curve

characteristic) were evaluated for alumina polycrystals with different
grain size. The Klc values were measured according to SEPB and IF
method according to JIS (.Japan Industrial Standard R 1607 - 1990; Test-
ing methods for evaluation of KIC values of high-performance ceramics).
R-curve characteristics were also measured by stable fracture test in
bending on SEPB and SEVNB specimens.

The KIC for an alumina polycrystal with a large grain size meas-
ured by SEPB was about 1.5 times larger than that measured by IF and
SEVNB methods. The deviation of the KIC became smaJl when the pap-
in crack in the specimen for the SEPB test was cut off by saw notch
leaving only its front portion. This experimental results proves that the
large value of the KIC obtained by the SEPB method for a polycrystal
with large grain size was due to the fracture surface traction behind the
front port.ion of the pop-in precrack.

The SEPB and SEVNB specimens of alumina polycrystal with large

grain size were provided for a stable fracture test in bending. Because
unstable fracture often occurred during the bend test, a new type of
crack stabilizer was applied to improve the stability of the fracture
process. The KIO values at the initiation of the crack was det.ermined by
the point where the compliance of the specimen changed with accompanied
by AE. In t.he present investigation, it is concluded that the KIC values
can be overestimated when the SEPB lIwthod is applied to R-curve materi-
als.

ACKNOWLEDGMENT

We thank Dr. M. Sakai (Toyohashi U. T.) for his kind discussion of

crack stability. We also express our gratitude to Mr. Awa.ji (.JFCC) for
pl"(~paratioll of SEVNB specimen.

REFERENCES

I) R. Warren and B. Johanneson, Powder Metal.,~}, 25(1984).

2) T. Sadahiro, J ..lpn. Soc. Powder and Powder Metal., ~, 422(1986).
3) T. Nose and T. Fujii, J. Am. Ceram. Soc.,7.!. 328(1988).
4) A. G. Evans and E. A. Charles, ibid., 59, 371(1976).
~j ) B. IL Lawn, A. G. Evans and D. B. Marchall, ibid., 63, c-182(l980).
6) K. Niihara, R. Morena and D. r. H. Hasselman, J. Mater. Sci. Letters,
(, 13( 1982).

285
 7) T. Nishida, T. Shiono and T. Nishikawa, .J. Ceram. Soc..lpn., Ii!;!, 604
(J 988).
R) T. Nishida, '1'. Shiono and '1'. Nishikawa, J. Europ. Ceram. Soc., l2, 379
( 1989).
9) T. Nishida, A. Nagai, T. Shiono and '1'. Nishikawa, J. Ceram. Soc..Jpn.,
9a, a96(1990).
10) D. Munz, IL '1'. Bubsty and J. L. Shannon, Jr., .J. Am. Ceram. Soc., ~;},
:mO(1980).
11) (0'. t·;. Buresc.;h, "Fracture Mechanics Applied to Brittle Materials", Ed.
by S. W. Freiman, ASTM STP-678(1979), 1'.151.
12) S. J. Burns and M. V. Swain, .J. Am. Ceram. Soc., Q\3, 226(1986).
13) A. G. Evans, ibid., 7.J, 187( 1990).
14) R. W. Rice, S. W. Freiman and .J. .J. Mechoiski, .Jr., ibid., §~, 129
(1980).
15) 1. Takahashi, S. {Jsami, K. Nakakado, H. Miyata and S. Shida, J. Ceram.
Soc..Jpn., 93, 186(1985).
16) H. Awaji and Y. Sakaida, .J. Am. Ceram. Soc., 13, 3522(1990).
18) P. L. Swanson, C. J. Fairbarks, B. R. Lawn, Y. W. Mai and B. J.
Hockey, ibid., 70, 279(1987).
19) R. W. Steinbrech, A. Reichl and W. Schaarwachter, ibid., 7J, 2009(1990).
20) M. Sakai and M. Inagaki, ibid., 72, 388( 1989).
21) T. Nishida, 1. Kameyama and T. Nishikawa, J. Soc. Mater. Sci. Jpn.,
4Q,411(1991).

APPf<;NDIX

Stability of brittle materials against fracture can be discussed by

cOllsi<kring the change ill free energy of both linear elastic specimen and
tl'sting llIaehine. Sakai ct a1. 20) succeeded in the explanation of the
fracture phenomenon in a perfect €~lastie material, from the most l1eneral
point of view, by introducing the concepts of dimensionless load (P) and
<Iilllcllsionle:;s load-point displacement (Li). They are respectively ex-
pressed as:

-=
I' 1 / Y(il~) (1)

U .::L((x) / Y(a) (2)

where the relative crack length (a) is given by the ratio a/W between
craek length (a), and specimen width (W). The parameter A (ex) repre-
sents the dimensionless compliance, and Y( a) is a shape factor defined
by the following relation:

Kr = (1' / BWI/2)'Y(a) (3)

where P and B are applied load and specimen thickness, respectively.

The total compliance <C(a» in an ordinary fracture test can be described
by a spring system arranged in a series of specimen compliance (Csp(a»)
and machine compliance (C m) as follows:

<C(a) > = Csp(a) + em (4 )

or

<A (a) > = A sp( a) + A m (5)

AI
Dimensionless equilibrium Gibbs free energy (Geq) of a specimen
during fracture test is expressed as follows:

Geq = (1/2)<A (a »p2 + (A - Ao) / BW (6)

286
where <A (ex) > is the resultant dimensionless compliance defined by
A (a) = C(a)BE', A and Ao are the fracture surface area and its initial
value, respectively, and E' is Young's modulus of the specimen.

Examples of the change in Geq during fracture of a specimen

loaded according to the JIS method are shown in Fig. 8. They are exam-
ples of the computer simulation for idl~ally stiff testing machine (.l m = 0),
usual machine (). m = 45) and soft machine ()... = gO) models. Although, a
dimensionless machine compliance (.1 m) around 45 is representative of a
fairly soft machine. This choice was done instead of considering the full
rigidity of the testing machine, because Uw maximum fracture load in
bending generally within in a few kgf for SErB test according to .J13 R
1607. 'rhesl' computer simulations for fracture stability represent only a
necessary condition for ideal Klc constant material. Larger positive
values of the slope (dGeq,!da) are a desirable condition to attain stable
fracture of actual ceramics, because of Uw d istri bu tion of the local KIe at
the crack front.

The crack stabilizer used in this work is shown in Pig. glIl. 1\

pair of elastic l'E!ctangular specimens without precrack or notch were
arr'anged on both sides and parallel to a SEPB specimen. Only the pre-
cracked specimen was found fr'actured by loading the ali system of
specimen and stabilizers. The resultant dimensionless compliance <.1.. (IX»
and the applied load (P) rl'presentcd in Eq. (6) for the compositp spring
system of Fig. 9, must be replaced by Eqs. (7), (8), respectively.

<A ( a )> = A m + A sp( ex ) • A ,,1 / (A "1. + 2A st( ex )) (7)

P= ((/Lsl. + 2,LsP(a)) / A"1)'I'sp (8)

The A"t is the dimensionless compliance of a stabilizer bar. I n the

case of a system for a bend-bar spec:imen with stabilizers (A"t = 30, 45)
with gf!Ometry according to Fig. g, the change ill Ceq during crack exten-
sion of a specimen by using usual machine (A m = 45) can be simulated as
shown in Fig. 10. It is clear that by applying stabilizers maximum bene-
fit for crack stability is obtained in the case of long crack size.

0,8.--------------,

>-
en
~ 0.6
cQ)
QJ

....
Q)
'-
VI
il 0.4
i.5

0.2 "--7--~_=_--~_=_----J.
0.4

Fig. 8 Equilibrium crack growth diagrams of a .JlS It 1607 spec:imen

tested by stiff machine (.l m = 0), usual machine (;t m = 45)
and soft machine (/\. m = 90).

287
 Fig. 9 Schematic drawing of crack stabilizer for bend-bar specimen and
its resultant spring system.

100.---------,...--~-~

\1.:) 80
>.
0>
c...
QJ
ffi 60
QJ
QJ
c...
..... 40
VI
.D
.0
15 20

0 0 .4 0.6 0.8
Relative crack length, a.

Fig. 10 Equilibrium crack growth diagrams of a JIS R 1607 specimen

tested by usual machine P. m = 45), and of the specimen with
crack stabilizer (A.,,'t = 30, 45) as shown in Fig. 9.

288
EVALUATION OF CRITICAL DEFECT SIZE OF CERAMICS

BASED ON R-CURVE METHOD

Keisuke Tanaka,* Kenji Suzuki,

** and Hiroshi Tanaka *
* Faculty of Engineering, Nagoya University
Nagoya 464-01, Japan
** Faculty of Education, Niigata University
Niigata 950-21, Japan

INrrRODUCTION

The fracture toughness of ceramics is as low as one tenth or one hun-

dred of that of metallic materials, and the critical size of defects for
fracture of ceramics is normally less than 0.1 rom. Therefore, the conven-
tional methodology of fracture mechanics often becomes inapplicable; the

critical value of the stress intensity factor (SIF) is dependent on the

defect size. Engineering approaches proposed to the size effect of the

. . 1 SIF va 1 ue are t h
cr~t~ca '
e po~nt stress mode 11 , the average stress model 2 ,
3
and the fictitious crack mode1 ,4. Although, they show some success in

correlating the defect size to the fracture strength, the underlying phys-
ical meanings are unclear. In the present paper, the fracture strength of
ceramics with small defects is evaluated based on the R-curve method.

R-CURVE METHOD
Shape of R-Curve

The resistance for crack growth in ceramics in most cases increases

with increasing crack length. According to several models proposed for

increasing resistance, the resistance K will be expressed by the follow-

R
ing equation:

K + K + K (1)
Oms

Fracture Mechanics of Ceramics, Vol. 9

Edited by R.C. Bradt et ai., Plenum Press, New York, 1992 289
where K is the fracture toughness of single crystals, K is the contribu-
O m
. . . 5,6 d .
tion by the m1crostress, m1crostructure, or gra1n structure , an K 1S
s
7
due to the crack-tip shielding by grain bridging , microcracking 8 , or
. 9.
transformat1on 1n the crack wake.

The shape of the R-curve depends on the mechanisms operating in the

fracture process of ceramics. By neglecting the contribution of K , the
m
R-curve will have such a shape as shown in Fig. 1. For a crack exten-
sion, c, less than c , K is equal to K ' while K reaches to a fracture
1 R O R
toughness of a long crack Koo at c larger than c • The c value is re-
2 2
garded as the transition crack length from short to long cracks. Cook et
10
al. proposed the following R-curve equation for a half penny-shaped
crack:

(2 )

11
and Mai and Lawn derived

(3)

for a through-the-thickness crack.

Koo
Q)
u
c
o
+-
(f)
(f)
Q) Ko
a::

C2

Crack length increment, C

Fig. 1. Resistance curve.

290
 A similar transition behavior from short to long cracks was found by
l2
Tanaka and Akiniwa in their study of a fatigue crack propagation from a
notch in metallic materials. The increase of resistance for a fatigue
crack growth is caused by the development of crack closure or contact
shielding. They proposed the following R-curve equation for crack length
between c and c :
1 2

(4 )

3
\ Moi-Lown(Penny-shoped crock)

0
~
""- 2
~

<J.i
u Moi-Lown(Through crock)
c
0
+- Tonoko(Through crock)
U)
U)
Q) Ko=1.73MPoVi'ii
0::: K,,=4.08MPoVi'ii
d=2~m
cl=4 Jim
C2=420Jim
0
0 5 10 15
Crack length, C/Cl
Fig. 2. Resistance curve for alumina with the grain size
of 20 ].lm.

From the fracture tests of alumina (the grain size = 20 ].lm) with a
IO
micro-Vickers indentation, Cook et al. determined the values in eqn (2)
as C =40 ].lm, c =420 ].lm, K =1.73 MPa~ and K =4.08 MPa~. The R-curves
1 2 O oo
given by substituting these values in eqns (2), (3), and (4) are shown in
Fig. 2. The increase of K is steeper in eqns (2) and (3).
R

Determination of Crack Extension Condition

When the SIF value applied as a crack driving force, K , is larger

A
than K , a crack can extend. The K value is given as the sum of the SIF
R A

291
values due to the applied stress, K , and due to the macroscopic residual
a
stress, K •
r

K + K ( 5)
a r

Figure 3 illustrates the determination of the crack extension condition by

the R-curve method. The condition for crack initiation is not taken into
account in Fig. 3. Some other criterion may be necessary. The lowest
stress 01 required for possible crack extension is the stress which passes
the point of K = K at c = c as shown in Fig. 3. The stress 02 is the
R O 1
stress required for unstable fracture.

RELATION BETWEEN CRITICAL STRESS AND DEFECT SIZE

Penny-Shaped Crack
By using the R-curves of eqns (2) and (4) with the values of alumina
10
reported by Cook et al. , the fracture strength 0B (equal to 02 in Fig.
3) for unstable fracture was calculated for a penny-shaped pre-crack. The
pre-crack is assumed to have no shielding or bridging. The srF value of
a penny-shaped crack with a radius, t, is

K = O&F (6)

where F = 2/TI. The equivalent crack length t was calculated by

eq

K 0v'TIteq = 0& F (7)

2
t tF (8)
eq

The relation between 0B and t is shown in Fig. 4(a). The critical srF
eq
value was calculated by

Koo

t Cl C2
Defect size

Crock length, C

Fig. 3. R-curve method to determine crack extension condition.

292
 500 ,---.----.-rTTTTTI"'""----r--r-T"TT"TTTT-,-,---,,"TTTTl

400 \Ko ". Ka,

~

o Mai-Lawn
~ 300
t3 --- " Tanaka

~ 200
+-
Ol '.
c: '.
Q)
L
+-
(f)

Q)
L 100
:=l
+-
U
o
L
u..
50 L...-....l..-....L.....l...J....I.J..l.LL-----'L.......J......L...L..LU.J..L-..--'-....L......I....Ll.JL..LlJ
0.1 10 100
EquivaLen defect Length. teq/d

Fig. 4(a). Effect of R-curve model on the relation between

fracture strength and equivalent defect length.

Penny-shaped crack
5r---r-.....-r..,..,-rrrr-,---,r-r-rTTnr----,-,-rrTTm

4.08MPavm - - - - - - - - - - -
4

~o 3
a..
2
~ 2

d=20jim
cl=40jim
c2=420jim

10 100
EquivaLent defect Length. teq/d

Fig. 4(b). Effect of R-curve model on the relation between

critical stress intensity factor and equivalent
defect length.

293
 Penny-shaped crack
600
500 -~----- -......
'.Ko,
Ko=1.73MPavm
'0 ~
·~.,Ko . . . " ",
0.... 400 K..=4.08MPavm
~
.'.. " ,,",
'
d=20pm
' '-,
300 cl=40pm
~

'\
~ "" ~,
c2=420pm
r;;
of-
200 ",,-,"",
Ol Detect without
C
<ll
L
bridging " \.~
of-
<Il '\
<ll
Detect with bridging
100 '"~ "-
L
:::J
of-
U
0
L
u.. ~,
~

50
0.1 10 100
EquivaLent defect Length, teq/d

Fig. 5. Effect of defect character on the relation between

fracture strength and equivalent defect length for
penny-shaped crack.

294
 (9)

where t is the initial defect size. Figure 4(b) shows the variation of K
c
with t . The strength calculated for small cracks by Mai-Lawn model,
eq
eqn (2), is larger than that by Tanaka-Akiniwa model, eqn (4). For large
cracks, K approaches to Koo in both models; the crack length at the ap-
c
proaching point is smaller for Mai-Lawn model. It may depend on the crack
nucleation criterion whether K can be lower than K or not. Both models
c O
nicely show that the fracture condition is the critical stress at small
cracks and the critical SIF at large cracks. This type of transition has
. .
b een reporte d f or varlOUS .
englneerlng ceramlCS 1,3,4 In the o
f 11 oWlng,
.

Mai-Lawn model will be used for further discussion.

13
A pre-crack can have grain bridging on its crack face , while it is
assumed to be free from bridging in the above analysis. In Fig. 5, the
fracture strengths calculated for two types of pre-cracks are compared. A
pre-crack with bridging gives a higher strength, and the region of a con-
stant strength is wider. K approaches Koo at shorter crack lengths for a
C
bridged pre-crack.

For several values of c ' the fracture strength was calculated for a
2
penny-shaped pre-crack without bridging and the results are shown in Fig.
6. The 0B value at small pre-crack length is larger for smaller c
2
values. The crack length at which K approaches to Koo is longer for
c
larger c values.
2

Penny-Shaped crock
500
400
--- ...:':: --........
.....
',K...

"6 300
-- --
.... .... ---- C2=2CI
Il- - - C2=10.5Cl
"" -,-C2=50Cl
""
.............. ' .~, ""
~ -..:'->:- ""'. .
.c 200 ...... "",.'. '
+- , ". ,',
",',v.,.
01
C .......
Ql
"- Ko......•......
,.<.
" ".
+- ~.
oJ)

".,.~\.
Ko=1.73MPovm
Ql
L
~
100 K",=4.08MPavm
'~
+-
0
d=20/lm

'.
cl=40/lm
0
"- ".~
".'100
LL "
50
0.1 10
Equivalent defect length, teq Id

Fig. 6. Effect of transition crack length on the relation

between fracture strength and equivalent defect
length for penny-shaped crack.

295
Elliptic Crack

For elliptical cracks with various aspect ratios, t/£ (t = half minor
axis, £ = half major axis), the fracture strength 0B is plotted against
the equivalent defect length, t , in Fig. 7. To calculate t , F=l/E(k)
eq eq
is used, where E(k) is the complete elliptic integral of the second kind
with an argument k = [1_(t/£)2]1/2. The crack extensions at the tips of
the minor and major axes are assumed to be independent. The aspect ratio
is reduced with crack extension. In Fig. 7, it is worthy to note that the
relation between 0B and t is almost identical for aspect ratios between
eq
1 and 0.3. This supports the use of the equivalent defect size to take
. 1,3,4
into account of the geometry d~fference of defects •

Spherical Void

The R-curve method was applied to spherical voids. The fracture

2
strength calculated is plotted as a function of t = tF (F = 2/n) in
eq
Fig. 8. The SIF value is

K
=-
ovnc [1.12 - 0.31 Xtan -1 (cit)]

x {I + [(4-5V)c+~/tr + 9~1+~/trJ /2(7-5V)} (10)

14
for an anular crack with length c. For a semi-circular crack at the
15
void surface , it is

K 0 & .: [1 + (K -1) 1 ] (11)

" t l+c/t

where K is the stress concentration factor given by the following func-

t
tion of Poisson's ratio V:

(27-15V) / (14-10V) (12 )

The former equation is appropriate for small voids, while the latter for
large voids. As seen in the figure, the fracture strength is nearly the
same as that for a penny-shaped crack for small voids. At larger voids,
it approaches to a constant value which is equal to the strength of flaw-
less materials divided by the elastic stress concentration (K = 2.01 for
t
V = 0.23).

Elliptic Hole
The fracture strength of a plate with a through-the-thickness ellip-
tic hole (whose half length is 10 mm) is also calculated by the R-curve

296
 Elliptic crock

~ 300 -... •• -.....:..::;..KO •.. t<.., ~

0.10: "
a
n.. .. '-.::::". . . - N
2
200 2l
~ 0.2 ~~ " .
.r::
+-
01 0.3 "'~'"
~ 100
L..
10
. Aspect ratio (til) ." . '~'"
+-
ff)

Q)
L.. Ko=1.73MPoVlTl'
::J
+-
Ko,=4.08MPoVM
U d=20ym
"
L..
LL
c\=40/lm
c2=420pm
30 '-----'-.J........L..L.LLUJ-----L---L.....L..L.J...u..u_...l-L...L.JL..l...L.UJ
O. I 10 10C
Equivalent defect length, teq/d

Fig. 7. Effect of aspect ratio of elliptic crack on the

relation between fracture strength and equivalent
defect length.

Spherical void
400 r-""-;-rnrTTTrr-":T""T""rrrn.,.,.----,--r-r'TTTTTl

, Spherical vaid
!S1 ... Evans's eq.
u
.r::
200 ,
~
--'-- \
'., --\.._------
....
Ol .~ .. SphericaL void
C
Q)
~. \, Borrotto's eq.

.~.\
l-
+-
ff)

.~. ~--.-
~
::J
100
+- Ko=1.73MPaVlTl'
U
a Ko,= 4.0 8MPoVlTl'
l- d=20/lm Penny-shaped
LL crock
cl=40/lm
c2=420pm
50 '-:---'----L....l-J...LLJ..ll----"--I....J.-l..J..J.J..l.L---I.-l-.Ll.J..1ilJ
O. 1 10 100
Equivalent defect length, teq/d

Fig. 8. Relation between fracture strength and equivalent

defect size for spherical void.

297
method. The SIF value at fracture is calculated by

K (13)
P

Figure 9 shows the change of K with the square root of the notch-tip ra-
p
dius. When the tip radius is smaller than a certain critical value, the
K value takes a constant value nearly equal to the critical SIF value for
p . 1,16
a pre-crack. Similar results were reported for notched ceram~cs

The critical value of the notch-tip radius is longer for larger c values.
2

MONTE CARLO SIMULATION OF BENDING FRACTURE

A Monte Carlo simulation of bending fracture of alumina was conducted

4
by using the technique developed by Hoshiide and Inoue The specimen is
a rectangular beam which has a width of 4 mm, a height of 3 mm, and a
length of 20 mm and is subjected to pure bending. Penny-shaped cracks
were distributed randomly in the specimen by a computer and the defect
size was also a random variable following the cumulative distribution
. 16
f unct~on;

(14)

where to is the smallest defect size and a is a shape parameter. Figure

10 shows the distribution for various a values. For a larger a value,
the size distribution is more concentrated near to.

el/
Elliptic hole. size t=10mm
~0 50
0...
~ Ko=1.73MPal/iTi
0
Kro =4.08MPal/iTi
:.:: d=20~m 2t ,-'-
,-
.:
0
cF40~m
,-
,/
./
+- ,/ /'
u
0 10 ,/
,/ "",,'
,"
"""
't-

>, ,/ /'
+- "
(J)
c
Q)
+-
_______ ::.::.::.~=_.//~g~~fO~~Cl
C2=50Cl
.S:
(J)
(J)
Q)
L-
+-
IJ)

1
0.5 1 10 50
Square root of notch-tip radius, "pi d

Fig. 9. Effect of notch-tip radius on the critical stress

intensity factor for elliptic hole.

298
 ....
~

I 0.8 I
/
I
/
/' -
-- --~--

....>. I
I
0(=6
~

:0 I 0(=4
c
.0
0.6 I 0:::=2
0
l-
0-
I
I
I '
/
(1)
0.4- I /
....>c I,
I I
I' H(t)=HtItof OC
I
~

~
E 0.2
i
~
u

0
0 2 3 4- 5
Defect lengt~ t/to
Fig. 10. Cumulative probability function of crack length.

~-Effi
+- --------<---------
Neutral axis

Fig. 11. Crack location in a bend. specimen.

299
 Figure 11 shows three types of cracks: inner crack, surface crack,
and corner crack. For surface and corner cracks, the SIF value is evalu-
ated at the surface and the deepest point, and the cracks are assumed to
grow semi-elliptically and quarter-elliptically. For inner cracks, the
SIF value is evaluated at the points nearest and farthest to the surface,
and the crack is assumed to remain circular as it grows.

After giving a defect distribution to a specimen, let each defect

grow independently under the applied bending moment. The resistance
10
curve used is that reported for alum~na The distribution of defects
projected on a plane perpendicular to the stress direction is shown in
Fig. 12, where a=4, to=lO ~m in eqn (14) and the crack density is S3/mm3.
The circles enclosed with the full line are the initial defects, and those
with the dotted line are the final shapes when a surface crack (denoted by
A in Fig. 12) becomes unstable. For the compression side, only the loca-
tion of defects is indicated with the dots. The defects near the neutral
axis do not show any growth.

The simulation was repeated for thirty specimens, each of which has a
different set of defects. The relation between the bending strength 0B

and the equivalent defect size t is shown in Fig. 13, where t is cal-
eq eq
culated from the initial size of the defect which causes fracture in each
specimen. The simulation was conducted for the two types of defects: the
one without bridging and the other with bridging. The latter type of de-
fects gives a higher bending strength. The bending strength is nearly

Neutral axis

Compression side

Fig. 12. Distribution of simulated cracks.

300
 Equivalent defect length. teQ (urn)

Fig. 13. Relation between bending strength and equivalent

crack length for penny-shaped crack.

301
 99
o Detect without
bridging
•
• De f~et WIt h
bridging
C
lJ.. 50
>,
+-
:::;
:n0
.&J Ko=1.73MPoVlTr
0
'- K.,=4.08MPoVlTr
a. d=201lm
10
3
'"
'- c,=401lm
c2=4201lm
'0 to= lOllm
lJ.. a: =4
Pc=8/mm

1
100 4D0

Fig. 14. Failure probability of bend specimens with

simulated crack distribution.

constant for small defects, and gradually approaches to the line of the
constant K value, Koo ' with increasing defect size.

Figure 14 shows the cumulative probability of the fracture strength

derived from Monte Carlo simulation. The straight lines in the figure
give the two-parameter Weibull distribution

(15 )

where m=15, 00=248 MPa for defects without bridging and m=38, 00=323 MPa
for defects with bridging.

CONCLUSIONS

The effects of various kinds of defects on the fracture strength of

ceramics were studied on the basis of the R-curve method proposed by Mai
and Lawn for grain bridging in alumina. The results are summarized as
follows:

1. For penny-shaped cracks, the fracture strength is constant for small

defects and the critical stress intensity factor constant for large de-
fects. The equivalent defect size is an excellent parameter to correlate
the fracture strength of elliptic cracks with an aspect ratio between 0.3
and 1.

2. For small voids, the fracture strength is nearly the same as that for
a penny-shaped crack. For larger voids, it approaches to a constant value

302
which is equal to the strength of flawless materials divided by the elas-
tic stress concentration factor. When the tip radius of deep notches is
small, the critical stress intensity factor is independent of the tip
radius.

3. A Monte Carlo simulation of bending fracture of alumina was performed

by distributing randomly penny-shaped cracks with random sizes in a speci-
men by a computer. Based on thirty runs of fracture simulations, the re-
lation between the bending strength and the defect size, and the cumula-
tive distribution function of the fracture strength were successfully de-
rived.

REFERENCES

1. S. Usami, H. Kimoto, I. Takahashi, and S. Shida, Strength of ceramic

materials containing small flaws, Eng. Fract. Mech., 23, 745
(1986) •
2. H. Neuber, Theorie der Spitzkerben, in: "Kerbspannungslehre", 2 Aufl.,
Springer-Verlag, Berlin, (1958).
3. K. Suzuki, K. Tanaka, Y. Yamamoto, and H. Nakagawa, Effect of grinding
residual stress on bending strength of ceramics, J. Soc. Mater.
Sci. Jap., 38, 8 (1989).
4. T. Hoshiide and T. Inoue, Simulation of anomalous behavior of a small
flaw in strength of ceramics, Eng. Fract. Mech., 38, 307 (1991).
5. R. W. Rice, S. W. Freiman, and J. J. Mecholsky, Jr., The dependence of
strength-controlling fracture energy on the flaw-size to grain-size
ratio, J. Am. Ceram. Soc., 63, 129 (1980).
6. A. G. Evans, A dimensional analysis of the grain-size dependence of
strength, J. Am. Ceram. Soc., 63, 115 (1980).
7. P. L. Swanson, C. J. Fairbanks, B. R. Lawn, Y.-W. Mai, and B. J.
Hockey, Crack-interface grain bridging as a fracture resistance
mechanism in ceramics: I, Experimental study of alumina, J. Am.
Ceram. Soc., 70, 279 (1987).
8. A. G. Evans and K. T. Faber, Crack-growth resistance of microcracking
brittle materials, J. Am. Ceram. Soc., 67, 255 (1984).
9. M. V. Swain and L. R. F. Rose, Strength limitations of transformation-
toughened zirconia alloys, J. Am. Ceram. Soc., 69, 511 (1986).
10. R. F. Cook, C. J. Fairbanks, B. R. Lawn, and Y.-W. Mai, Crack resis-
tance by interfacial bridging: Its role in determining strength
characteristics, J. Mater. Res., 2, 345 (1987).
11. Y.-W. Mai and B. R. Lawn, Crack-interface grain bridging as a fracture

303
 resistance mechanism in ceramics: II, Theoretical fracture mechan-
ics model, J. Am. Ceram. Soc., 70, 289 (1987).
12. K. Tanaka and Y. Akiniwa, Resistance-curve method for predicting prop-
agation threshold of short fatigue cracks at notches, Eng. Fract.
Mech., 30, 863 (1988).
13. S. J. Bennison and B. R. Lawn, Role of interfacial grain-bridging
sliding friction in the crack-resistance and strength properties of
nontransforming ceramics, Acta Metall., 37, 2659 (1989).
14. F. I. Baratta and A. P. Parker, Mode I stress intensity estimates for
various configurations involving single and multiple cracked spher-
ical voids, in: "Fracture Mech. Ceramics,S", 543 (1983).
15. A. G. Evans, D. S. Biswas, and R. M. Fulrath, Some effects of cavities
on the fracture of ceramics: II, Spherical cavities, J. Am. Ceram.
Soc., 62, 101 (1979).
16. H. Awaji and Y. Sakaida, V-notch technique for single-edge notched
beam and chevron notch method, J. Am. Ceram. Soc., 73, 3522 (1990).
17. M. Ichikawa, On reliability analysis of ceramics under multi-axial
stress states (1st report: Examination of application of two-
parameter Weibull distributions), Trans. Jap. Soc. Mech. Eng., 51,
2368 (1985).

304
CRACK WAKE EFFECTS ON MgO FRACTURE RESISTANCE

J. LLorca* and T. Ogawa t

*Department of Materials Science. Polytechnic University of Madrid

ETS de Ingenieros de Caminos, 28040 - Madrid, Spain
tDepartment of Mechanical Engineering, Gifu University
1-1 Yanagido, Gifu, Japan

INTRODUCTION
The effect of the interaction between the crack surfaces on the fracture be-
haviour of monolithic ceramics has received considerable attention in recent years.
Most of this work has been carried out on polycrystalline hcp materials, such as alu-
mina, and today there is wide experimental evidence that the fracture resistance is
mainly due to phenomena which take place in the crack wake, such as grain bridging
and grain pull-out 1-3. Interaction between the crack surfaces in the crack wake
has been observed when the mechanism of crack propagation was intergranular and
transgranular, and this is responsible for various experimentally observed behaviours.
For instance, the crack growth resistance increases with crack length 2-6, as the in-
teraction zone develops, and also with ceramic grain size 2,5-7, because the larger
the grain, the more energy is dissipated by friction in the crack wake. In addition, as
the crack opening displacements in ceramics are small, the interaction zone can be
up to several millimeters in length. When specimen dimensions and crack length are
comparable to the interaction zone length, the crack growth resistance is no longer a
material property and becomes dependent on the specimen geometry 5-6 and on the
loading conditions 8.
Several physical mechanisms have been proposed to explain the development
of closure forces in the crack wake 2 • As the crack propagates, some grains remain
unbroken, giving rise to elastic bridges which exert a closing force on the crack sur-
faces. Further crack growth leads to the fracture of these bridges, by either grain
or interfacial fracture. The closure forces behind the crack tip are influenced by
grain morphology and size, as the grains often have to rotate before being pulled out
from one surface, and by the internal residual stresses left by the anisotropic thermal
shrinkage of grains after sintering, which enhance energy dissipation during grain
rotation and pull-out.
The work referenced above has been performed on alumina, but cubic ceramics
do not exhibit the behaviour which is typical in materials toughened by crack wake
interactions. Specifically, the fracture energy does not show an increase with average
grain size in dense polycrystalline Mg0 7 ,9-1o and ,8-SiC 7 , and stable quasi-static

Fraclure Mechanics afCeramics, Vol. 9

Edited by R.C. Bradt el al., Plenum Press, New York, 1992 305
crack growth from a notch root is very rarely seen in polycristalline MgO, being
limited to one grain dimension before the crack becomes unstable and catastrophic
failure takes place l l . Although grain pull-out has been observed in the fracture
surfaces11 , dislocation movement is considered the main toughening mechanism in
MgO at ambient temperature. Evidence of plastic deformation around a notch tip has
been reported11-12, and Evans12 carried out an estimation of the energy dissipated
by dislocation movement. The results of this study are in good agreement with the
measured values of polycrystalline MgO fracture energy10.
The main aim of this work was to study the quasi-static, stable growth of cracks
in polycrystalline MgO under different loading conditions: tension, cyclic compres-
sion, and cyclic tension. The results related to tension and cyclic compression are
presented here, whereas the cyclic tension behaviour is addressed in another paper
in these proceedings 13 .

MATERIAL AND EXPERIMENTAL TECHNIQUES

Polycrystalline MgO, commercially available from Custom Technical Ceram-
ics, Arvada, Colorado, was used in this investigation. The main impurity added as
a sintering aid is 2.3% Y203. Sintering temperature was 1560 0C and the flexural
strength, as reported by the manufacturer, is 227 MPa. The material density was
3400 Kg/m 3. The microstructure included two populations of grains, the first with
an average grain size of 2 f.1.m (60%) and the other with grain sizes ranging from 6
to 8 f.1.m (40%). The Young's modulus, E, was experimentally determined, giving a
value of 258 GPa.

d = 25 mm

1
ao = 17.6 mm. -

r ~O
14m m.

l Q6smm
J
3 0 mm. 50 mm.

31 mm.

I=
d 10
I
mm.

(a) CT (b) SEN

Fig. 1. Specimens tested. (a) Compact tension (b) Single-edge notch.

One compact tension (CT) and three single-edge notch (SEN) specimens were
machined to the dimensions depicted in Figures la and Ib respectively. Specimen
thickness was 5 mm in all cases. The notch thicknesses were 0.4 mm and the notch
tips were approximately semicircular, with a notch tip radius of 0.2 mm. Initially, all
the specimens were subjected to fully compressive far-field cyclic loads at a frequency

306
of 10 Hz to introduce a sharp crack at the end of the notch root 14. The maximum and
minimum loads in each cycle were -0.637 KN and -6.37 KN respectively for the SEN
specimens, and -1.56 KN and -15.6 KN for the CT samples. Tests were stopped aSter
20.000 cycles. It was assumed, following the experimental observations presented by
other authors 14 , that the crack length reaches a saturated value after a few thousand
cycles.
After precracking in cyclic compression, specimens were tested in tension and
bending in a screw-driven test machine to study quasi-static crack growth. Two holes
were drilled in the CT specimen to apply the tensile loads, as depicted in Figure 1a.
For the single-edge notch specimens, three different loading systems were used, i.e.
uniaxial tension (SET), three-point bending (TPB) and four-point bending (FPB). In
the case of the FPB test, the outer span between supports was 40 mm and the inner
span 20 mm. The TPB test was carried out with a span of 40 mm between supports.
The tests were carried out under stroke control, with an applied displacement rate of
2.54 pm/min, until the crack became unstable, and catastrophic failure took place.
Fracture surfaces were observed in a scanning electron microscope to ascertain the
main features of crack propagation.
Load and quasi-static crack length increments from the fatigue crack tip were
monitored during the test, the latter by using a surface film technique previously
developed by one of the authors l5 . In this technique, a layer of carbon is sputter-
deposited on the specimen surface (by vacuum evaporation) which atomically bonds
the carbon film to the specimen surface. The propagation of a crack fractures the
carbon film and the crack length increment can be related to the changes in the elec-
trical conductivity of the carbon layer. The measurement of the electrical resistance
of the carbon film during the test is carried out by connecting the film to a bridge
circuit. Crack length increments of several microns can be detected with this system.

RESULTS
Crack growth under cyclic compression was observed in the four specimens,
but the crack length increment, b.acf' was different in each case (see Table 1). The
cracks grew uniformly through the specimen thickness. Post-mortem scanning elec-
tron microscopy of the fracture surfaces showed that the crack growth was mainly
transgranular and that debris particles were present on the fracture surfaces (Figure
2a). The debris particles were concentrated around raised fractured grains on the
fracture surface (Figure 2b), indicating that contact between the crack surfaces took
place during crack propagation. The porosity of the material can also be observed in
Figures 2a and 2b, the pores being within the grains and at the grain boundaries.

Table 1. Quasi-static stable crack growth lengths in MgO

under different loading conditions
Specimen b.acf b.at yO
\R
(pm) (pm) (MPa m 1 / 2 )

TPB 80 26 0.75
FPB 100 39 0.79
SET 130 109 0.82
CT 200 552 1.19

307
 Fig. 2. Fracture surface in cyclic compression, show-
ing transgranular fracture and debris particles (a) Low
magnification (b) High magnification.

Quasi-static, stable crack propagation was also observed in tension and bending
in all cases. The fracture resistance, K R , was calculated from the external load
and the crack length by using the appropiate shape functions for the stress intensity
factors. The results are shown in Figures 3a and 3b, where K R is plotted vs. the
crack length increment from the compression fatigue crack tip. Stable crack growth
started when a critical initial value of the stress intensity factor, K~, was attained.
K~ was different in each specimen, increasing with the length of the compression
fatigue crack (see Table 1). Beyond this point, the fracture resistance increased with
crack length until a critical value K c was reached and catastrophic failure occurred.
K c was very similar in the four specimens, varying from 2.0 to 2.1 MPa m 1 / 2 . Taking
an average value of 2.05 MPa m 1 / 2 , and assuming plane stress conditions at the crack
tip, the fracture energy "I can be calculated according to

(1)

which gives 16.3 J 1m2 • This value is in agreement with others reported in the liter-
ature for polycristalline Mg0 7 ,lO-1l.

308
 2.5
a
2

'"
1.5
E
III
c.
==
a: -o-TPB
:ll:

-O-FPB
0.5
-o-SET

o0 0.02 0.04 0.06 0.08 0.1 0.12

M(mm)

2.5
b
2

-
~

'"
1.5
E
III
C.
~ 1
:ll:a:

0.5

00 0.1 0.2 0.3 0.4 0.5 0.6

M(mm)

Fig. 3. Fracture resistance curves in polycrystalline MgO (a) TPB,

FPB and SET specimens (b) CT specimen.

309
 The fracture surfaces created in tension showed transgranular crack growth
(Figure 4a) as did those in cyclic compression. Crack surfaces are mainly covered
by cleavaged grains which belong to the larger size population, indicating that they
are fractured more easily than the small ones. The crack plane changes from grain
to grain, due to the different orientation of the cleavage planes in each grain (Figure
4b). Debris particles were not found on the fracture surfaces, as they were in cyclic
compression. Moreover, the fracture surfaces in tension were microscopically flatter
than those in cyclic compression, as is shown in Figures 2a and 4a.

Fig. 4. Fracture surface in tension (a) Low magnification (b) High

magnification.

DISCUSSION
Cyclic compression
Our results clearly show that stable crack propagation can be achieved in
notched specimens of polycristalline MgO when they are subjected to fully compres-

310
sive cyclic loads. The propagation of cracks in brittle solids under cyclic compression
has been thoroughly analysed by Suresh and co-workers, who studied different ce-
ramic materials, including alumina l 4, Mg - PSZ 16 , and Si 3 N4 - SiC composites 17 .
From the mechanics viewpoint, stable crack growth in cyclic compression is always
associated with the presence of non-recoverable deformations around the notch root
during compression. This region is surrounded by an elastically strained material,
and upon unloading, the displacement compatibility between the elastic and non-
elastic regions leads to the development of large tensile residual stresses around the
notch tip, which give rise to the propagation of a crack. The crack can extend only
through the tensile residual stress dominated zone, and as compressive stresses are
dominant far away from the notch root, it is intrinsically stable. The physical mech-
anisms which generate non-linear irrecoverable deformations around the notch root
during compression depend on the material. Grain boundary microcracking in com-
pression has been identified in alumina, due to the combined effects of the stress
concentration at the grain boundaries (because of the anisotropic mechanical prop-
erties of adjoining grains), and the thermal tensile residual stresses which arise upon
cooling from the sintering temperature at the grain boundaries due to the different
crystallographic orientations (and, hence, different thermal expansion coefficients) of
the adjoining grains in hcp ceramics. Upon unloading, these microcracks may not be
fully closed, due to friction, and permanent deformations develop. Further evidence
of this behaviour can be found in the intergranular nature of crack growth in alu-
mina, and in the impossibility of propagating a stable crack in cyclic compression in
alumina single crystals, where there are no grain boundaries 14 .
Crack growth under cyclic compression in polycrystalline MgO is predominantly
transgranular, and no evidence of grain boundary failure is observed in the fracture
surfaces. Moreover, thermal tensile residual stresses in the grain boundaries are far
lower in cubic than in non-cubic ceramics because of the isotropic properties of the
grains. Thus, a different mechanism has to be found to justify this behaviour. It
is known that cubic ceramics can undergo plastic deformation at room temperature.
Evaluating the magnitude of the resolved shear stress to move dislocations within
MgO grains, Davidge 18 obtained a value of 90 MPa. Thus, dislocations can move in
favourably oriented grains at an applied stress of 180 MPa.
To ascertain the possibility of plastic deformation under the minimum (max-
imum in absolute value) compressive load, finite element analyses of the notched
geometries were performed. The material was assumed to be linear elastic, char-
acterized by its Young's modulus. Constant displacement boundary conditions at
the specimen ends were used to simulate the experimental set-up used to apply the
compressive loads. The elastic stress distributions perpendicular to the notch plane,
lJ yy , are plotted vs. the distance from the notch root, r, in Figure 5 for both speci-
mens. The CT specimen is likely to experience larger plastic deformations than the
SEN one. Also, dislocation movement is expected to take place through the ligament
in the CT geometry, whereas it will be confined in a region which extends up to 2
millimetres from the notch tip in the SEN specimens.
Upon unloading, tensile residual stresses will develop in the notch tip region,
in accordance with the mechanism mentioned above. The magnitude of the stresses
and the length of the tensile stress zone are difficult to evaluate because they depend
on various factors. First, the smaller the maximum compressive stress (minimum in
absolute value), the larger the tensile residual stresses 16. Second, the debris particles
in the crack wake lead to a crack closure effect, reducing the tensile residual stresses.

31 1
This effect was proved experimentally by Ewart and Suresh 14 , who showed that if
the debris particles are periodically removed during cyclic compression, the crack
grows longer. However, our numerical analyses do show that larger tensile stresses
are expected to appear upon unloading in the CT specimen. The experiments of
crack propagation under cyclic compression are in agreement with this result: the
crack propagated 200 Ji-m in the compact specimen and between 80 and 130 Ji-m in the
SEN specimens. The differences in the crack increment length in the SEN specimens
may be due to small variations in the notch tip geometry, which modify the stress
state near the notch root.

·800
FCll
~
-;-
Q.
·600
:IE
,..
0'" -400

-200

2 4 6 8 10 12 14
r (mm)

Fig. 5. Variation of the stress perpendicular to the notch plane, (J yy,

with the distance from the notch root, r, under minimum (maximum
in absolute value) compressive load.

A mechanism of fracture, which involves dislocation motion, was proposed by

Evans ll - 12 to explain polycrystalline MgO transgranular fracture in tension. Tensile
stresses can produce slip in suitably oriented grains. The dislocation movement is
stopped by grain boundaries, and grain boundary pile-ups form. Alternatively, pile-
ups can be developed at slip plane intersections. The stress concentration induced by
dislocation pile-up cannnot be relieved if the slip planes in the adjacent grain are not
adequately oriented, and a crack is initiated and propagates through the grain. The
same mechanism may be invoked in cyclic compression. The tensile residual stresses
generated during unloading are the driving force for dislocation movement. In each
cycle, the tensile residual stresses produce dislocation movement. When the critical
condition for fracture is reached in a grain boundary, the crack propagates through
the adjoining grain. As the crack propagates, however, the tensile residual stresses
are relieved, and the crack is stopped at the grain boundary. In the following cycles,
tensile residual stresses are again developed, and the whole process is repeated. The
overall observed behaviour is a slow crack growth. As the tensile residual stresses
diminish with the distance to the notch tip, the dislocation activity decreases with
crack length until the crack finally stops.

312
Tension
The experimental results presented in this paper show that slow, quasi-static
crack growth can occur in polycrystalline MgO under monotonic tensile load. More-
over, stable crack growth is accompanied by an increase in the crack growth resistance
until a critical value is reached. This behaviour is usually found in hcp ceramics but,
to the authors' knowledge, it has not been reported in cubic ceramic materials. The
aspect of the fracture surfaces created in tension is very similar to those reported
by other researchers U - 12 , and the magnitude of I agrees well with the estimations
made by Evans 12 , which assumed that dislocation movement prior to fracture is the
main mechanism of energy dissipation.
According to the mechanism outlined above, tensile stresses create dislocation
pile-ups at the grain boundaries until a crack is initiated. Once the crack has begun to
propagate, the energy release rate increases with the crack length because the external
load is constant, as opposed to the tensile residual stresses which vanish as the crack
grows. If the crack has propagated through a grain, it is very likely that it will break
the next one, and catastrophic failure will take place. The presence of stable crack
growth prior to fractureshows that another mechanism has to be active to restrain
unstable crack propagation. The existence of stable crack growth in hcp ceramics is
attributed to crack wake interactions, which in turn are due to the residual stresses
induced by the thermal anisotropy of the hcp crystals. We assume that a similar
mechanism is active in our case, but the origin of the residual stresses is different.
It has been shown that plastic deformation can take place during compression near
the notch root. However, as the number of slip systems in MgO crystals is reduced,
dislocations can move only in suitably oriented grains, whereas others do not undergo
plastic deformation. Upon unloading, the uneven deformation may induce residual
stresses in the grains. In some grains the remote tensile stresses are added to the
tensile residual stress field leading to grain fracture whereas other grains, in which
the tensile residual stresses are lower or compressive, remain intact in the crack wake.
These grains bridge the crack, reducing the severity of the stress singularity at the
crack tip, and have to be pulled out, consuming energy by friction. Both processes
contribute to an increase of the material fracture resistance as the crack grows, in
agreement with our experimental results.
Thus, the toughening mechanism observed in tension and bending tests comes
about as a result of the presence of large uneven residual stresses in the material,
similar to the one proposed for polycrystalline alumina by Vekinis et at. 2 , which also
exhibited transgranular fracture. The main difference is found in the origin of the
residual stresses, which lies in the thermal anisotropy of the grains in alumina and
in the not uniform plastic deformation under cyclic compression in magnesia. This
assumption also indicates that stable crack growth in tension will take place only in
the zone affected by residual stresses. Our experimental results are in agreement with
this fact. The CT specimen, which underwent more extensive plastic deformation in
compression, exhibits longer stable crack growth (see Table 1).
It should be indicated at this point that residual stresses are developed by cyclic
compression along the notch plane upon unloading, wherever plastic deformation took
place. Obviously, the closer to the notch root, the larger the residual stresses. In the
zone cracked in cyclic compression, the tensile residual stresses are large enough to
produce crack propagation. Far away from the notch, tensile stresses do exist but
they need the help of external tensile stresses to propagate the crack.
Another important feature of our experimental results is that stable crack

313
growth started only when a critical applied stress intensity factor at the crack tip,
J{~, was overcome. Although this can be due to several factors, a plausible explana-
tion can be found in the existence of frictional stresses between the fracture surfaces
created in cyclic compression. The dependence of J{~ on 6.a e j is in line with this
hypothesis.
MODELLING STABLE CRACK GROWTH IN TENSION
The cohesive crack model has been widely used to model the crack growth
resistance in monolithic ceramics toughened by crack wake interaction 5 - 6 ,19-20. As-
suming that the same mechanism is active in our material, an estimation of the
increase in the fracture resistance with crack extension can be obtained. The crack
growth resistance in a cohesive material for a crack which propagates in tension from
the compression fatigue crack tip is given by

'"
KR(a) = l a

ao+Aa c /
2a(x)
c;: . H(ald,xla) dx
y7l"a
(2)

where a is the crack length, d the specimen width (Figure 1), x is a dummy variable
that stands for the distance from the place where a cohesive force is applied to the
notch mouth, and H(ald,xla) the stress intensity factor shape function for a pair
of cohesive stresses a( x) acting on the crack surfaces. It has been shown 21 that if
the cohesive zone is small when compared with a, the shape function given by Tada
et ai. 22 for an infinite length beam with an edge crack is accurate enough for the
finite plates used in this investigation. The stress distribution in the crack wake
a( x) is obtained from the cohesive crack constitutive equation. Several constitutive
equations have been proposed in the literature for monolithic ceramics 5-6,19-20, and
all have in common that the stress transferred through the crack decreases with the
crack opening displacement w. There is no evidence that anyone of them is better
than the others, and we have arbitrarily chosen a power-law function expressed by

(3)

where a* is the limiting value for the bridging stress, We is the critical magnitude of
the crack opening displacement at which the interaction between the crack surfaces
vanishes, and n a fitting parameter. It seems reasonable in MgO to choose a* equal
to the flow stress (180 MPa). On the other hand, the area under the curve a = a( w)
has to be equal to " the experimentally determined fracture energy, which leads to
the relation,

(4)

We and n are not independent because of equation (4). Several pairs of valid We and
n values are given in Table 2.

Table 2. We and n values in polycrystalline MgO

We (pm) 0.091 0.181 0.272 0.453 0.543

n 0 1 245

314
 The calculation of the fracture resistance (equation 2) requires a knowledge
of the crack opening displacement W along the crack wake. w depends on both
the cohesive stresses and the external load, and it has to be evaluated following a
procedure previously developed by one of the authors 23-24. The details are not given
here and can be found in the quoted references.
The calculated fracture resistance curves for the SET specimen are plotted in
Figure 6 for different values of n. The results for the other geometries are not plotted
because they are practically identical to those of the SET specimen, due to the small
size of the cohesive zone when compared with the total crack length, a, and the
unbroken ligament, d - ao. The experimental results are plotted in Figure 6 as well.
The influence of n (or we) on the fracture behaviour is clearly observed in this Figure.
The experimental data for the TPB, FPB and SET specimens are close to the model
results obtained with low n (0 or 1) whereas the CT behaviour is better modeled
when n is 4 or 5. The higher the n, the larger the We, which leads to larger stable
crack increment. It has been previously pointed out that the development of cohesive
forces in the crack wake comes about as a consequence of the presence of not uniform
residual stresses. Our results seem to indicate that We increases with the magnitude
of the residual stresses. The CT specimen, in which residual stresses are maxima,
also exhibits the largest stable crack length increment.

2.5
n = n =5
2

--E
N

1.5
til
Q.

~
lr
~

0.5

0
0

Fig. 6. Experimental (thin lines) and calculated (thick lines) fracture

resistance curves in polycrystalline MgO.

At this point it is necessary to notice the main limitations of the model. The
contribution of the frictional stresses in the cyclic compression crack has not been
taken into account. This effect is likely to be important at the beginning of crack
propagation in tension, and explains the differences between the model and experi-
ments at the early stages of crack propagation. As the crack grows, and the crack
opening displacements increase, the energy dissipated by friction in the cyclic com-
pression crack should become negligible. Another important shortcoming is the con-
stitutive equation for the cohesive crack. The proposed function is reasonable, and
in agreement with those used by other authors 5 ,J9-20, but it does not respond to

315
any actual physical mechanism. This drawback is common to all the cohesive crack
models employed to study the fracture behaviour of monolithic ceramics 25 .

CONCLUSIONS
An experimental and analytical study of stable crack propagation in polycrys-
talline MgO was performed. Cracks propagate steadly from the notch root under
cyclic compression. The tensile residual stresses that develop around the notch upon
unloading in each cycle are the crack driving force are. These residual stresses
arise from the plastic deformations which take place when the specimen is loaded in
compression.
Stable crack growth has also been detected in monotonic tension and bending
from the compression fatigue crack tip. The increase in crack growth resistance with
crack length is attributed to the development of closure forces in the crack wake. This
behaviour seems to be related to the compression fatigue technique used to precrack
the specimens. During compression fatigue, uneven plastic deformation occurs along
the notch plane in suitably oriented grains, giving rise to tensile and compressive
residual stresses. When the specimen is loaded in tension, the crack propagates
through the grains with tensile residual stresses, whereas those in compression are left
unbroken in the crack wake. These grains bridge the crack, increasing the magnesia
fracture resistance. Analytical modeling of the fracture behaviour in tension and
bending by using a cohesive crack model is in agreement with the experimental
results.
Ackowledgements:The authors are grateful to Prof. S. Suresh for his help during the
course of this work.

REFERENCES
1. P. 1. Swanson, C. L. Fairbanks, B. R. Lawn, Y. W. Mai, and B. J. Hockey, J.
Am. Ceram. Soc., 70: 279 (1987).
2. G. Vekinis, M. F. Ashby, and P. W. R. Beaumont, Acta Metall. Mater., 38:
1151 (1990).
3. J. Rodel, J. F. Kelly, and B. R. Lawn, J. Am. Ceram. Soc.,73: 3313 (1990).
4. R. W. Steinbrech, R. Knehans, and W. Schaarwiichter, J. Mater. Sci., 18:
265 (1983).
5. R. W. Steinbrech, A. Reichl, and W. Schaarwiichter, J. Am. Ceram. Soc.,
73: 2009 (1990).
6. J. LLorca and R. W. Steinbrech, J. Mater. Sci., 26 (1991). In press.
7. R. W. Rice, S. W. Freiman, and P. F. Becher, J. Am. Ceram. Soc.,64: 345
(1981).
8. T. Ogawa and J. LLorca, in "Proceedings of the Anual Meeting of the Japan
Society of Mechanical Engineers", 910-17, Vol. A, JSME, Tokyo (1991).
9. J. B. Kessler, J. E. Ritter, and R. W. Rice, in "Surfaces and Interfaces of Glass
and and Interfaces of Glass and Ceramics", V. D. Frechette et al., eds., Plenum
Press, New York (1974).
10. F. J. P. Clarke, H. G. Tattersall, and G. Tappin, Proc. Hr. Ceram. Soc.,
6: 163 (1966).
11. A. G. Evans and R. W. Davidge, Phil. Mag.,20: 373 (1969).
12. A. G. Evans, Phil. Mag.,22: 841 (1971).
13. T. Ogawa, Fract. Mech. Ceram., 9-10 (1991).
14. 1. Ewart and S. Suresh, J. Mater. Sci.,22: 1173 (1987).

316
15. T. Ogawa and S. Suresh, Engng. Fract. Mech., 38 (1991). In press.
16. S. Suresh and J. Brockenbrough, Acta Metall., 36: 1455 (1988).
17. S. Suresh, L. X. Han, and J. J. Petrovic, J. Am. Ceram. Soc., 71: C-158
(1988).
18. R. W. Davidge, J. Mater. Sci.,2: 339 (1967).
19. Y. W. Mai and B. R. Lawn, J. Am. Ceram. Soc.,70: 289 (1987).
20. C. H. Hsueh and P. F. Becher, J. Am. Ceram. Soc., 71: C-234 (1988).
21. C. H. Tsai and C. C. Ma, Int. J. Fracture, 40: 43 (1989).
22. H. Tada, P. C. Paris, and G. R. Irwin, "The Stress Analysis of Cracks Hand-
book", Del Research Corporation, Hellertown (1985).
23. J. LLorca and M. Elices, in "Structural Ceramics - Procesing, Microstructure
and Properties", J. J. Bentzen et aI., eds., RiS0 National Laboratory, Roskilde
(1990).
24. J. LLorca and M. Elices, Int. J. Fracture, 43 (1992). In press.
25. J. LLorca and M. Elices, in "Cyclic Deformation, Fracture and NDE of Ad-
vanced Materials", ASTM Special Technical Publication, Philadelphia (1992).

317
INTERRELATION BETWEEN FLAW-RESISTANCE, J(R-CURVE BEHAVIOR,

AND THERMAL SHOCK STRENGTH DEGRADATION IN CERAMICS

Ekkehard H. Lutz and Michael V. Swain

University of Sydney
Department of Mcchanical Enginccring
New South Wales 2006
Australia

ABSTRACT

Flaw resistancc, J( R-curve bchavior, and thermal shock strength degradation of a range
of different ceramics are investigated. The results are analysed and compared with previous
theoretical considerations. An attcmpt is made to cstablish an intcrrelation among the above
three properties of ceramics.

INTRODUCTION

Many ceramics show a rising crack resistance or toughness during crack extension,
namely R- or J(R- curve behavior, which is a direct consequence of energy-dissipating tough-
ening mechanisms which rcduce the crack driving force at the crack ti pl-3.

Generally two different types of It-curves are distinguished. A flat R-curve, i.e. R
constant and independent on crack extension, is expected in perfectly brittle linear-elastic
materials, such as glass and most fine grain size single phase ceramics. Rising R-curves have
been observed in a wide range of ceramics 3- 12 such as large grain size ceramics with thermal
expansion anisotropy3-7 a.nd transformation toughened ceramics S - 12 .

In recent years a number of short- and long-range contact- and zone-shielding mecha-
nisms have been described l l , such as crack deflection and crack branching 12 - 14, transforma-
tion toughening and microcrack toughening8-13.15-17, residual stresses 7,9,12,13, and toughen-
ing by bridging and load-canying processes behind the crack ti p4,10,12,13,18, which produce a
more or less pronounced R-curve behavior. It is difficult to estimate the contribution of a sin-
gle mechanism to J(R from experimental data12 . On the one hand not all toughening effects
are visible, and on the other they seldom appear singly. Since toughening mechanisms are
in many cases activated by stresses caused by thermal expansion mismatch or phase trans-
formation which are temperature sensitive their magnitude and, hence, their contribution to
J(R is also expected to depend on temperature.

Cook and Clarke 19 suggested that the J(R-curve could be represented by a power
function, that is

(1)

with 0 ::; T ::; 0.5. ](0 is regarded as the base toughness of the material in the absence of
any toughening mechanisms and the term a o as the spatial extent of the crack at which

Fraclure Mechanics of Ceramics, Vol. 9

Edited by R.C. Bradt el aI., Plenum Press, New York, 1992 319
toughening begins. The slope of the power function, T, can be easily evaluated by linear
regression of a double-logarithmic plot of J(R versus a. The situation where T=O corresponds
to constant toughness, T >-0 indicates a pronouced J(R-curve behavior. Although Cook and
Clarke19 chose a simplistic expression to describe the J(R-curve shape, it is a useful approach
to characterize the steepness of such curves.

The thermal shock behavior of ceramics is conventionally measured by quenching small

beams from an elevated temperature into water at room temperature and measuring their re-
tained strength, O'R, or modulus of rupture, MOR. For 6.T >- 6.Te rapidly growing cracks are
thought to arrest either when all of the strain energy is converted into fracture surface energy
(Hasselman thermoelastic approach 20 ,21) or when the statically defined stress intensity fac-
tor, K, becomes less than the critical stress intensity factor, K e22. Following Hasselman 2o ,2t,
a damage resistance parameter, Rill', can be calculated for any ceramic material with:

I/II - E,eff
R - 2 (2)
O'B

,eff is the specific work of fracture and O'B the initial strength of the material. Since RI/II
should be proportional to the retained strength, O'R, when normalized to the initial strength
of a material, O'B, a correlation between the R-curve behavior and the thermal shock strength
degradation can be derived semi- empirically by modifying eqn.(2) t0 2I :
O'R ,..., RI/II ,..., ,WOF
(3)
O'B ,ie

where ,WOF is the specific work offracture required to extend a crack, approximately given
by the average R-curve value 24, and ,ie is the energy to initiate crack growth, equivalent
to the initial R-curve value. For a flat R-curve bWOF )/bic) has it's minimum value of
1.0. The steeper the R-curve, the larger the ratio becomes and the less is the anticipated
strength degradation. Although it has been shown that this relationship holds reasonably
well for alumina 23 , Mg-Partially Stabilized Zirconia ceramics 24 , and duplex- ceramics I2 ,25,
this approach is very simplistic, because the elastic strain energy which has been used to
derive eqn. (2) is difficult to estimate 26 - 28 .

Toughness and "flaw resistance" (may also be thought of as the "contact damage
resistance" or "mechanical damage resistance") of ceramics can be conveniently measured
using the "Indentation-strength in bending (ISB)-" method 29 . According to this technique,
the retained strength of a sample is measured after introducing a crack or "damaging" it's
surface by a Vicker's indentation of a certain load, PI. For very small loads, i.e. as long as
the damage is smaller than the inherent flaw size, the strength is not reduced. For higher
indentation loads, P} >- PI, however, the strength decreases from O'} to 0'1 with increasing
load 29. The strength decrease as a function of the Vickers indentation load of a material
describes it's "flaw resistance" .

The influence of a material's It-curve on the flaw resistance or resulting strength degra-
dation has been considered in detail by Cook et aI 19 ,30 and Chantikul et aPI for the specific
case of pointed indentation. These authors found that the extent of strength degradation was
strongly influenced by the microstructure which in turn determined the R-curve behavior.
They investigated a range of alumina ceramics varying from single crystals through fine to
coarser grained. Although the initial strength decreased with increasing grain size, the flaw
resistance increased continuously.

Cook and Ciarke I9 suggested that the decrease in strength as a function of the Vickers
indentation load can be described by the following expression:
2 p2
-O'r = [r
- J(£=1)
2T+3 (4)
O'} PI
with 0 ~ T ~ 0.5.

320
 The relationship between the [(R-curve behavior and the flaw resistance as described
by the above equation is schematically illustrated in Fig. 1 as a plot of logO"/ versus logP/.
From the slope of the resulting straight line 7 may be estimated. For 7=0 the absolute
~alue a! the slope is maximum wi th ~ indicating tha,t the materia.l is "flaw-sensiti~e": W.ith
mcreasmg 7 the absolute value of the slope decreases approaclung 0 at 7=0.5 mdlcatmg
"ideal flaw-tolerance". It should be pointed out here that the derivation of eqn. (4) is based
on linear-elastic fracture mechanics.

IgO'
1913's '"
A
19l1i .- - - B
IgUe .~-_'''~-.-.-.':._
19(),'

, "'lgG?

IgP

Figure 1. Schematic illustration of the correlation between mechanical damage or flaw re-
sistance and KR-curve behavior suggested by Cook and Clarke 19 (eqn. (4)). The
logarithm of the strength is plotted versus the logarithm of the Vickers indenta-
tion load for two different materials with 7 =
0 and 7 )- O.

Lateral crack growth 32 , the presence of strong residual stresses on the surface33 ,34 and about
pressurized inclusions in duplex ceramics 12 are considered to have a considerable influence
on crack pattern and crack propagation from the initial crack beneath the indentation, and
hence, on the shape of the flaw resistance curve.

As described above, two different correlations are already well known. There is the cor-
relation between the R-curve behavior and the thermal shock strength degradation on the
one hand. It can either be simply described by the empirically derived proportionality in
eqn. (3)20,21 or calculated using the more sophisticated stress-intensity concept 22 ,26.28. On
the other hand there is the theoretically predicted correlation between the ](R-curve be-
havior and the Jlaw-resistance described by eqn. (4)19 which is based on the assumption
that the materials behave linear-elastic and that any ](R·curve can simply be expressed in
the form of the power function in equ. (1)19. If it were possibly to establish a relationship
among all three properties, flaw resistance, J(R_ curve behavior and thermal shock strength
degradation, two of them could be easily predicted by the knowledge of one alone.

The aim of this work is to investigate and compare flaw resistance, ](R-curve behavior,
and thermal shock behavior of different ceramic materials. For the comparison of the results
with e.~l. (4) an atte.mpt will be made to u~e 7 as a quantitative measure for flaw-resistance
and Ii. -curve behaVIOr of the tested matenals.

321
EXPERIMENTAL PROCEDURE

The tests were carried out on the following materials:

(1) Four Al 20 3 ceramics with grain size of rv 1 JLm (CT 8000 SG, Alcoa), 25 J-lm and
34 J-lm (both Grade Taimei), and 48 J-lm. The 1 Jim material was fabricated as described
below in section (2). The 25 J-lm alumina was fired at 1700°C for 17 hours. By an additional
heat treatment at 1900°C for 3 hours in N 2 the grain size increased to 34 J-lm. A 16 Jim
alumina fabricated by Steinbrech et al 4 ,40 was also fired at 1900°C for 3 hours in N 2 • After
the heat treatment the material had an average grain size of 48 J-lm. Whereas the aluminas
with grain size of 1 and 48 J-lm exhibited a classical equiaxed microstructure, the Taimei
materials were somewhat acicula and showed a wide grain size distribution. In the 34 J-lm
material occasional grains up to 500 Jim size were found.

(2) 2Y-TZP (2-mole-% yttria tetragonal zirconia polycrystals), 3Y-TZP (3-mole-%

yttria tetragonal zirconia polycrystals) plus 20 wt.-% Al2 0 3 (Tosoh, Japan), and various
duplex-ceramics based on these materials and on Al 2 0 3 (1 Jim - see (1) above). Different
mixtures of A1 20 3 (CT 8000 SG, Alcoa) and 35, 50, 80 vol.-% of monoclinic (m- )Zr02
(Dynazirkon F, Dynamit Nobel), and pure m-Zl'02 were used as inclusion ("pressure zone")
component B. The materials were sintered at 1500°C for 2 h in air and, in some instances,
hot isostatically pressed (IIIP'ed) at 200 MPa and 1600°C for 10 min in N 2 . The fabrication
procedure of these composites is described in detail by Lutz et al. 35 .

For further discussions the matrix components (A), 2Y-TZP, 3Y-TZP + 20 wt.-%
A1203, and A1 20 3 are labeled 2YZ, 3YZ20A, and AO, respectively. The pressure zone
components (B), Al 20 3 + 35, 50, and 80 vol.-% m-Z7'02, and pure m-Zr02 are labeled az35,
az50, az80, and z100, respectively. For small (16-32 J-l diameter) and large (45-65 J-l diameter)
pressure zones the indexes "s" and "L", are used, respectively. The duplex-ceramic labeled
3YZ20A-20az50s e.g., consists of 20 vol.-% of small pressure zones composed of A1 20 3 + 50
vol.-% m-Zr02 dispersed within a matrix 3Y-TZP + 20 wt.-% A1 20 3.

(3) Precipitated partially stabilized zirconia containing 9 mole-% MgO (Le., Mg-PSZ).
Simultaneous sintering and heat treatment in the cubic phase field, followed by controlled
cooling and subeutectoid heat treatment for longer periods resulted in materials of maximum
strength (MS) and high thermal shock resistance (TS)9. The fabrication heat treatment and
resultant microstructures have been described in detail by Hannink 36 and Hannink and
Swain37 . In addition, an overaged Mg-PSZ material (TSN, 768 ST)) containing 3.0 % MgO
and 0.6 % Silica provided by Nilcra, Australia, has been tested. The TSN material had
a grain size of 25-50 J-llll with 74.2 % of the Zr02 grains transformed into the monoclinic
modification.

(4) Si 3 N 4 composites containing 10,20,30, and 40 wt.-% llN (Kawasaki Steel, Japan).
Fabrication conditions, microstructure, and mechanical properties of these materials are
described in detail by Isomura et a]38. The materials exhibit residual porosity increasing
from 18 to 38 % with increasing BN content 38 . The composites, Si 3 N 4 + 10,20,30, and 40
vol.-% BN, are labeled SNBI0, SNll20, SNB30, and SNB40, respectively.

The flaw resistance tests were carried out 011 small rectangular beams (for dimensions
see below) using the indentation-strength-in-bending (ISll) method 29 • The specimens had
the following dimensions: SNll-materials - 5.2-6.2 x 2.5-3.1 x 32 mm; ".11 20 3 (1 J-lm), 2YZ,
3YZ20A, and duplex-ceramics based on these materials - 2.9-:3.4 x 3.2-3.8 x 45 mm; Mg-PSZ
(MS and TS) - 3.4 x 4.4-4.8 x 42 mm; Mg-PSZ (TSN) - 2.25 x .5 x 20-30 mm. The smaller
side of the specimens was indented using various loads between 1 and 1000 N. Three to five
samples were tested per indentation load. The retained strength was measured in 4-point
bending (span 24/8 mm and span 18/6 mm) using a cross-head speed of 0.3 mm/min.

The J( R- curve experiments were performed using compact tension (CT-) tests. One
side of the testpieces was polished. The samples were precracked by starting the crack from
a chevron-like prenotch. When a sharp straight-through crack was achieved the specimens
were renotched to a point as near as possible behind the crack front. The notch depth/sample

322
width ratio, ao/w, was chosen to be 0.51-0.61 for the SNB-specimens and 0.58-0.65 for all
other materials. The samples were loaded using a cross-head speed of lOJ.Lm/min. The
crack propagation was measured directly using a traveling microscope. The J(R-values were
calculated on the basis of the load P, the relative crack length a/w, the sample thickness b,
and the appropriate Y-function 39 .

The CT-samples had the following dimensions: SNB-materials - 25-27 x 32 x 5.2-6.2

mm; Ah03 (1 J.Lm), 2YZ, 3YZ20A, and duplex-ceramics based on these materials - 21-25.5
x 26-27 x 2.9-3.4 mm, 25 and 34 J.Lm Al 2 0 3 - 37.0 x 38.5 x 3.7 mm; 48 J.Lm Al 2 0 3 - 34.8 x
18.2 x 2.3 mm; Mg-PSZ (TSN) - 28.4 x 29.6 x 2.25 nun.

In order to critically appraise Cook and Clarke's19 suggestion (eqn. (4)) it was at-
tempted to classify ISD- and J(R-results according to their logarithmic steepness. The ISB-
results were plotted as log( O'R) versus log( PI). Only those points where fracture passed
through the indentation were used for the quantitative evaluation of To Based on the as-
sumption that the decrease in strength in the 10g(O'R)/log(O'B) relationship is decribed by a
straight line it's slope has been evaluated by a linear regression with a computer. In order to
directly compare ISD and J(R results, the value of "TISB" was calculated from the obtained
n
slope value assumin that it equals (2T - 1)/(2T + 3) according to eqn. (4). For direct com-
parison with the J( -curves the logarithmic steepness "TJ(" of the measured J(R-curves was
evaluated in a similar procedure, namely by linear regression of the 10g(I(R)/log(a)-plots.
This can be easily done without the knowledge of ](0 and a o defined in eqn. (1).

The above evaluation technique was used for all results obtained in this work (with the
exception of the SND materials for the reasons outlined below) and also for results borrowed
from previously published papers.

Thermal shock tests were carried out by measuring the retained bending strength after
quenching samples from successively higher temperatures into 20°C water. Their strength
or modulus of rupture (MOR) was measured in 4-point bending (span 24/8 mm and 18/6
mm) at a cross-head speed of 0.:1 mm/min. The specimens had the following dimensions:
SNB-materials - same as for lSD-testing; ;t! 2 03 (1 jIm), 2YZ, 3YZ20A, and duplex-ceramics
based on these materials - 3.5 x 3.5 x 45 mm.

RESULTS

The results of the lSD-tests, ](R-curve measurements, and thermal shock tests are
shown in detail in the Figs. 2-7. The plots of the J( R-curves shown in Figs. 3b-7b were drawn
by simple connection through the experimentally derived data. The TJ( values determined
by linear regression are associated with these plots. The results also include numerous other
data published by different authors 9,31,37,38,4o-42 in the last few years.

Fig. 2 contains results obtained from alumina of different grain size The upper diagram
shows three of the indentation-induced flaw resistance curves measured by Chantikul et a1. 31
for alumina of 2.5,14.6, and 305.2 Illll grain size. The results were obtaiued from disks broken
under flat-on-three ball biaxial loading conditions. Although the 14.6 J.Lm samples indented
with 0.3, 0.5, and 1.0 N broke from the indent, and can hence not be interpreted as belonging
to the plateau, the indentations caused no or only a very small strength reduction. This may
have been due to the very limited area exposed to the maximum stress in the balloon-ring
biaxial test when compared to 4-point bending conditions. Neglecting the above three data
points in the regression analysis results in a T-value of 0.13 and including them increases T
to 0.19.

The flaw-resistance curves measured by Chantikul et a1 31 show a clear tendency.

Although the initial strength of alumina decreases with increasing grain size, their flaw-
resistance increases continuously.

The diagram in the middle illustrates the J(R- curve behavior of alumina of different

323
 a 700 --~:.Q,~.
0 500 Al 203
Q..
::E: _.!:~YL ....

'tf 300
T=032
------~-----~
6
1'.6pm
200
35.2)Jm 0 ::--

100
0.1 10 30 100
N
P,N
::> b
E Steinbrec.h
'6Jlm-r~O, 9
0
Q.
10
::E: 8 '.... T.O.OJ
a:
::.:: 6 !
2
0
a 6 8
a.mm

c 1.0
l>

0.8
~
........
l:3' 0.6

0.' 3'pm

0.2
l)Jm
0
a 200 '00 600
liT. ·C

Figure 2. Flaw resistance (a), J(R- curve behavior (b), and thermal shock
behavior (c) of alumina ceramics of different grain size.

324
Figure 3. Flaw resistance (a), J{R- curve behavior (b), and thermal shock
behavior (c) of :3YZ20A a.nd three duplex-ceramics, HIP'ed
3YZ20A - 20a.z50s. - lOzlOOs, and - 20z100s.

325
 a o 3YZ20A - 200z35 5
500
0 • 3YZ20A· 100z50l
0..
:::!: 300
=U&[L •
•
3YZ20A - 200z80 5
3YZ20A· 100z80 l
.j'
200 .1.:.:9.2_9..........

100

10 100 1000
~,N
~ b 15
E
0
0..
:::!: 10
cr
~

2
a,mm

C \,0

-
0.8
~
0.6
~
0.'

0.2

0 '00 600
liT, 'C

Figure 4. Flaw resistance (a), [(R·curve behavior (b), and thermal shock
behavior (c) of 3YZ20A and three duplex-ceramics, 3YZ20A -
lOaz50L, - 20az80s, and - lOaz80L.

326
 a
500
0
a.. 300
::E
~ 200

100

50
I 10 100 1000
P,N
s: b
E 20 T·0.68
0
a..
::E 15
a:
~ T·0.30
10

5 -'--T'O,O~

a
a 2 6
O,mm

c \.0 t:.-"~ )l;

0.8 ~:=r:----.
--
L----x.
CD '---...6
'0
.,g 0.6 .-.~
O.~

0.2

o 200 600
6T. ·c

Figure 5. Flaw resistance (a), ](R·curvc bchavior (b), and thermal shock
behavior (c) of AO and three duplex-ceramics, AO . lOaz35s,
. 20az35s, and· lOa.z50s.

327
 a _!;;.Q --
0 1000 ,
Q.. _!:£m ..
~ -j';-o.J"--_::·:;~-,
500
'oeD -r; 0.08- --- -----
300

-~~~~---------_.
100
10 100 1000
P, N
N
"- 12
-E b ,' "=0.1.9 • 2YZ HIP
,f ,. -- "=0.31 o 2YZ-lOoz35 L
HIP
::!:
8 I
"=0.17
n:: I

~ "=0.05
"=0.11

0
0 5
o,mm

C i.O

0.8
..g
........
'on:: 0.6

0.1.

0.2

0
0 200 1.00 500
CIT, 'c

Figure G. Flaw resistance (a), J(R- curve b~havior (b), and thermal shock
behavior (c) of three differently aged Mg-PSZ ceramics (MS,
TS and TSN), 2Y-TZP (2YZ) and 2YZ· lOaz35L.

328
 \-\
C 1.0

0.8
~
---- .
\

"oIL 0.5 \
~ ",\
- -.. '"
O.L
o SNB 10 " :. .....~t
'0
• SNB20
0.2 tlSNB30
• SNBl.Q
a
a LOa 800 1200
6T. ·c

Figure 7. Flaw resistance (a), J( l?-curve behavior (b), and ther-

mal shock behavior (c) of SNB-composites. The bro-
ken lines in (a) are the anticipated response for the
various SNB materials using the J(R-curve plateau
values as A'/c for the calculation of the ISB retained
strength 29 . The basis for the overestimation of J([c
by using the ISn technique in discussed in the text.

329
grain size. The results are compared to curves borrowed from Steinbrech et al. 40 and Swain 41 .
The J(R-curve of a 16 /lm material has been calculated from the R-curve measured by
Steinbrech40 in 3-point bending (single edge notched beam (SENB- )specimen dimensions
7.0* x 5.0 x 60 mm). Fig. 2b also shows the ](R-curve obtained from a double cantilever
beam (DCB) test (specimen dimension 3.3 x 14.2 x 80* mm) by Swain41 with the 16 /lm
alumina fabricated by Steinbrech4.4o . The superscript "*,, used above indicates in which
direction with respect to the specimen dimensions the crack was propagated. The J(R-curve
of the l/lm material is almost flat. Although the curves reported by Steinbrech et a1. 40 and
Swain 41 for exactly the same 16 /lm alumina are different as a result of the different sample
geometry and testing technique, they show a similar logarithmic steepness r with 0.19 and
0.17 (Fig. 8). The 25 /lm material exhibits a relatively steep curve with r = 0.24. The heat
treatment at 1900°C for both the 16 tLm Steinbrech and the 25 /lm Taimei material results
in an increasingly pronounced [(R-curve behavior.

The thermal shock behavior of 1, 10, and 34 /lm materials is demonstrated in the
lower diagram in the form of the normalized retained strength, (JR/(JB, vs. the quenching
temperature difference l:1T. The curves of the 10 and 34 /lm materials have been borrowed
from Gupta42 . A1 20 3 shows no substantial reduction of l:1Tc with increasing grain size, but
increased retained strength after severe thermal shocks.

The signiftcant change of the mechanical and thermal shock properties of a brittle high-
strength matrix which can be achieved by incorporating pressure zones is demonstrated in
the Figs. 3 - 5 for the matrices 3YZ20A and HIP'ed AO. The [(R-curves of AO - 20az35s
and - 10az50s are extremely steep and exhibit r-values exceeding 0.5! As has been previously
illustrated 12 .25 ,43,44 and as is here apparent from both figures the strength of the matrices
decreases markedly with increasing volume fraction and dilatation (i.e. m-Zr02 content)
of the zones, whereas the resistance to mechanically introduced surface flaws and severe
thermal shocks and the steepness of the [(R-curves increase. Another interesting feature
of the J(R- curve behavior of duplex-ceramics is that, although it's steepness increases, the
location of the curves is first shifted to higher [(R-values, passes through a maximum, and
decreases again. This effect can be observed e.g. in Fig. 3 by comparing the curve of 3YZ20A
- 10z100s exhibiting a r-value of only 0.28 with the curve of 3YZ20A - 20z100s which shows
a logarithmic slope as high as 0.48. The J(R-values of 3YZ20A - 20z100s are on average
lower but display a steeper (logarithmic) path than the curve of 3YZ20A - 10z100s.

Flaw-resistance, ](R-curve behavior, and thermal shock behavior of HIP'ed 2YZ and
the 2YZ-based duplex-ceramic, 2YZ - 10az3.5L, are depicted in Fig. 6 and compared with
the curves of the three Mg-PSZ ceramics. The incorporation of pressure zones in 2YZ
leads to a pronounced strength reduction, but also to a slightly increased flaw-resistance,
steeper J(R-curve, and higher thermal shock retained strength. The KR-curve and thermal
shock behavior of the MS- and TS- Mg-PSZ materials were published by Marshall and
Swain9 and Hannink and Swain37 in previous papers. The thermal shock properties of
TSN were measured by Nilcra, Australia. There is no significant difference in the flaw
resistance of the two differently aged ceramics although their J(R-curve and thermal shock
behavior are different. The TSN material exhibits a comparably flat J(R-curve despite a good
flaw-resistance and high thermal shock retained strength. However, this material displayed
exceptionally stable crack growth behavior, and unlike most materials with flat R-curves, a
very substantial residual crack opening displacement upon unloading.

Flaw-resistance, J(R-curve behavior, and thermal shock behavior of the SNB materials
are shown in Fig. TIs. The thermal shock results have been borrowed from a paper of Isomura
et al. 38 with the exception of the result for ClT = 1200 DC. The strength of the materials
decreases with increasing BN content because of the increasing residual porosity38,45. All
materials show a similar flaw resistance behavior. The strength reduction is quite low for
indentation loads up to 100 N, but is apparently more pronounced for higher loads with
a final slope of the curves closer to (-1/3). All SNB-composites exhibit flat [(R-curves
with their toughness analogous to their strength decreasing with increasing BN-content. No
visible toughening mechanisms were observed. A thermal shock of l:1T= 1200 °C into water
at room temperature results in a strength loss of 56 - 66 %. The retained strength of the
SNB-ceramics subjected to such severe thermal shock decline in proportion to their initial
strength as the BN content increases.

330
DISCUSSION

A comparison of the resulting flaw-resistance, J(R-curve and thermal shock behavior

shows that there are trends in the interrelation among all three properties. These trends are
not only found in alumina of different grain size, but also in complex duplex-structures and
to some extent in pronounced quasi-ductile Mg-PSZ ceramics and Si 3 N 4 - BN structures
exhibiting residual porosity. As has been mentioned in the introduction there are many
parameters which can influence the experimental results which are thought to limit attempts
to quantify this interrelation. Limitations seem to come from the restricted interpretability
of the flaw-resistance for predicting J(R-curve behavior, especially for the SNB and Mg-PSZ
materials, and the unknown influence of temperature and quasi-plasticity on the material's
behavior during thermal shock.

There are three quantities which will be used to quantitatively analyse the interrelata-
bility of the material properties shown in Figs. 2 - 7: The flaw-resistance will be characterized
by the T-value obtained from the logarithmic slope of the flaw-resistance curve, TISB. A mea-
sure for J(R-curve behavior is it's logarithmic steepness, T[{, and for thermal shock resistance
it is the normalized retained strength obtained after a severe thermal shock.

There is no justafiable physical basis for the characterization of flaw- resistance or

J(R curves by a measure T. However, the use of a power function to describe an observed
empirical relationship between dependent variables was widely used in mechanical property
characterization, e.g. slow crack growth, creep, and strength (Weibull modulus). In Fig.
8 the J(R-curves for the 16 ~tm alumina borrowed from Steinbrech et al. 40 as measured
using the SENB technique and Swain 41 who used DCB geometry (Fig. 3b) are illustrated
as 10g(I(R) - log(a) plot and compared with the straight lines obtained by linear regression.
Although the curves shown in Fig. 2b seem to be different, they obviously exhibit similarities
in shape and steepness in Fig. 8. Most measured J(R curves can be reasonably well fitted
by a straight line when plotted as 10g(I(R) versus log(a). An example of a very good fit is
shown in Fig. 9 for the J(R-curves of AO, AO - 10az35s and AO - 10az50s shown in Fig.
3b.

A relatively bad fit is shown in Fig. 10 for 3YZ20A - 20az80s and - 10az80L. The linear
regression of all data points give straight lines which are steeper than would be expected
from a simple graphical examination. The reason is that the computer equally accounts for
the first points of the J(R-curves which show a considerable deviation from the trend. Since
the tolerance for measuring the crack length during the R-curve experiment is bout 0.05 mm,
a small error in the first steps of crack propagation has a tremendeous effect on the location
of the data points in double-logarithmic graphs. Even if the first points are neglected, the
J( R-curve of 3YZ20A - 20az80s has a higher logarithmic steepness than the curve of 3YZ20A
- 10az80L, a situation which is not apparent from Fig. 4b.

Figs. 11 and 12 show the plots of TISB versus T[{. According to eqn. (4) TISB should
equal T[{ which is apparently not overall the ca.se. However, despite a considerable deviation
from the theoretical prediction for some materials, Figs. 11 and 12 confirm that the flaw-
resistance increases with increasingly pronounced R-curve behavior. Both, the TS and TSN
Mg-PSZ ceramics show a significa.nt deviation from the trend in Fig. 11.

The plot of the normalized retained strength, Un/UB, after a thermal shock of tlT
= 500°C vs. TISB and T[{ shown in Figs. 13 and 14 reveals the relationship between the
thermal shock retained strength and both, the flaw-resistance and J(R-curve behavior. The
general trend is the same in both figures. The retained strength increases first linearly with
increasing T and seems to approach a constant value of ca. 0.8 - 0.9 with T exceeding 0.3.
There is, however, slightly better agreement between TISB and T/\ for TZP based duplex
ceramics in Fig. 13 than for the alumina based materials in Fig. 14.

The flaw-resistance behavior of the SNB-composites could be interpretted as indi-

cating R-curve behavior. The J(R tests, however, reveal that all SNB-composites exhibit
flat J(R-curves. The flat J(R-curve behavior which is unaffected by increased BN-contents
also explains the severe thermal shock strength degradation which is similar in all SNB-
mixtures. Assuming that the measured plateau values represent J( Ie of these obviously

331
 brittle materials 45 , it is possible to reconstruct the flaw resistance curves anticipated from
the J(R-results using the expression to calculate the ISB toughness 29 • The resulting plots
which exhibit the logarithmic slope of (-1/3) (TISB = 0) are shown in Fig. 7 as broken
lines. It is apparent that the ISB-results greatly overestimate the measured J(R values. A
possible explanation for this significant difference may be the reduction in residual stresses
about the indentation impression due to the intrinsic porosity of these pressurelessly sintered
materials 45 .

The present study suO"gests that there are some limitations of the proposed approach
between flaw resistance, J(JI-curve behavior, and thermal shock retained strength, particu-
larly for transformation based quasi-ductile materials such as Mg-PSZ and the fine grained
porous Si 3 N4 -BN composites. In both instances, the concept breaks down because the
ISB-technique appears unsuitable for the determination of the R-curve behavior.

20
AI 2 0 3 -16}Jm

10
~ 8
7
E Ii
0
a.. Steinbrech
2:
a:
::<:
t.
3
f SENB
en
2- 2

1
0.01 0.1 10

log o. mm

Figure 8. Double-logarithmic plot of the J(R-curves of a 16JLm alumina borrowed from

Steinbrech et a1. 40 and Swain 41 .

CONCLUSIONS

Investigations of flaw resistance, J(R-curve and thermal shock behavior of different

ceramics show that there is a clear qualitative, but only semi-quantitative relationship among
all three properties. Flaws whether caused mechanically by Vickers indentation or severe
thermal stresses both lead to a similar strength degradation. In both cases the strength
degradation depends on the stejfness of the J(R- curve. It is found that the logarithmic
slopes of flaw resistance and J( - curves represent simple and useful measures for their
characterization and for the prediction of the strength degradation upon severe thermal
shocks. These measures, however, can not be used unreservedly. For quasi-ductile behaving
materials and porous ceramics care must be exercised to predict J(R-curve behavior and
thermal shock strength degradation by the ISB derived flaw resistance.

ACKNOWLEDGEMENT

One of the authors (H.E.L.) thank the Deutsche Forschungsgemeinschaft, Bonn, West-
Germany, for the financial support under contract number lu 416/1-1. N. Claussen and P.
Greil are thanked for their assistance to make this project possible.

332
 AO -10az50 s /
r:0.68 , 0
i<O?AO_
10 - 10az35s
8 -
7 -
01 6- T:O.OI. AO
S! "'_
I. -

2 -

0.1 1.0 10
log a. mm

Figure 9. Double-logarithmic plot of the J(R-curves of AO, AO -

10az35s, and AO - 20az35s.

20

10 0°
~ 8
E 7
0 6 o
a... o
::E
x
'"
~
3 3YZ 20A -10az80 l
01
S! 2

10

log a. mm

Figure 10. Double-Iogartihmic plot of the J(R-curves of 3YZ20A

20az80s and :3YZ20A - 10az80L.

333
 0.5 v
o 3YZ20A
o 2YZ /

O.L. fJMg-PSZ /

t,Al 2 0 3 0 , /

~ 0.3
'0
/ fJ

, t;.
/

0.2
0 t,9
, '0
0.1 fJ
'0

0
0 0.1 0.2 0.3 O.L. 0.5
'115B

Figrue 11. Plot of the logarithmic slope of the J{R-curves,

TJ(, vs. TISB, obtained from the logarithmic
slope of the flaw-resistance curves, for alumina
of different grain size, 2YZ, 3YZ20A, and var-
ious duplex-ceramics based all these matrices.

0,7
•
~
0.6 I
J
0.5 I
~ I
0.4 /
I
I
0.3
I
•
I
0.2 I
/
/
/
0.1
/

0
0 0.1 0.2 0.3 0.4 0.5
1"iSB
Figure 12. Plot of TJ( vs. TISB for AO
and various duplex-ceramics
based on this matrix.

334
 1.0 , . . . - - - - - - - - . . . . ,
m ISB _.
~ 0,8 I, - -.
:Uo 0,5 / /0. K
I

.
.
Lf) I
\;:jII 0.• I

'b'" 0,2 -/
• o·2YZ
/ e-3YZ20A
o .~
o 0.1 0.2 0.3 0.. 0.5
1I<·1'lse

Figure 13. Plot of the normalized retained strength, aRlaB, af-

ter a thermal shock of t.T = 500 0 vs. TISB and TJ( e
for 2YZ, 3YZ20A, and various duplex-ceramics with
these matrices.

m 1.0
b
~ 0.8 0 .... •
.u ~
0 I
0
Lf) 0.6 ISS I
II
I-
I
K
<] A.. 0
,I
'tf 0,2
/

0
0 0.1 0,2 0,3 0.• 0,5 0.6 0,7

~.TIS8

Figure 14. Plot of the normalized retained strength, aRlaB, after a

thermal shock of t.T = .500 a vs. TISB and TJ( for AO and e
various duplex-ceramics with this matrix.

335
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337
MICROCRACK TOUGHENING MECHANISM IN BRITTLE MATRIX COMPOSITES

N. Miyata, S. Akada*, H. Ornura** and H. Jinno***

Department of Industrial Chemistry, Faculty of Engineering

Kyoto University
Sakyo-ku, Kyoto 606, Japan

ABSTRACT

The present study was undertaken to gain further understanding of the

microcrack toughening of ceramic materials. Model two-phase, glass-glass
particulate composites were chosen for study. In these composites, both
elasticity and toughness mismatches between phases are negligibly small and
only thermal expansion mismatch is important. Spheroidized silica glass
particles sized to 6 and 26 ~m in average diameter, were dispersed by hot-
pressing technique in two different soda lime silica glasses having thermal
expansion coefficients greater than the expansion of silica particles. These
two composite systems were designed by selecting a combination of differen-
tial thermal expansion and particle size, whereby microcrack toughening is
expected to occur most effectively. Fracture toughness and flexural strength
were determined for the composites containing up to 45 vol% of silica parti-
cles. An attempt was also made to use indentation-strength procedure to
evaluate an R curve in a selected composite composition. In both composite
systems, fracture toughness was found to increase linearly with increasing
volume fraction of dispersed particles before decreasing rather sharply. A
rising R curve was obtained for the composite in which microcrack toughening
is presumed to contribute most favorably. Experimentally observed toughness
behavior is consistent with a micromechanics model of microcracking which
predicts that the increase in toughness is primarily due to a crack-tip
shielding induced by fully developed wake of microcracked material.

INTRODUCTION

Microcracking is one of the most commonly accepted toughening mechanisms

in brittle matrix composites. This mechanism which is primarily due to
thermal expansion mismatch between constituent phases is believed to be oper-
ative if a condition defined by both differential thermal expansion and par-
ticle size is satisfied. I - 3 There has been a substantial advancement of our
understanding of the microcrack toughening mechanism in the last decade, but
it is still difficult to generalize on the optimal condition for microcrack

* Now with Asahi Glass Co., Ltd.

** Now with Matsushita Electric Industrial Co., Ltd.
*** Now with Department of Chemistry, Faculty of Science and Technology
Sophia University, Tokyo, Japan
Fraclure Mechanics afCeramics, Vol. 9
Edited by R.C. Bradt el al., Plenum Press, New York, 1992 339
toughening in brittle solids and to predict the possible toughening level for
a given material. This difficulty arises principally from the fact that, in
real materials, a variety of energy dissipative mechanisms including micro-
cracking contributes simultaneously to the overall fracture toughness. It
has long been considered that microcrack toughening of brittle materials can
be exerted by a crack-tip shielding due to the reduction in the elastic
moduli in microcrack process zone. Recently, a micromechanics model origi-
nally developed for transformation toughening 4 was extended to describe
microcrack toughening mechanism. 5 ,6 This model predicts that the crack-tip
shielding may be induced by both the elastic modulus reduction in the frontal
process zone and the dilatation caused by microcrack opening in the process
zone wake. The analysis based on this model also predicts that the increase
in toughness by microcracking is primarily due to the crack-tip shielding
induced by fully developed process zone wake. Such an influence of the wake
should necessarily give rise to R-curve behavior similarly in transformation
toughening mechanism. Although the proposed model explains successfully the
observed phenomena, real pictures of microcrack toughening remain to be
further verified by systematic experiments.

The purpose of the present study is to examine experimentally microcrack

toughening behavior in ceramic matrix, particulate composites and to gain
further understanding of this mechanism. Model two-phase, glass matrix-
glass particle composite systems where elastic and toughness mismatches are
negligibly small were designed in order that we can observe the microcrack
toughening behavior in the absence of appreciable effects of concurrent mech-
anisms.

EXPERIMENTAL PROCEDURE

Material Preparation

Glass matrix-silica glass particle, two-phase composites were designed

as model materials where microcrack toughening may exclusively occur during
their fracture process. As the matrix glasses, two different soda lime
silica glasses were formulated to have thermal expansion coefficients greater
than the expansion of silica. Table I lists the matrix glass compositions.
These glasses will be referred to as Gl and G4, respectively. The glass
batches of reagent grade powders were melted at 1450 to l500 0 C in platinum
crucibles to produce homogeneous, bubble-free glasses. The melts were air-
quenched and then ground in a vibratory mill.

Table I Materials used for study

Linear
Coeff. of
Thermal Young's
Composition Expansion Modulus
Notation (wt %) a /10-6 K-l E / GPa

MATRIX GLASS Gl 80Si02 l5Na20 5CaO 8.8 61.9

G4 65Si02 30Na20 5CaO 14.5 64.2

DISPERSED S( 6 ]lm) Fused Silica

0.5 72.2
PARTICLES S (26 ]lm) (flame-sprayed)

340
 Table II Composite systems studied

Difference in Therm.Exp.Coeff.
Composite System (am - a p ) /10-6 K- l

G4 - S ( 6 11m) 14

Gl - S (26 11m) 8.3

As the dispersed phase, spheroidized silica glass particles* were used.

In composite systems where low-expansion particles are dispersed in a high-
expansion matrix, the particle is subjected to a uniform compressive stress
and the matrix to radial compressive and tangential tensile stresses.? This
tangential tensile stress is expected to induce, under certain conditions,
matrix microcracking during fabrication or during subsequent stressing. It
has been recognized that the occurrence of microcracking in particulate com-
posites depends strongly upon both thermal expansion mismatch between con-
stituent phases and dispersed particle size. 2 It has also been suggested
that microcrack toughening in such materials can occur most favorably as the
dispersed particle size approaches the critical size for spontaneous micro-
cracking due to thermal expansion mismatch. S An expression for this criti-
cal particle size Dc below which microcracks are not formed spontaneously was
derived by Lange 9 for the case of spherical particle dispersion;

Dc k / S2 (1)

with
(am - ap) tiT
S (2)
1 + vm 1 - 2V p
+
2Em Ep

where S is the residual internal pressure induced at the matrix-particle

interface due to thermal expansion mismatch, k is a constant for a given
matrix-particle pair, a is the linear thermal expansion coefficient, 6T is
the temperature cooling range over which the matrix plasticity is negligible,
E is the Young's modulus, v is the Poisson's ratio: the subscripts m and p
refer to the matrix and particle, respectively. As preliminary experiments,
silica particles with different sizes were dispersed in both Gl and G4 ma-
trices. Such systematic experiments enabled us to estimate Dc for spontane-
ous microcracking in each of the matrices. Two combinations of differential
thermal expansion and particle size, by which microcrack toughening is ex-
pected to occur at optimum levels were thus selected for the present investi-
gation: silica particles sized to 6 and 26 11m in average diameter were dis-
persed respectively in G4 and Gl glass matrices. Hereinafter, these two
silica powders will be referred to as S(6I1m) and S(26I1m), respectively, and
two series of composites thus designed will be referred to as G4-S(6I1m) and
Gl-S(26I1m), respectively. The S(26I1m) powder was obtained by screening the
silica particles into a narrow range of size, 26 ± 6 11m. The S (6I1m) powder
was prepared by passing finer silica particles through 20l1m-sieve to separate
them from coarser ones. The prepared S(6I1m) powder, therefore, exhibited a
wide spread of particle sizes less than 20 11m, as shown in Fig.l: it con-
tained large amounts of particles smaller than the average size.

* Spheroidized silica powders were kindly supplied by Sumitomo Chemical Co.,

Ltd, Osaka, Japan

341
 30

~ 20
<I)

S
;:l

~ 10

0
0 4 8 12 16 20
Particle Size / p,m
Fig.l Particle size distribution for S(6~m) powder.

For both G4-S(6~m) and Gl-S(26~m) composite systems, disk specimens 30

mm in diameter and 5 or 10 mm in thickness containing up to 45 vol% silica
particles were fabricated by hot-pressing. The technique used for specimen
fabrication is described elsewhere. 10

Microstructure Characterization

Polished surfaces of as-fabricated specimens were observed using opti-

cal and scanning acoustic microscopy. Densities of the prepared composites
were determined by the Archimedes immersion technique in kerosene relative
to a fused silica standard.

Mechanical Property Measurements

Bending strength. Hot-pressed disks were cut into rectangular bars

2.5 by 6 by 28 mm with a precision diamond saw. Bending strength was
measured with a testing machine using three-point bending over a 20 mm span.
The diamond-sawed surface was stressed to failure. Measurements were car-
ried out at room temperature at a loading rate of 0.05 mmmin- l . To minimize
the effect of moisture-assisted slow crack growth, a dry nitrogen gas was
continuously blown at a constant rate on the stressed surface of the specimen
during testing. Six to eight specimens were fractured for each composite
composition.

Fracture toughness. Fracture toughness(Kc) was determined using the

three-point bending test of a single-edge-notched-beam(SENB). Specimens were
prepared in the form of rectangular bars 2.5 by 5 by 25 mm by cutting from
the hot-pressed disks. Pre-cracking was accomplished by thermal shock and
bridge-indentation techniques. Pre-crack lengths were measured by optical
microscopy prior to testing and these were also confirmed by post-fracture
observation of the fracture surface. Pre-crack length/specimen height ratio
was kept within 0.3 to 0.4. Specimens were tested in three-point bending
over a 20 rom span at a cross-head speed of 0.5 mm min- 1 All measurements
were made at room temperature under a dry nitrogen environment. Six to eight
specimens were fractured for each of the composites. Kc values were deter-
mined from sfecimen dimensions and fracture load using the equation of Brown
and Srawley. 1

342
 Indentation strength. Indentation strength-in-bending(ISB) procedure 12
was used to evaluate crack-size dependent toughness behavior(R-curve behav-
ior) of a microcracking composite. Gl-S(26~m) composite containing 30 vol%
silica particles was selected for this purpose. Flexural specimens were
prepared in the form of rectangular bars 3 by 5 by 28 mm by cutting from the
hot-pressed disks. A Vickers indentation was made at the center of the
prospective tensile surface of each specimen in such a way that the pyramidal
edges are aligned with respect to the longitudinal axis for the specimen.
The indentation loads were varied from 2 kgf(19.6N) to 13.3 kgf(130N). To
minimize the effect of moisture-assisted slow crack growth, a drop of liquid
paraffin was placed on the pre-selected site prior to indentation experi-
ments. Bending strength of the indented specimens were measured by three-
point loading over a 20 mm span. For each specimen, fracture experiment was
performed 30 minutes after indentation. During fracture testing, a dry ni-
trogen gas was continuously blown on the tensile surface of the specimen.
Six to eight specimens were tested for each indentation load.

2.8
'"I G4-S(6)
Ei
Jf 2.6

.-
~

'"0...... • • • • •
';:: 2.4
.-::
"'CI
Q)

CI 2.2
0 10 20 30 40 50

2.8
'"I GI-S(26)
Ei
Jf 2.6
'"~ )-o-o-o-o-O--O---O~"'-~---I
-.... u 0
>. 2.4
.-::
"'~
CI 2.2 l.-~~~_~~~_~~~--'

o 10 20 30 40 50
Volume % Silica
Fig.2 Densities of prepared composite specimens as a function of
volume fraction of dispersed silica particles.

RESULTS

Microstructure Characteristics of Hot-Pressed Composites

Figure 2 shows the variation of measured density with volume fraction of

silica particles for G4-S(6~m) and Gl-S(26~m) composite systems. Solid lines
in the figure are theoretical density curves predicted from the densities of
the matrix and the silica particles. In Gl-S(26~m) composite system, the

343
measured densities of the specimens containing less than 35 vol% silica, were
in fair agreement with the theoretical predictions. Further additions of
silica particles in this composite system caused gradual increase in porosi-
ty, and the porosity finally reached about 2 percents for the specimens con-
taining 45 vol% silica. In G4-S(6~m) composite system containing finer
silica particles, some deviations appeared from lower volume fractions of the
particles; fair agreements between measured and theoretical densities were
found for composite specimens up to 15 vol%, but the porosity gradually in-
creased with increasing volume fraction, and reached about 2.5 percents for
the specimens containing 45 vol%.

The examination of polished surface of the hot-pressed specimens by

optical microscopy revealed that, for Gl-S(26~m) composite specimens, silica
particles are distributed uniformly in the matrix at even higher concentra-
tions. However, for G4-S(6~m) composites which contain large amounts of
finer silica particles, the particle distribution in the matrix was not nec-
essarily uniform: it was macroscopically uniform, but local agglomeration or
clustering of dispersed particles gave some ununiformity.

As noted earlier, residual tangential tensile stress can induce radial

microcracks in the matrix in the present composite systems where am > ap ,
if the dispersed particle size is equal to, or larger than Dc expressed in
Eq. (1). In the system G4-S(26~m), the average size of dispersed silica par-
ticles must be close to the critical particle size for spontaneous micro-
cracking. Some difficulties arose in confirming such microcrack formation
under optical reflection microscope. However, the use of scanning acoustic
microscopy made it easier to detect some radial microcracks around particles.
Figure 3 shows an acoustic micrograph of polished surface of as-fabricated
G4-S(26~m) composite containing 25 vol% silica particles. Observed inter-
ference fringes clearly suggest that radially-induced microcracks join up be-
tween silica particles (brighter sites in the photomicrograph). But it should
be noted that this as-fabricated specimen was subjected to lapping and pol-
ishing procedures prior to microscopic observation. It is then quite possi-
ble that external stresses set up during these procedures may enhance some
growth of microcracks originally induced by residual thermal stresses.
It is unlikely that the specimens immediately after hot-pressing contain

Fig.3 Acoustic photomicrograph of polished surface of hot-pressed

Gl-S(26~m) composite containing 25 vol% silica particles.

344
 Table III Compilation of toughness and strength data

Fracture Flexural
Toughness Strength
Kc / MPa·m l / 2 Of / MPa
Volume
Percent
Composite System Silica, <jJ Mean Std Dev Mean Std Dev

G4 - S(6j.Jm) 0 0.771 0.078 94.4 8.5

5 0.796 0.053 77 .8 7.7

10 0.823 0.051 67.9 9.0

15 0.851 0.069 58.5 4.8

20 0.918 0.075 55.3 8.6

25 0.969 0.044 55.5 7.1

30 1.06 0.05 49.8 3.9

35 1.12 0.07 52.5 4.3

40 1.22 0.07 55.4 8.2

45 1.11 0.11 52.2 3.0

Gl - S(26j.Jm) 0 0.771 0.053 102.9 8.0

5 0.826 0.040 88.7 2.8

10 0.946 0.105 83.3 5.8

15 1.02 0.07 66.5 6.9

20 1.07 0.09 63.7 3.6

25 1.08 0.07 67.5 5.6

30 1.19 0.09 64.1 5.3

35 1.08 0.07 56.9 3.5

40 1.10 0.12 57.5 4.5

45 1.00 0.07 49.5 3.2

345
 Table IV Indentation-strength data for Gl glass and GI-S(26~m)
composite containing 30 vol% silica particles

Flexural
Strength
of / MPa
Indentation Load
P /kgf Mean Std Dev

Gl glass 2.0 50.5 7.1

3.3 42.1 5.2

5.0 35.2 3.3

8.3 30.6 4.6

10.0 29.7 2.6

12.0 27.9 4.3

Gl - S(26~m) 2.0 56.6 4.6

:30 vol% silica
3.3 49.5 4.1

5.0 45.7 4.2

7.0 41.2 3.7

8.3 38.3 4.8

9.3 39.7 3.1

10.0 38.0 3.3

12.0 38.4 3.0

13.3 36.8 3.0

such large microcracks. It seems that the average size of microcracks

induced during fabrication are much smaller than that estimated from micro-
scopic examination made on the polished surfaces. Microcracking situations
characterized by scanning acoustic microscopy were almost the same for G4-
S(6~m) composite specimens.

Mechanical Data

In table III, the results of strength and toughness measurements are

summarized. It is seen that, for both composite systems, fracture toughness
increases with increasing volume fraction of dispersed silica particles
before decreasing at higher volume fractions. The flexural strength is found
to drop sharply at lower volume fractions and to fall below the strength of
the host glass. The indentation-strength data obtained for Gl-S(26~m) com-
posite containing 30 vol% silica particles are compiled in Table IV. These
data will be presented graphically in the subsequent discussion.

346
INTERPRETATION

Toughness and Strength Characteristics

Fracture toughness. In the upper diagram of Fig.4, the variations of

fracture toughness with volume percent of silica particles for G4-S(6~m) and
Gl-S(26~m) composites are shown. The Kc values are normalized by matrix
toughness Kern. It is seen that, in both composite systems, fracture tough-
ness increases almost linearly with increasing volume percent of dispersed
silica particles before dropping rather sharply. The relative toughness
curves for both systems resemble each other in shape.

1.6
0 •
"~ • 0 •
1.4
0
0 0
• 0

••
........ 0
0
~ 1.2

•
••
0
1.0

1.0 ) • G4 - S ( 6 \lm)
o Gl-S(26 \lm)

".... 0.8 Q 0

--.... •
b

0
b 0.6 ~ ~
•• 0
~ ~
•
0
0.4
0 10 20 30 40 50

Volume % Silica
Fig.4 Variation of fracture toughness and flexural strength
with volume percent of dispersed silica for G4-S(6~m)
and GI-S(26\1m) composites.

In the present glass-glass composites, differences in elastic modulus

and toughness between constituent phases are negligibly small and only ther-
mal expansion mismatch is important. The similarity in toughness between the
matrix and the particle enables us to consider that the crack pinning by
particles is not involved in operative energy dissipative mechanisms. It
can be then considered that the energy dissipation during fracture process
of the composites is due primarily to thermal expansion mismatch. The most
important energy dissipative mechanism due to this mismatch is microcrack-
ing. 2 The average particle sizes in the two composite systems must just
or approximately satisfy the most favorable condition for microcrack tough-
ening(Eq. (1», so the observed increase in toughness can be primarily attrib-
uted to microcracking. Thermal expansion mismatch between particle and
matrix may also cause a propagating crack to deflect around particles. 13 ,14
Such crack deflection is well-known as one of the direct crack tip-particle
interaction mechanisms which may contribute to toughness increase. However,
in the case of a dispersion of spherical particles, its contribution is not

347
appreciable. 13 Thus, it can be considered that the toughness increment
observed in the present composites consists of a primary contribution due
to microcrack toughening and of a small additional contribution due to crack-
deflection toughening.

It is found that there is a delay in rising of the toughness curve for

G4-S(6~m) composite system. This may be caused by a wide spread of parti-
cle size distribution in this system. As pointed out earlier, 6~m-average
silica powders contain large amounts of smaller particles not generating
microcracking. In fact, the toughness curves for both G4-S and Gl-S compos-
ites exhibit similar trends in shape, and maximum toughening levels are ap-
proximately the same(about 1.5 to 1.6 fold increases in Kc relative to the
matrix toughness).

Crack-tip shielding due to the reduction in the effective elastic moduli

resulting from microcracking is counteracted by the decrease in the crack-
growth resistance of the microcracked process zone. 5 A sharp maximum ob-
served in the toughness curves of both composite systems may be explained by
the assumption that the microcrack density reaches a critical level within
the process zone. 1 ,5,15 High density of microcracks will make it easier to
propagate the primary crack by crack coalescence mechanisms.

Evans and Faber 5 proposed a micromechanics model for microcrack toughen-

ing. This model is based upon the concept that microcracks invariably form
in regions of residual tensile stress and release of this stress by the
microcrack results in residual opening and associated dilatation. Their
analyses have revealed that the fracture toughness due to microcrack toughen-
ing can be approximated by

( 1 + a f ) Kc * + bEf8h 1/2 (3)

where Kc is the measured toughness, Kc* is the intrinsic crack-growth resist-

ance of uncracked material(base toughness), f is the volume fraction of
microcracks at saturation, h is the microcrack zone width, 8 is the volumet-
ric dilatation induced by microcracking, E is the Young's modulus of un-
cracked material and a and b are constants estimated at 0.4 and 0.25, respec-
tively. The first term is the toughening due to the differential elastic
moduli between the microcrack process zone and the uncracked matrix, and the
second term is the toughening due to the dilatation that accompanies micro-
cracking. Eq, (3) can also expressed using the intrinsic crack-growth
resistance Kce~p in the process zone ahead of the crack tip as follows;

1 + af
KC + (4)
1 - f

with Kctip = Kc*(l - f). 5 The resistance Kctip corresponds to the reduced
local crack-growth resistance of the microcracked(damaged) material ahead of
the crack tip. On the basis of the proposed model, Evans and Faber 5 con-
cluded that the dilatation caused by microcrack opening in the process zone
wake is the prime source of toughening.

Later, Hutchinson 6 discussed the effect of profuse microcracking at the

tip of a microcrack and computed the shielding effect of microcracks to the
lowest order in microcrack density, considering a number of possible models.
According to his results, the fracture toughness due to microcrack tough-
ening is given in a general form by

1
Kc + (5)
1 - Of

348
where 0 and ~ are constants which depend upon microcrack distribution,
microcrack-nucleation criterion taken into account, etc. If the orienta-
tion of the microcracks is assumed to be randomly distributed within the wake
and if a critical mean stress is selected as a microcrack-initiation crite-
rion, the constants 0 and ~ are evaluated at 1.278 and 0.214, respectively.6
Eqs. (4) and (5) differ somewhat in expressed form, but they are approximately
identical for smaller microcrack densities.

If we assume that an annular microcrack rings each of the dispersed

particles, f can be linearly related to the volume fraction of particles,6
and hence Eq. (4) or (5) can be expressed in terms of the volume fraction of
dispersed particles ¢. Lineraly increasing toughness behavior observed in
Fig.4 seems to be consistent, at least phenomenologically, with these analyt-
ical results.

Flexural strength. In the lower diagram of F~g.4, the variations of

flexural strength with volume percent of silica phase are shown. The
strength values are normalized by matrix strength ofm. Flexural strength
is found to decrease rapidly at lower volume percents of silica phase, and
down to about 55 to 60 % of the strength of the host glass. This indicates
that the critical flaw size in all composites increases by the addition of
silica particles when compared to the host glass. Recall that the two con-
stituent phases of the present composites have approximately the same tough-
ness. This means that the particles act as "penetrable" obstacles from
the viewpoint of differential toughness, although residual compressive stress
within the particles may provide some resistance to crack penetration.
The addition of such particles which can hardly inhibit an increase in crit-
ical flaw size unavoidably leads to the reduction in strength.

Indentation-Strength Behavior

Indentation-strength method is based on the work of Chantikul et al. 12

According to their analysis, bending strength of a specimen pre-cracked by
Vickers indentation can be related to the fracture toughness Kc of a mate-
rial as follows;

(6)

where XR is a dimensionless constant for Vickers-produced median/radial

cracks, depending on indentation geometry and material properties, Y is a
geometry factor for an indentation-induced crack and Of is the bending
strength of a bar indented with load P. Writing

n [ (256/27) y3 XR ] 1/4 (7)

for convenience, we can express Eq. (6) as

Kc = (r
n"f
pI h ) 314 (8)

Thus, a plot of Of vs. P on a logarithmic scale makes it possible to examine

a crack-size dependence of Kc .

In Fig.5, the logarithmic plots of bending strength against indentation

load for Gl glass and GI-S(26~m) composite containing 30 vol% silica are
shown. For homogeneous Gl glass, experimental data follow a straight line
with slope of - 1/3 as expected. The data for GI-S(26~m) :30 vol% composite
deviate from the constant Kc model, suggesting that Kc increases with in-
creasing crack size. That is, the composite is found to exhibit a rising
R-curve behavior.

349
 P Ikgf
2 3 4 5 10 15

1.8
60
0

~O
50
0
III

,
III
:t 1.6 40
~
III
Slope = •_ 0 000
,
III
00

.,.
.... :t
b .~ ......
b
01
0
........... 30
.-l

0 G 1 - S (26 lJrn) 30 voH ~

1.4
• G 1 Matrix Glass
L--_ _-'---_ _--l..._ _- " ' - -_ _..l--_ _--LJ 20
1.2 1.6 2.0
log [PI N)
Fig.5 Bending strength Of as a function of indentation load P
for Gl glass and Gl-S(26lJm) composite containing 30 vol%
silica particles.

Evaluation of R Curve from Indentation-Strength Data

Here, an attempt will be made to evaluate an R curve of the composite

for which indentation-strength data are listed in Table IV and illustrated
in Fig.5. For this purpose, the indentation-strength procedure must be
extended to the case involving crack-tip shielding induced by a process zone
wake.

Crack-tip stress intensity. When a process zone wake shields the

crack-tip from the applied stress, the stress intensity factor just ahead of
the tip, Ktip may be characterized by

Ktip Kap - l'IK (9)

where Kap is the applied or remote stress intensity factor determined by the
applied stress and crack size, and l'IK( >0) is the stress intensity change
due to crack-tip shielding. It is the near-tip field stress intensity that
provides tha crack extension criterion;

(10)

where KO is the fracture resistance of the material immediately ahead of

the crack tip. The observed toughness is, therefore,

KO + l'IKc (11)

where l'IKc is the l'IK at the fracture criticality.

350
 Indentation-strength procedure. Suppose the case where an indentation
crack with a microcracked process zone wake which induces a shielding effect
at the crack tip is subsequently subjected to a bending stress. As a first
approximation, it is assumed that the dilatation induced by microcracking
produces in turn a uniform crack-surface closing stress(traction stress)
acting over a whole length of the crack (Fig.6) . The near-tip stress-
intensity factor Ktip can be expressed as

+ (12)

where a is the size of indentation crack, P is the indentation load, is °

the applied stress, Os is the crack-surface closing stress produced by the
dilatation, and Y and y' are the crack-geometry factors which embrace various
effects such as free surface effects and crack-interaction terms other than
purely geometrical factor. The first two terms of the right-hand side of
Eq. (12) correspond to Kap and the last term to 6K in Eq. (9) .

By inserting the equilibrium crack-growth condition Ktip KO into Eq.

(12) and requiring the equilibrium to be critical (do/da = 0), the critical
stress of and critical crack size af are defined as follows;

Of (13)

(14)

The combination of Eqs. (13) and (14) leads to an expression for observed
fracture toughness Kc .

1- 1/ 4
I
)
(15)

with
3/4
- 0 )p l13
y' )
y s (16)

1/4
n = 256 y3 I
[ 27 XR J

(1.! ! ! Ktip

iii

Fig.6 Applied stress intensity factor Kap ' near-tip stress-

intensity factor Ktip and crack-surface traction stress os.

351
 Evaluation of R curve. The preceding analyses indicate that, if the
values of KO' n and as are reasonably determined, af and Kc can be calcu-
lated from indentation-strength data using Eqs.(14) and (15), respectively.

An expression for the fracture strength of of a pre-cracked specimen

may be derived from a simple transformation of Eq. (16) .

+ (17)

Eq. (17) suggests that a plot of of against p- 1 / 3 should give a straight line
with a slope of (Ko/n)4/3 and an intercept of (Y~/Y)os. Figure 7 shows a
of vs. p- 173 plot for Gl-S(26~m) :30 vol% composite. In accordance with
Eq. (17), the plot is found to be linear. From the slope, we obtain

(Ko/n)4/3 (18)

Furthermore, the extrapolation of the linear plot to the intercept gives the
value for (Y~/Y)os'

(Y~/Y)Os 14.4 MPa (19)

According to Marshall and Lawn, 16 the crack-geometry factor, Y is estimated

at 0.9708 for a Vickers-produced median/radial crack. Another crack-
geometry factor Y~ which is associated with the crack and residual loading
geometry may be somewhat different from Y, but its difference is assumed to
be small. Hence, by taking y'/y z 1, as is estimated at about 14.4 MPa.

In order to calculate the critical crack size af, the value of XR or

related n must be known. The value of n can be experimentally evaluated
from Eq. (18), if we take an appropriate value for KO' In the present analy-
sis, KO must include the shielding contribution due to modulus reduction.
That is, from Eq. (5),

70

60

50
~
p..
40
::E
---....
b
30

20
l1. = 14.4 MPa
10

0
0.0 0.1 0.2 0.3 0.4
p-t / wt
Fig.7 of vs. p-l/3 plot for Gl-S(26~m) :30 vol% composite.

352
 1
K tip (20)
1 - Of c

Kc tip can. be approximately related to the base toughness Kc * by the expres-

sion KctlP = Kc*(l - f). Then,

1 - f
KO Kc * (21)
1 - Of

For small densities of microcracks, one finds KO ~ Kc *. Kc * must be consid-

ered as the base toughness of the composite which does not undergo stress-
induced microcracking. Even in the present composite, Kc * does not coincide
with the fracture toughness of the matrix. It must include minimal contri-
butions due to direct crack-particle interaction. To evaluate Kc * experi-
mentally, fracture toughness measurements were carried out on different Gl
matrix composites where much smaller silica particles (3 ~m-average diameter)
are dispersed. In this Gl-S(3~m) system, silica particles do not induce
microcracks because of their very small size. Figure 8 demonstrates the
variation of fracture toughness with volume percent of silica phase for Gl-
S(3~m) composites. It is found that fracture toughness increases slightly
with increasing volume percent of silica. This increase in toughness can
be attributed to direct crack-particle interaction mechanisms such as crack
deflection 13 resulting from large thermal expansion mismatch between con-
stituent phases. At 30 vol% silica, fracture toughness is found to be 0.84
MPa m1/ 2 .
o
Since the increase in toughness due to direct crack-particle
interaction must be only dependent upon volume fraction of dispersed phase
and independent of particle size,13 it may be quite reasonable to consider
that this value corresponds to Kc * in Gl-S(26~m) :30 vol% composite.

On the other hand, for the present type of composites where matrix
cracking occurs, it is difficult to estimate the microcrack density f without
the knowledge of the size and shape of microcracks. 6 In the absence of
definite inforwation in this connection, we assume here that the microcrack
density is low, so that KO ~ Kc * holds. Then, by taking the value of 0.84
MPa o m172 for KO' n is estimated at 0.762 from Eq. (18). With the values
n = 0.762 and Y = 0.971, XR is obtained at 0.0388 from Eq. (7).

1. 5 ,----,--..--,--.,.--,--.,--,

G1 - S( 311m)

1.0
T
T;Z; 0
o_2-- 2---.L
J..
... o-~-~-l

0.5

10 20 30

Volume % Silica

Fig.8 Variation of fracture toughness with volume percent of

dispersed silica particles for Gl-S(3~m) composites.

353
 1.3
o 0
1.2 00

o o 0
~a 1.1 o

-
<is
A..
o
~ 1.0

~ 0.9
Ko = 0.84 MPa·rn t
~-----------------
0.8

o 200 400 600 800

af / J.Lrn

Fig.9 Crack-growth resistance data for GI-S(26~m) :30 vol% com-

posite plotted against critical crack size af'

using the values for Ka, XR and as thus determined, Kc and af were cal-
culated from the indentation-strength data for GI-S(26~m) :30 vol% composite.
The calculated crack-growth resistance data are plotted using af as abscissa
in Fig.9; in the figure, we use the symbol KR instead of Kc following usual
notation for crack-growth resistance. It is found that this plot gives a
rising R curve as already expected. At af values around 700 to 800 ~m, cal-
culated KR values agree with the SENB data within the experimental scatters.
This seems to suggest that the saturation of KR is closely approached from
this crack size range. Thus, the indentation-strength procedure permits to
evaluate rather simply the R curve behavior of microcrack-prone material.

Tentative estimation of microcrack zone width. The product fe involved

in Eqs. (3) through (5) can be considered as an effective permanent dilatation
within the process zone, eT, which is the sum of the dilatation induced by
all the randomly distributed microcracks. As noted earlier, reasonable esti-
mations of e and f are difficult without the knowledge of microcrack size
and morphology. However, it is possible to evaluate e T from crack-surface
traction stress as, if we assume e T ~ 3(os/E). Taking as = 14.4 MPa and
E = 64.8 GPa(calculated Young's modulus of the composite containing 30 vol%
silica), we obtain e T = 6.7 x 10- 4 • This e T value may be reasonable in
the sense that the value is smaller than the volumetric thermal expansion
mismatch strain(3 x /';o.·/';T = 1.25 x 10- 2 ), which is directly related to e.

Eq. (5) can be written in terms of Kc * as follows;

1
( (1 - f) K c * + (22)
1 - Of

with known e T value, let us try to roughly estimate the value of h in the
Gl-S(26~m) :30 vol% composite. First of all, we assume that Kc determined
by SENB technique (= 1. 2 MPa'm 1/2 ) is close to the crack-growth resistance
at saturation. If we assume that the microcrack density is very low, h is
estimated at about 900 ~m. However, this may be an overestimated value for

354
h. On the other hand, if we assume randomly oriented annular microcracks
with size c around the equator of each spherical particle with radius R(i.e.,
outer radius of a microcrack is R + c), Hutchinson' s analyses 6 enable the
crack size parameter c/R and the microcrack density f to be calculated from
the values of aT , residual stress due to thermal expansion mismatch and
volume fraction of particles. This gives c/R ~ 1.1 and f ~ 0.26. With
this f value, we obtain h ~ 240 ~m. Naturally, these are tentative results
based on many assumptions, so their validity remains to be further examined.

CONCLUDING REMARKS

Toughening phenomena observed in the present microcracking model com-

posites could be interpreted well on the basis of a micromechanics model of
microcracking. However, the magnitude of the parameters, f, a and h in-
volved in the model has not yet fully inderstood in terms of material proper-
ties and microstructure. Then, further study should be undertaken to gain
quantitative knowledge of these parameters.

ACKNOWLEDGMENTS

This research was supported in part by a Grant-in-Aid for Scientific

Research on Priority Area "Advanced Inorganic Materials" from the Ministry
of Education, Science and Culture, Japan. The authors are indebted to
Prof. K. Komai of Kyoto University for scanning acoustic microscope that was
made available in his laboratory. Thanks are also due to Mr. S. Kinoshita
for his technical assistance in the acoustic microscopy.

REFERENCES

1. N.Claussen, J.S.Steeb and R.F.Pabst, Am.Ceram.Soc.Bull., 56, 589 (1977).

2. R.W.Rice, Ceram.Eng.Sci.Proc., ~, 661 (1981). --
3. D.J.Green, in "Fracture Mechanics of Ceramics", VoL 5, R.C.Bradt et aI.,
eds., p.457, Plenum Press, New York (1983).
4. B.Budiansky, J.W.Hutchinson and J.C.Lambropoulos, Int.J.Solids Struc.,
19, 337 (1983).
5. A.G.Evans and K.T.Faber, J.Am.Ceram.Soc., 67, 225 (1984).
6. J.W.Hutchinson, Acta Metall., ~, 1605 (1987).
7. J.Selsing, J.Am.Ceram.Soc., 44, 419 (1961).
8. D.J.Green, J.Am.Ceram.Soc., 64, 138 (1981).
9. F.F.Lange, in "Fracture Mechanics of Ceramics", VoL 2, R.C.Bradt et aI.,
eds., p.599, Plenum Press, New York (1974).
10. N.Miyata,S.Ichikawa, H.Monji and H.Jinno, in "Fracture Mechanics of
Ceramics", Vo1.7, R.C.Bradt et aI., eds., p.87, Plenum Press, New York
(1986) .
11. W.F.Brown, jr. and J.E.Srawley, "Plane Strain Crack Toughness Testing of
High Strength Metallic Materials", ASTM STP 410, ASTM, Philadelphia
(1966) .
12. P.Chantikul, G.R.Anstis, B.R.Lawn and D.B.Marshall, J.Am.Ceram.Soc., 64,
539 (1981).
13. K.T.Faber and A.G.Evans, Acta Metall., 31, 565 (1983).
14. N.Miyata, M.Ogawa, H.Ornura and H.Jinno, in "Proceedings of the 34th Japan
Congress on Materials Research", p.149, The Society of Materials Science,
Japan (1991).
15. W,Kreher and W.Pompe, J.Mater.Sci., ~, 694 (1981).
16. D.B.Marshall and B.R.Lawn, J.Mater.Sci., 14, 2001 (1979).

355
R-CURVE BEHAVIOUR OF ALUMINA AND PSZ AT AMBIENT

AND HIGH TEMPERATURES

M. Saadaoui*, C. Olagnon, and G. Fantozzi

INSA, GEMPPM, U.A. 341, Lyon, France

*Ecole Mohammadia d'ingenieurs, B.P. 765, Rabat Marocco

ABSTRACT

Some monolithic ceramics have been shown to exhibit increasing crack growth
resistance with crack extension.
R-curve behaviour of alumina and partially stabilized zirconia containing mainly
tetragonal or monoclinic phase has been investigated. The influence of the starting
notch (precracked or sawed), the environment, the temperature, the microstructure and
the toughening mechanisms has been studied.
For high tetragonal phase content PSZ that shows mainly transgranular fracture mode,
the starting notch shows no effect on the crack resistance curve. Along the rising part of
the R-curve, tetragonal to monoclinic transformation defers stress corrosion effect, while
along the plateau subcritical crack growth becomes preponderant and leads to a crack
growth resistance decrease. At low temperature, a crack growth resistance
enhancement is observed, owing to a concomitant decrease of stress corrosion and
increase of the phase transformation thermodynamic driving force.
Alumina and high monoclinic phase content PSZ show a similar behaviour. Precracked
notch produces a larger extent bridging that induces a higher crack growth resistance
than that obtained with sawed notch. Stress corrosion starts during the early stage of
crack propagation. Microcracking has been shown to contribute as well to the R-curve
effect.
A quantitative analysis of those results has allowed us to specify the toughening
mechanism parameters present within those materials.

INTRODUCTION

Several studies conducted on the crack growth resistance of polycrystalline alumina /1-
3/ and zirconia /4-8/ have reported an increase of fracture energy with crack extension,
so called R-curve behaviour. The R-curve provides a more refined analysis than a
unique parameter such as Klc or Glc. There is not, however a unique R-curve for a
material and it is strongly dependent on the environment, the specimen type, the crack
location and geometry as well as on the evaluation method.
Such a behaviour has been explained in terms of energy dissipation mechanisms such
as frontal process zone, some wake effect like bridging and friction between surfaces
/2,9,10/, crack deflection or stress induced phase transformation in the case of zirconia
based ceramics /11,12/. The contribution of each specific mechanism is however difficult
to estimate.

Fracture Mechanics of Ceramics, Vol. 9

Edited by R.C. Bradt el ai., Plenum Press, New York, 1992 357
 In the case of alumina, Steinbrech 113/, and Deverler 121 works have shown that R-curve
is not an intrinsic material property but depends on both microstructure, and loading
rate. Moreover, results have been shown to depend strongly on the testing method ie.
SENB, DCB and DT tests, which have been explained by the interaction crack opening
displacement/microstructure that varies with sample geometry.
Two main reinforcement mechanisms have been proposed:
(i) microcraking in the process zone in front of the crack tip which leads to crack
shielding,
(ii) crack surface bridging by interloking grains behind the crack tip.
Some researchers /141 have demonstrated the presence of a wake contribution to
reinforcement in alumina. They have monitored the R-curve behaviour on a straight
notch specimen. After sawing the wake of the first crack and recording again the R curve,
they show that the initial energy has returned to the initial value of the first experiment.
The existence of a process zone contribution to reinforcement has not been observed for
this type of material.
In the case of partially stabilized zirconia materials, it has been shown 13,6,15,16,171
from SENB and DCB experiments on Mg-PSZ that the initiation energy and the R-curve
amplitude depends on material microstructure. A high tetragonal phase content material
shows a starting KR value close to 7MPa.m 1/ 2 that can reach 18MPa.m 1/ 2 for a crack
length increment of 5001lm. However, it has also been shown that an approach in terms
of propagation energy R that takes into account the residual deformation after unloading,
leads to a decreasing R-curve, which has been explained by plasticity induced by phase
transformation at the crack tip.
The mechanism responsible for reinforcement is mainly t-->m transformation for high
tetragonal phase content, while microcracking and crack coalescence takes place in
material having a high monoclinic phase content. The existence of the process zone is
difficult to demonstrate, however some authors 1181 have clearly observed it in duplex
zirconia/alumina based ceramics.
The target of this work was to give more insights in the evaluation and the understanding
of R-curve behaviour of polycrystalline alumina and PSZ material. The influence of the
starting crack type, environment, temperature, microstructure and reinforcement
mechanisms on the crack propagation resistance has been investigated. Since the
evaluation method is of importance, the macroscopic behaviour of the material has been
first investigated.

I R-CURVE DETERMINATION

The R-curve is determined from the measurement of the stress intensity factor KR or the
energy release rate G as a function of the crack length. The difficulty being therefore to
obtain a controlled fracture all along the loading cycle. Several methods are usually
applied, depending on the material behaviour ie.: (i) linear elastic, (ii) linear non elastic
or (iii) non linear.
When the material behaviour is linear elastic, the stress intensity factor may be
determined as a function of the crack length "a" according to the relation:

KR =(J.Y.a 112 (1 )

with (J applied stress. G may therefore be calculated from the relation between G and KR
or directly from:

G = (p 2/2B).dC/da (2)
wher C, is the material compliance, B sample thickness and P applied load.
When the material shows a linear non elastic behaviour due to energy dissipation
mechanisms, a remnant deformation is still present after unloading. In such a case, G
must be separated into two terms:

358
 G = G' +$ir (3)

where G' is the propagation energy and cl>ir the contribution to irreversible mechanisms.
When the materials show a non linear behaviour. the R-curve may be obtained from the
J integral concept. Several methods for determining the J integral has been proposed in
the literature, among which two were proposed by Sakai /19,20.21,22/.
The first one consists of conducting cyclic loading of samples. The total energy
associated to crack propagation is obtained from the increase of crack surface between
two cycles. which is measured from the area in the load displacement curve. This area
may again be separated into two parts:

~1t = ~1te +~1tir (4)

where ~1te corresponds to the net propagation energy and ~1tir corresponds to
dissipative mechanisms.
The second method of Sakai is based on a monotonic loading of the specimen. The
load displacement curve is compared with a dimensionless curve corresponding to a
linear elastic behaviour. The crack propagation resistance may therefore be calculated
according to:

R=G+Rir (5)
where Rir corresponds to the irreversible dissipative mechanisms.

II EXPERIMENTAL PART

11.1 Material

Three different materials types have been used: Alumina (A 1), and two grades of
partially stabilized zirconia: (PSZ1) and (PSZ2).
The (A1) alumina is a 99.7% pure polycrystalline alumina (AF997, Desmarquet
Ceramique technique, France) with a density equal to 3.95g.cm-3 .
The two other materials have been obtained from heat treatment of 9mol% Mg-PSZ
(Desmarquet Ceramique technique. France). The starting material is constituted of a
cubic matrix containing tetragonal and monoclinic phase precipitates. The volumic
proportions of the different phases present in the material have been evaluated from X-
ray diffraction peak intensities from Garvie /23/ relationship. PSZl and PSZ2 have been
heat treated at 1OOO°C/l hand 1300°C/6h respectively. The phase contents are
displayed in Table I. It can be seen that the tetragonal phase content of the PSZ2
material is very low compared with that of the PSZl material.

Table I. PSZ characteristics

Heat-treatment Vm(%) Vt(%) Vc(%)

PSZl 1000°C/l h 7.5 28 64.5
PSZ2 1300°C/6h 55 3 42

11.2 Sample preparation

The toughness and crack propagation measurements have been recorded on two
different three point bending specimens: (i) Single edge notched beam (SENB) where
the notch has been made in two steps: a pre-notch is made with a 0.3mm thickness saw
and a second thin notch is made at the end of the first one with a 70jlm cutting wheel. (ii)
Single edge precracked beam (SEPB) on which precracking has been induced by

359
 ~------6'-H'-+-----------

--,------1(1+,1-11--1-1------.--- -

-.:....----:.----Il+JI:f-I+:l-lfk--------·-

Fig.1. Alumina. Cyclic load-displacement curve on a SENB sample.

bridge indentation method /24,25/. In this case. the samples were polished down to 11lm
on the three faces and the crack has been initiated from three indentation cracks
regularly made on the sample face(100N load).

11.3 Calculation of the crack resistance parameter

Cyclic loading of alumina samples have been carried out. Fig.1 shows that cycles
present some hysteresis initiated at the onset of crack propagation. Moreover, a residual
deformation is to be noted. The first Sakai's method has therefore been applied to
calculate the elastic and non elastic contribution to fracture energy. It is to be noted that
non reversible phenomena contribution dominates the fracture. Acoustic emision
recorded during the loading has shown that the permanent deformation could be
attributed to debris formation that prevents the crack from closing, and does not
correspond to fracture. Moreover, the stiffness at the loading step or at the un-loading
step is different.
This method based on cyclic loading leads to erroneous results of Re and Rir since the
residual deformation is only apparent.
Thus monotonic loading that prevents damage due to cycling has been applied. The
fracture energy R has been calculated according to the second Sakai's method. The
result has been represented in Fig.2 where the fracture energy KR2/E obtained under the
assumption of a linear elastic method has also been represented. It is clear that the
fracture energy calculated from Sakai's method does not show any significant
differences with that calculated under the assumption of a linear-elastic behaviour. Such
a good agreement has also been constated with PSZ material.
Finally, at low temperature, the R-curves have been characterized using a monotonic
loading under the assumption of a linear-elastic behaviour. However, at high
temperature, the second Sakai's method has been applied since the above hypothesis
could not be supported any more.

360
 120 r----.---~
,----.---~----.--.,
[]

O'---........--..L..-----"---....L...------''--_-J
o 1 2 3
6a (mm)

Fig.2. Alumina. R-curve calculated from J-integral evaluation method proposed by

Sakai/21 ,22/ from monotonic loading, and from KR evaluation under the assumption of
linear elastic behaviour.

III RESULTS

111.1 Alumina

Preliminary experiments (Fig.3) on alumina SENB specimen have shown that the R-
curve was independent of the starting notch depth for crack length to sample thickness
ratio (aIW) between 0.3 and 0.7. Only a minor initial stress intensity factor fall off has
been recorded for aJW=0.7 and assumed to be due to edge effects, which shows that the
method is relevant even if the initial crack length varies.

2'--..L...-...L..-""""--...L............--'----J..---'---"--''--'"-.L..-.............,
0,3 0,4 0,5 0,6 0,7 0,8 0,9 1,0
?NV

Fig.3. Alumina. Influence of the relative notch depth on the KR curve.

The effect of the starting notch radius on the R-curve has been investigated. For this
purpose, a notch has been made with a 0.3mm thickness saw that leads to a tip radius of
1501lm. FigA Shows that the starting toughness goes from 2.77 MPa.m 112 for a tip radius
(p) of 351lm to 3.3 MPa.m1/2 for a radius of 150llm and the discrepancy decreases with
increasing crack length. The effect of a natural crack (SEPB) has been represented in
FigA. The starting KR value, for the same relative depth, is much higher than that

361
obtained with SENB (p=35J.lm). Moreover the whole SEPB curve is above that
measured on the notched specimen. This may be explained by considering that the
crack surfaces of the SEPB specimen are not stress free. Surface contact may lead to
wear, interlocking mechanism or any energy dissipating mechanisms.

7..-----r---..----.. . . . .- --.,,----r----.,

4 lC lC lC .\\.* • •• ~:f •• y
lC ~• • • lC SENB 170 I.l
3 •••• • SENB 35 I.l
o SEPB
2L.-_......_ _L.-_......_----JL...-_......_---'
0.6 0,7 0,8 0,9
Relative crack depth

Fig.4. Alumina. KR-curve of SENB(notch radius of 35mm and 170mm) and of

SEPB sample.

The influence of the subcritical crack growth (SCG) on the R-curve has also been
investigated by carrying out experiments under different environments as well as at low
temperature. R-curve have therefore been recorded in ethanol. In this later case, the
specimen was first hold at 100°C for 3 hours, then immerged in alcohol for 30 mn before
the experiment. The crack resistance curve obtained in alcohol is clearly above that
obtained in air (Fig.5). This result may be correlated with the subcritical crack growth
reduction associated with low moist medium such as absolut ethanol. It is as well
important to note that KR reduction observed after the maximum value in air is not
present in alcohol.

8 .
• Air
0
0 Ethanol 0
7 0
000 0

.,• ..................
000 o 0 o 0 0 0
E
7 ~
11l 0
D.. 6
6
II: •• ••••
~

5 .; •
•
4L...--........---'---"----'-----'---.L..-l
0,6 0,7 0.8 0,9
Relative crack depth

Fig.5. Alumina. KR-curve measured in air and in ethanol.

The influence of slow crack growth has also been investigated with experiments
conducted at -65°C (Fig.6). The samples were cooled by projection of liquid nitrogen in
a thermally insulated box and the temperature was recorded with a thermocouple near

362
the sample. The crack resistance curve at low temperature is clearly above that obtained
at 20°C. The high KR value at the propagation onset may be attributed to subcritical
crack growth decrease at low temperature like it is in alcohol.

,.:
6r-----r----.---.--..,.--...---,r-----r---,

••••••• • • • •
5
• • •• •
aaaaa
19 aa E:tI aO 0
4 a0 0
E oaO
a O
"?
~ aO
::E
C(
~
3 r'
0
•a -65°C
20°C

2
0,0 0,5 1,0 1,5 2,0
~(mm)

Fig.6. Alumina. KR-curve at ambient temperature and at -65°C

Controlled fracture of SENB alumina has been carried out at 800°C and 1000°C (Fig.7).
Maximum load decreases with rising temperature and non linear deformation
contribution increases. Initial R values at 800°C and 1000°C are similar but slightly
lower than that at ambient temperature and the R-curve slopes significantly decreases
with rising temperature.

,-.....,--"""T'"--or----,
,•
120 ......--,..--"T"""

100

80
••• .
•••
•• rP
la:
60
•••
••••••
a a
rP#
40 •••• aaO 0
•• 0 a 0
oa 0000000 aD
20 ~e r:P eP 0 0

Ol.--.........--L---.........- -L---........-----'
o 2 3
6. a (mm)

Fig.? Alumina. R-curve at ambient temperature, 800°C and 1uUO°C. Note that the
behaviour has not assumed to be linear.

11.2 Zirconia

For comparison, the R-curve of the two zirconia grades have been recorded on SENB
specimens (Fig.8) For the lower tetragonal phase content material, the initial value is
equal to 5.6MPa.m 1/2 and fastly rises up to 7.8MPam 1/2 for a M=600llm and decreases
for further crack extent. Although the initial value observed for the PSZ2 sample is much
lower, the rising domain is longer. The decrease of KR curve after the rising part has
been attributed to slow crack growth.

363
 •••••• •••••• • •• • •
10

• •• ••
8 •
•C~~""~dIoe dIn!l ~.
•
• C~
E
Cil
Q. 6
~ 00000 0000 0 QDooOo
a: 00
::.::: 00 00
0
4 0 ~ ~
0
# 0 SENB C SENB
• SEPB • SEPB
2
0 1 2
11 a(mm)

Fig.a. PSZ. KR-curve from SENB and SEPB sample for PSZ1 (high tetragonal phase
content) and PSZ2 (high monoclinic phase content) material.

The influence of the starting crack has also been investigated on PSZ1 and PSZ2
samples (Fig.8). The R-curves of PSZ1 are very similar and therefore do not seem to
depend on the starting crack. The monoclinic high content phase shows a different
behaviour. The R-curve corresponding to SEPB specimen is clearly above that
corresponding to SENB. The initial and plateau values rise from 2.8 and 5.3 to 6 and
9.8MPa.m 1/2 when starting with a natural crack. In this later case, the effect of the
starting notch on the crack resistance curve is similar to that observed for alumina.

9,...-----...----,-----.-------,
. . . . . . . . . . . . . . . . • ccccce
rI' aJoObD C D Dc CCCC • •
000 0 00000000
0 0 0

- ...
7 E.SZ..l.;
.. ; 6 .. .e. .e..e..e... 6 ..

..........
.. .e..e. o Air
.... .e..e.. C Ethanol
.. water
••••••
•• .. ..........
r.I
3
• Air
• Toluen
.. Water
1L.-----'----....L------''-----'
o 1 2
11 a(rrm)

Fig.9. PSZ. KR-curve from SENB samples of PSZ1 and PSZ2 in air, in water and in a
low humidity content medium.

The influence of slow crack growth has been investigated from experiments conducted
in air, in water and in a low humidity medium. For the high tetragonal phase content
material, while the starting parts of the several environment KR-curves coincide, the
differences increase with increasing crack length. The KR decrease observed in air is
significantly accentuated in water. Moreover, some instabilities have been observed in
this later case. On the contrary, experiments conducted in alcohol leads to a
continuously rising R-curve.
The influence of the environment is very different in the case of the PSZ2 material. The
different K-curves are systematically shifted to higher K values with decreasing humidity.

364
Those results show that the crack resistance is strongly dependent on slow crack growth
which depends on the microstructure.
R-curve obtained at low temperature, are again higher than that obtained at ambiant
temperature.
Observations of fracture surfaces (Fig.10) show that the fracture of the PSZ1 material is
mainly transgranular while that of the PSZ2 material is both trans- and intergranular.

Fig.10. SEM micrograph of fracture surface of (a) PSZ1 material and (b) PSZ2 material.

IV DISCUSSION

The R-curve of alumina is generally attributed to interaction between surface cracks due
to debonded grains in the crack wake /14,26/. The above reported results on relative
crack length on R-curve behaviour and comparison between SENB and SEPB samples
sustend this hypothesis. The experiment conducted on SENB has shown that the
starting value of R-curve at different crack length are identical. Since the crack surfaces
are free from interactions at the propagation onset, the starting values are the same, and
when the crack growths, compressive stresses on crack surface lead to reinforcement.
The crack surface interactions explain the result differences observed between notch
and pre-cracked alumina samples.
It is to note that when the controlled rupture experiment is conducted straight after
precracking (before any annealing), no reinforcement is observed, which means that the
interaction zone has reached its maximum length value. Annealing the sample after
precracking leads to residual stress relaxation, however, during controlled crack
propagation, interactions are again developped, which again lead to material
reinforcement. The higher level of K-curve obtained on SENB sample may be explained
by observing that those residual stresses may be not fully annealed.
The reinforcement observed in alumina may be characterized by the interaction length
Zm and by crack opening at the end of that zone Om (Fig.11).

365
 Crack Tip

I
I
I

~'
Zrn

Fig.11. Schematics of the bridging zone in the crack wake

Sakai /27/ has proposed an experimental method to calculate this interaction zone. The
KR-curve must be plotted as a function of the square root of the crack increment:

KR = Ko + 4 op ~ zm/21t (6)

where Ko is the starting stress intensity factor. The crack opening may be also
calculated from:

8 _ rz;; _rz;; Ko
Om = E '{p [ap \j p + -{2 ] (7)
This theoretical calculation has been established under the assumption of a KR-curve
exhibiting a plateau.

Table II . Alumina bridging parameters.

ap (MPa) zm (j.U11) Om (j.U11)

SENB 32 676 1,05

SEPB 41 225 1,08

The values of ap, Zm and Om are presented in Tablell for SENB and SEPB samples. The
bridging stress value is in good agreement with values reported in the literature on
similar material /28,29/. The value obtained for SEPB is larger owing to the residual
stresses exerted on crack surfaces. While the interaction zone of the SENB specimen
starts at the onset of crack propagation, it starts during precracking for the SEPB
specimen. The Zm length, therefore corresponds to the extension of the zone and not to
the maximum zone length. It is important to note that stress corrosion (experiments in air)
may increase the crack growth value before steady state, which means that the value of
Zm is overestimated for SENB.
It is important to note that although interlocking grain interactions seems to be the main
reinforcement mechanisms, other mechanisms are operating. Crack deflection and
crack branching have been observed by SEM. However the specific contribution of
those concomitant mechanisms is difficult to specify.
While the tetragonal phase content of polished PSZ1 is equal to 28%, only 7.6% is
measured on fracture surface of tested samples. This shows that t-->m phase
transformation occurs during material fracture, which leads to reinforcement in that case.
The behaviour of the PSZ2 material is far different. Both the contribution to slow crack
growth and the influence of the natural crack are different. Since the tetragonal phase
content is very low (3%), the reinforcement by t-->m phase transformation is negligible
and the main mechanism is bridging of crack surfaces behind the crack tip, driven by the
intergranuar fracture mode observed in this type of material. In the end, the behaviour is

366
similar to that observed in alumina. The bridging characteristics calculated from
equ.(6)&(7) applied to a SENB specimen gives: op=52.5MPa, zm=960lJ.m and
&1=3.7J.1.rn.
Those results show that crack bridging is directly linked to intergranular fracture mode.
However, fracture is different in alumina and PSZ2: the intergranular fracture of alumina
is related to grain size while that of PSZ2 to microcracking at the grain boundaries.
Crack growth resistance of alumina or zirconia is clearly influenced by subcritical crack
growth since at low displacement speed, the time during which SCG takes place is
significant. The real crack length is therefore higher than initial crack length value. For
instance, controlled fracture in air leads to a KR decrease which has also been reported
in the literature /30/. The t-->m transformation that leads to the observed reinforcement,
reduces the subcritical crack growth. The KR decrease due to SCG is counteracted by
the increase due to phase transformation at the onset of crack growth (rising part of KR-
curve). At the plateau, the phase transformation contribution is maximum and can not
match the SCG, which leads to KR decrease in water or in air.
For Alumina and PSZ2, SCG influence is observed at the onset of crack growth since
the whole curve is shifted towards higher values. Bridging grains do not allow to delay
SCG effect and SCG is promoted by intergranular fracture and by potential
microcracking.

CONCLUSION

R-curve behaviour of alumina and partially stabilized zirconia has been investigated.
Although alumina and PSZ do not exhibit a linear elastic behaviour, it has been shown
that R-curve calculated under this assumption, from KR values, was very close to that
calculated from the J-integral.
It is desirable to avoid cyclic loading which leads to erroneous results owing to debris
that prevent the crack from closing during the unloading step.
High tetragonal phase content PSZ, that exhibits mainly transgranular fracture mode
does not show any effect of the starting notch on the crack resistance curve. Moreover,
the stress corrosion effect is deferred along the rising part of the R-curve by t-->m phase
transformation.
Alumina and high monoclinic phase content PSZ show similar R-curve behaviour. The
influence of the starting notch is significant and precracked initial flaw leads to higher
crack growth resistance owing to the interlocking grain bridging zone induced by
transgranular fracture mode. Sress corrosion starts during the early stage of crack
propagation.
High temperature R-curve have only been recorded on alumina because zirconia has
been seen to exhibit brittle behaviour. However, R-curve of alumina strongly decreases
with temperature.

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 7: M.J. READY, A.H. HEUER, A.W. STEINBRECH - Crack propagation in Mg-PSZ -
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369
R-CURVE BEHAVIOR OF PZT CERAMICS
NEAR MORPHOTROPIC PHASE BOUNDARY

S. Baik, S. M. Lee, and B. S. Min*

Department of Materials Science and Engineering

Pohang Institute of Science and Technology
Pohang 790-600, Korea

ABSTRACT
The aim of this study is to investigate the characteristics of mechanical failure of
PZT ceramics in terms of their compositions and microstructures near morphotropic phase
boundary where commercial applications are mainly concentrated. R-curve behaviors are
identified by indentation-fracture testing and analyzed to determine key parameters related.
It is found that the fracture toughness is composed of three different terms representing
particular microstructural processes in front of advancing cracks; intrinsic cleavage, 90°_
domain switching, and microcracking. Their relative contributions to an over-all crack
extension resistance varied depending on the length of advancing crack and, more
importantly, the composition of PZT. The study also demonstrates that R-curve analysis ca
be utilized to probe further into the microstructural responses of materials in front of
advancing crack and to quantify them, particularly, in the situation where several different
processes are competing each other in the system like PZT.

INTRODUCTION
Lead Zirconate Titanates or PZT are widely used as a key material for various
sensors and actuators[I,2]. The ferroelectric properties of polycrystalline PZT are highly
sensitive to the compositions and microstructural characteristics. For specific applications,
one has to tailor their compositions, porosities, grain sizes, domain structures, and so on.
However, the optimization of ferroelectric properties does not necessarily guarantee the
mechanical stability of PZT ceramics. They are often conflicting each other. The aim of
this study is to establish a relationship of the mechanical failure of PZT ceramics to their
compositions and microstructural variables by analyzing R-curves near the morphotropic
phase boundary(MPB), where the ferroelectric properties such as the coupling coefficient
and the relative permittivity are usually maximized.
The solid solution system Pb(ZrxTi 1_x)03 exhibits a number of crystal structures
depending on x as shown in Fig.I, a phase diagram of PbZr03-PbTi03[3]. An abrupt
structural change between tetragonal and rhombohedral phases occurs at MPB which is
known to be close to x = 0.535 for undoped PZT. Therefore, MPB denotes a narrow region
of x where tetragonal and rhombohedral phases co-exist. A significant feature of MPB is
*Now with Samsung Electrics, Suwon, Korea

Fraclure Mechanics o/Ceramics. Vol. 9

Edited by R.C. Bradt el aI., Plenum Press. New York, 1992 371
 Tetragonal

Rhombohedral
(high-temperature
foim)

Rhombohedral Morphotropic
(low-temperature phase boundary
Orthorhombic
form) \
0.8 0.6 0.4 0.2

Fig. 1. PbZr0 3-PbTi03 subsolidus phase Jiagram[2, 3].

2000 I
I
I
0.7
I
I
I 06
1500 I
I
I 0.5
I
I
I
I 0.4
1000

!J
€,
I kp
0.3
I
I
k I 0.2
500
€, i 0.1
I
I

PbZrOJ PbTiO J

Fig. 2. Coupling coefficient ~ and permittivity € r versus the composition of PZT. The
maximum values occur at the morphotropic phase boundary [2].

that most of the ferroelectric properties change rapidly near MPH and peak at MPH as
shown in Fig.2[3]. Therefore, the compositions near MPH have been exploited heavily for
commercial applications. However, Freiman et al.[4] recently demdnstrated that the critical
fracture toughness(K1C) of various commercial PZT components shows a distinct minimum
at the MPH. The fracture toughness data are reproduced in Fig.3. Large decrease in K1C is
evident near MPH. However, the data is not sufficient to determine whether the minimum
K1C is coincident with the exact position of MPH. It has been already established that the
MPH varies significantly depending on the types and amounts of dopants which are
frequently added in commercial compositions[3]. They are not specified in the data
presented in Fig.3, which make it improper to be utilized for the compositional formulation
of PZT ceramics with higher fracture toughnesses.

372
 2.0

1.8 r-
•
t:!
-~ 1.6 r-
t
a.
-- t
to

tI •
I
~ \ to

.',
, I
I
!J 1.4 l- I

:ll:: \
\
\
I
\ I
\ I

- 1
\
1.2 \

-',ii •
\
\ I
I

,
1.0 -
I I I I -, I
0.9 0.8 0.7 0.6 0.5 0.4 0.3

PbZr~ .--x PbTi03-

Fig. 3. Critical fracture toughness, K,c as a function of the composition of various
commercial PZT ceramics[4].

Freiman et al.[4] argued that the minimum in fracture toughness observed in PZT
is due to a trade-off between the contributions of twinning (90°-domain boundary motion)
and of microcracking of grain boundary facets with residual tensile stress. At the MPH,
the twinning is facilitated and contributes to reducing crack extension force. Away from
the MPH, particularly toward PbTi03 in the tetragonal phase field, the contribution
of microcracking becomes increasingly important, while that of twinning diminishes. It
was thus explained that the minimum in K,c appeared because the toughening due to
twinning is less effective than that due to microcracking. On the other hand, Mehta and
Virkar[5] demonstrated convincingly that domain switching (twinning) in the stress field of
a crack tip is a viable toughening mechanism in fully-tetragonal PZT ceramics. The
samples they used for fracture toughness testing were of commercial PZT ceramics with x
= 0.54, which implies that the MPH of the composition is located at x > 0.54 due to the
presence of unspecified dopants.

In the situations when any dilatational relaxation processes are operating in front of
(or, in some occasions, behind) the advancing crack and thus promoting a toughness
increase, R-curve behaviour would be inevitably observable[6]. The characteristics of R-
curves, rising fracture toughness with crack extension, are sensitive to the mechanistics of
particular relaxation process at the crack front. The most prominent example can be found
in partially stabilized zirconia (PSZ)[7]. A variety of microstructures could be produced by
simply taking different thermal processing routes using polycrystalline zirconia stabilized
with 9.5 mol% MgO. The characteristics of R-curves determined afterward were found
dramatically different as shown in FigA. For PSZ containing tetragonal zr0 2 precipitates
which transform readily to monoclinic phases in a crack front, the R-curves were rising fast
but saturated at high toughness values within 20-30Jlm of initial crack length. Whereas, for
PSZ with continuous m-ZrO? phase showing extensive microcracking and crack branching,
they were rising slowly but continuously over a large crack extension upto a few hundreds

373
11m. Furthermore, in the case of alumina where R-curve is believed to be originated from
the bridging of unbroken ligaments of the grains behind the crack front, the R-curve was
rising continuously even upto a few mm of crack length[8].

An evidence of R-curve behavior in ferroelectric materials was, in fact, presented

by Okazaki in 1984[9]. However, as pointed out later by Mehta and Virkar[5], their interpreta-
tion of the observed dependency of fracture toughness on indentation crack size was
incorrect. The parabolic dependency of K1C on c, crack length, is not due to residual stress,
but most likely due to an R-curve behavior. Non-linear dependence of log fracture strength
on log indentation load in PZT with x =0.95 was also interpreted mistakenly in terms of
residual stress[4]. Pohanka and co-workers[lO,ll] uncovered strong correlation of K 1C with
microstructural parameters, e.g. grain size, in another commercially-important ferroelectric
material, BaTi0 3. Cook et al.[12] re-interpreted it later in terms of an R-curve behavior.

14~-------------,

t 12 Transformation Toughening

~
! 10 Microcracracking

I 8

I
CI

~!
:l
6 I Mg-PSZ

~ 4

o 200 400 600 800

Crack Extension (11m)

Fig. 4. R-Curve behaviors with two different microstructural conditions[7].

Special features of examining R-curves of polycrystalline ceramics are that, firstly,

the dimensionality of microstructural parameters which affect crack-tip stress field can be
identified because the critical crack size below which rising K1C can be observed is believed
to be directly related to a toughening zone size in front of the crack tip. Secondly, it
provides us with the asymtotic values of K1C at the higher end of crack-size spectrum that
can be used safely for the evaluation of effectiveness of particular compositional or micro-
structural variations on fracture resistance.

EXPERIMENTAL PROCEDURES

Specimen Preparation

The compositions selected for the present study were Pbo.94Sro.o6(ZrxTil_x)03' a

typical hard PZT, with x varying between 0.50 and 0.60. The starting materials were PbO,
ZrOz' TiOz' and SrC03 with >99.5% of purities. 3.0 mol% of excess PbO were added in all
the compositions in order to compensate for PbO loss during calcination and sintering.
After mixing by ball milling in ethyl alcohol, the dried powder batches were calcined at
850°C for 4 hours. The calcined powder were crushed and ball-milled for 24 hours, and
pellets were made by cold isostatic pressing at 150 MPa. The pellets were fired at 500°C for

374
5 hours to bum out binders, and then sintered at 1250°C for 2 hours. To minimize PbO-loss
during sintering, a PbO-rich atmosphere was maintained by placing environmental powder
(PbZr0 3 + 10 wt% ZrO z) between the pellets in a closed alumina crucible[ 13]. Sintered
densities were determined by the Archimedes' technique, and the grain sizes were measured
by the linear intercept method.

Determination of MPB

Crystalline phases, and their lattice constants were determined by X-ray diffraction
(XRD) of powder samples taken from the sintered pellets. The relative amount of each
phase, tetragonal(T) and rhombohedral(R) phases, was determined by measuring the
integrated intensities of corresponding XRD peaks, T(200)+T(002) and R(200),
respectively. Being overlapped, they are separated by running a multiple peak separation
program* before taking integration. The percentage of each phase was calculated using the
following equation. For instance, for the case of R-phase,

% R-Phase = x 100.
I.r(ZOO) + I.r(002) + I R(200)
where I's represent the integrated area of XRD peaks. Lattice constants were determined by
using a lattice constant refinement program*.

Indentation-Strength Test

Some of the samples were selected for the Vickers indentation and subsequent
uni-axial 4-point bending tests. The dimensions of bending bars were 3mrn x 4mm x
25mm. After machining, they were polished and annealed at 1100°C for 30 minutes to
eliminate surface flaws as well as residual stresses prior to the testing. The edges of the
specimens were rounded. Some of the specimens were electrically poled in the direction
parallel or perpendicular to the crack advancing plane[5,9,14]. An electric field of 2.5
kV/mm was applied for 3 min at 100°C in a dielectric oil. The specimens were indented at
the center of their tensile faces with a Vickers diamond pyramid. The indentation loads
varied from 5N to 200N. All indentations were made in air with a steady loading rate that
required 15 sec to produce a full load and another 10 sec under the full load. Care was
taken to orient one set of radial cracks normal to the tensile axis. A drop of silicon oil was
placed at the indentation site immediately after the indentation to minimize fatigue effects
[14].

Uniaxial bending tests were performed in a 4-point bending fixture made of 7mm
inner span and 23.5mm outer span. The bending strength was calculated from the following
equation;

(1)

where F is the maximum load to break the specimen, II = 23.5mm, 12 = 7mm, b = 4mm, and
t = 3mrn.

RESULTS

Table I summarizes the microstructural characteristics, the phases identified, densities,

and grain sizes of the specimens prepared for our experiments. The variations in final
densities and grain sizes are insignificant in comparison to the phase change observed.The
fractional amount of each phase within MPB region where T- and R-phases are co-existing
was determined by the XRD patterns illustrated in Fig.5 after separating overlapped
T(200), T(002), and R(200) peaks as demonstrated in Fig.6. The MPB region where the

*Rigaku, Japan

375
Table I. Microstructural Properties of PZT Ceramics, Pbo.94SrooiZrxTil.•)03' prepared for
mechanical testing.

Specimen x Phases Density(g/cm2) Grain Size (Ilm)

PZT50 0.50 T 7.40 6.5

PZT51 * 0.51 T 7.36 5.6
PZT52 0.52 T+R 7.45 6.0
PZT53 0.53 T+R 7.45 6.3
PZT54* 0.54 T+R 7.48 8.0
PZT55* 0.55 T+R 7.62 6.0
PZT57 0.57 R 7.52 7.1
PZT60* 0.60 R 7.63 10.9

* used for indentation-strength tests.

PZT57

- >.
'iii

-
c:::
Q)

.E

\__.._JJ1\ .-,~
20 30 40 50 60 70
2 (degree)-

Fig. 5. XRD peaks of experimental PZT ceramics.

two phases are present was in the composition range, x = 0.51-0.57. As shown in Fig.7, the
exact MPB where the two phases are in equal quantity appeared at x = 0.554. Apparently,
the doping of 0.06 mol% SrO induced slight shifting of MPB toward R-phase field. It is
also interesting to note that a simple lever rule can not be applied to detennine the phase
quantity within the MPB region, contrary to the suggestion by Nomura and co-workers
[15]. Unit cell distortions of T-phase (cia) and R-phase (90°-a) are determined and plotted
in Fig.8.

Fig.9 is a plot of the fracture strength (am) versus indentation load (P) for some of
the samples shown in Table I. A distinctive feature of the data is that all approach a plateau
at the lower end of the indentation load. It is a definitive demonstration of R-curve

376
 40 .----------------~-------~----...,

30

?:
'iii

-
c
CIl 20
E

10

o -. l i i-J..1-~
~T "- ••

43 44 45 46
28(degree) -

Fig. 6. XRD peaks separated by a multiple peak separation program. The peaks from the
left are T(002), R(200), and T(200).

1009-------.lr----r-------"7!=-&----,

80

III
~ 60

-
III
~
0.
o

-c
.2
( ,)
III
It
40

20

_
09-------L._...L--.loL-----L.----L.....I..----J_--l-_~~ ___L.._____J

0.60 0.58 0.56 0.54 0.52 0.50

-x -PbTiOJ

Fig. 7. The fraction of phases as a function of x, the mole fraction PbZrO y The exact MPB
is found to be at x=0.554.

377
 I
I
I
I
I
C I
t
b0- I 1.03
I
I ....tV
. ...
C I U
0 I
:;: t c
1 0
0
1;) I 1.02
:c 1° 1
I 0
I 1;)
! I :c
"0
I
I
1.01 'i
.! I c

-~
I
.0
I
~
E
0
9 ~
~
a: 0°
~

L..---L._ _- - L _ - ' - - - 1 1 . -_ _.L..-_ _...L-_ _-'------'0.99

0.60 0.58 0.56 0.54 0.52 0.50

PbZr03 - -x ""-PbTi0 3
Fig. 8. Unit cell distortions at room temperature for tetragonal and rhombohedral phases
nearMPB.

behavior[12]. Interestingly, the asymtotic values of om at the lower end of P are almost
identical. It indicates that the flexural strength of the material does not change greatly while
its composition and phases varies. On the other hand, the critical indentation load (P*)
below which R-curve behaviors are observable changes significantly as the composition
moves away from MPB toward T-phase field. At the higher limit of P, log om became
linearly dependent on log P with a slope of -1/3. It suggests that 0mpl13 is appproaching a
constant value asymtotically and the asympotic values of fracuture toughness which are
independent to P (or c) can be obtained from a linear indentation fracture mechanics[16].

R·CURVE ANALYSIS

Cook et al.[12] proposed a closed-form solution of an apparent fracture toughness

as a fuction of indentation load from a simple extension of the indentation fracture
mechanics[16]. It was also shown to be applied reasonably for analyzing the indentation-
fracture testing results of various ceramics materials including BaTi0 3• The proposed
equations of the fracture strength as a fuction of indentation loads are,

(2)

where Of denotes the asymtotic value of am in the limit of small crack. Then, the critical
fracture toughness over the entire range of P can be obtained from the equation given by
Chantikul et al.[16],

(3)

It is thus possible to define the R-curve function Kc(P) combining Eqs.(2) and (3) such
that,

378
 100

80

"....,
60
c
Cl..
:::E
.......,
J
-
40
~
C)
r:::
CD
~
III

- PZT51
CD
L 00000
::J
20
AA~AA
PZT54
PZT55
()
c
PZT60
L
u... 00000

1~:'::-On-----..Jl0-::1f,--------...Ll0""'2-----103

Indentation load, P (N)

Fig. 9. Plots of fracture strength versus indentation load for PZT with different
compositions.

2D r - - - - - - - ' - - - - - - - - - - ,

~c 1.5 PZT54
Cl..
:::E
()
~

Iii
III
CD
r:::
~ 1.0
C)
::J
.E
CD
L
::J
(;
C
L
u...

o·~L,6:r----....l10-.r----1L01;-----1...L~..-------...J103

Fig. 10. Fracture toughness as a function of indentation load obtained from the data in
Fig. 9.

379
 (4)

where K:represents the upper limit of toughness in high P region. Hence, the value of ~
may be calculated directly from

(5)

using or and p* determined by Eq.(2). The solid lines in Fig.9 represent the least-square fit
of Eq.(2) to the experimental data with two adjusting parameters, or and P*. The fitting is
surprisingly good. The resulting R-curves computed using Eq.(4) are shown in Fig.10. A
cutoff value of Kc at the low-P end of the curves is adopted to be 0.6 (MPa"m). It was
determined from the specimen electrically poled perpendicular to the crack plane (see the
following Discussion). Ko represents an intrinsic toughness determined either by surface
energy or by grain boundary energy in the Griffith formulation. Hence, K o can be assumed
constant, and insensitive to x or P. We then define Kc as

(6)

where K~(P) denotes all the microstructural contributions on fracture toughness. Now, the
remaining task is to define K~(P) in terms of microstructural parameters of relavant
toughening processes.

Table II summarize the values of key parameters determined. For each P*, we can
also estimate a critical crack length c*, which might be correlated to a zone size of the
relavant toughening process. Estimated values of c* and their normalized values with
respect average grain sizes are also included in the table.

Table II. Indentation-Fracture Parameters of PZT Ceramics.

Composition Or (MPa) P*(N) K~ (MPa-.Jm) c* (Ilm) (c*/d+)

PZT51 67 61 1.82 203 36

PZT54 77 16 1.43 97 12
PZT55 75 8 1.21 69 12
PZT60 76 9 1.24 73 7

+ average grain size

DISCUSSION

It has been shown that the indentation-strength test data could be reasonably
analyzed by following the R-curve model proposed by Cook et al.[12]. The major criticism
of the model was that it often has not been possible to get the slope of -1/3 at large
indentation loads in the plot, log om vs log P, particularly in large-grained alumina[l7] and
whisker-toughened ceramic composites[l8]. However, alternative power-law descriptions
were not adequately fitting all data over a wide indentation load spectrum with a single
value of the power-law exponent. Justification of adopting the model proposed by Cook et
al.[12] to PZT ceramics lies in the fact that the typical dimension of toughening zone
influencing rising K~ is limited within about 30 grains at most in front of crack tip (Table
11).

380
 2.0
-0- K~[Eq.5]
K;'
;:E --<>- Kc Ondentation]
-+- K~[poled]
& 1.5
~
'"'"~
.s::.
01
::J
{2 1.0
Ko
2! ~
::J
iJIV
It
-
- --- ----
0.5

-x
Fig. II. Fracture toughness as a function of the composition of PZT near MPB.

As discussed in the Introduction, microcracking and twinning (domain switching)

have been identified as dominant toughening mechanisms in PZT ceramics near MPB [4,5,
10,11]. Relative contribution of each process to the toughness should vary as the
composition or microstructure changes. However, their contributions to the crack-tip stress
relaxation are additive, and then

(7)

where KM represent the toughness due to microcracking and KD due to domain switching.
Combining Eqs.(6) and (7), we get

In order to interpret the R-curves shown in Fig. 10, it is necessary to separate each term in
Eq.(8) for a given composition. An approach we have taken is to measure the fracture
toughness of each sample electrically polarized in the direction perpendicular to the crack
plane. By orienting 90 o -domains in the direction of tensile axis in front of crack-tip
electrically beforehand, it is possible to eliminate a feasible contribution of domain
switching[5,19]. Fig.ll compares the toughness values determined by an indentation
technique for poled and unpoled samples as a function of the composition. The toughness
decreases monotonically as the composition approaches MPB from T-phase field. It
reaches a minimum at the MPB, and remains constant as R-phase increases. The difference
between the two represents the asymtotic value of toughness due to domain switching, K~.
Moreover, when x =0.57 and 0.60 ( fully R-phases), the remaining portion, a contribution
by microcracking (K:), is also negligible. The reason is that a much smaller residual stress
is produced by a rhombohedral distortion in comparison to that by a tetragonal distortions
in PZT ceramics (see Fig.8). Hence, it is concluded that (1) the toughness measured from
the poled R-phase PZT can be adopted tentatively as the value of K o (-0.6), and (2) KD(P)
is essentially independent to x near MPB.

381
 O r-"--------------..,
1•.

0.8f- /
/

/
/

I
P PZT51
I

0.6f- /
/
/
/
/
/
/
/
0.41- I
I
I
I
/
/
P7T54 /
o.f-
I
I
o
PZT55 /
I

O,l-_-Q.J_
",'; _---I_
I _---L_
I _--L._
I _--I

o 10 20 30 40 50
['P,<i -1)C*'12] (m'l2)
Fig. 12. Toughness due to Microcracking plotted as a function of the parameter defined in
eq.(9). B is estimated from the slope of the line.

Microcracking contribution to the toughness now can be determined by substracting

Ko and K o from Kc ' Fig.ll shows that it increases gradually from MPB as the amount of
T-phase increases. Hutchinson[20l analyzed the microcracking in brittle materials and
showed that K~ - Ea...Jh where E is the modulus, a is the misfit strain caused by micro-
cracks, and h is the microcracking zone size under a steady-state crack growth condition.
Supposing that h is scaling with c*, we obtain

(9)

where B is a proportionality constant, and <t>t is the fraction of T-phase. Using the data in
Fig.?, Fig.8, and Table II, K: is plotted in Fig.12 for x = 0.55, 0.54 and 0.51. More data are
needed to test the validity of Eq.(9) properly. However, the linearity between K: and
[<t>t(c/a - l)...Jc*l is quite good. From the slope of the line shown in Fig.12, the approximate
value of B is estimated to be 400 MPa.

The implication of our analysis on R-curve characteristics of PZT ceramics near

MPB is summarized schematically in Fig. 13. The R-curve of Ko rises faster than that of KM
in a small-crack region. It implies that, in the limit of small crack where the crack extension
behaviors of natural flaws can be assimilated, the twinning in the crack front is a dominant
mechanism for the resistance to crack extension. Whereas, the microcracking will playa
increasingly important role as the crack grows. However, its contribution to fracture
toughness is significant only in T-phase field.

The effects of microstructural characteristics on the fracture toughness of PZT

ceramics can be re-assessed based on our analysis. For instance, the change in grain size
would affect each term differently. Firstly, Ko should not be influenced by the grain size as
long as the change in grain size does not induce the change in the mode of fracture from
intergranular to transgranular, or vice versa. Secondly, Ko would not be sensitive to the

382
 c~
I /

c~ -~:-f' -------:;:-.;;;.-...-~----:=:.:...:..=~:::=:.:..:.::..~-
1/ MICROCRACKING

____ J~' ;__ 7~-:~::;....._-.- __-+__--::D~0MA::::::;~ING~..".-_ _

/

/' / SWITCHING
;
/ "/ K..
I I K
//./.01 0

INTRINSIC

o
- Crack Extension

Fig. 13. Shematics of R-Curves of toughening processes found in PZT ceramic near MPH.

Fig. 14. SEM micrographs for fracture surface showing domain structures of tetragonal
PZT ceramics of (A) PZT50, and (B) PZT54. Intergranular microcracking is also
evident.

383
grain size either. The dilatational strain caused by 90°-domain switching is proportional to
the size of twins, which is believed to be essentially constant above a critical grain size, for
instance, about 10 11m in BaTi03[21]. Fig.l4 shows the domain structures of some of our
samples. The average width of the 90°-domains (twins) is approximately in the order of 1
11m. No attempt was made to quantify d vs the average twin size. However, it is expected
that the average twin size is invariant as long as d is larger than 111m. Finally, K M will
certainly be the term that should be affected by the change in grain size. The increase in K c
by increasing grain size has been observed in BaTi0 3[1O]. According to Eq.(9), it is
consistent with our model. The size and population of microcracks should influence c*, the
critical crack size which is related to the microcracking zone size.

Our results shown in Fig.ll is inconsistent with those 'by Freiman et al. [4,10]
shown in Fig.3, particularly in the R-phase rich region. They reported that the toughness
increased again from the minimum at MPH as the composition shifted toward R-phase
field. A stress induced phase transformation from R- to T-phase was suggested as a
possible cause of the increase. We could not observe such an increase in R-phase field. The
discrepancy might be originated from the difference in the nominal compositons employed
in the experiment. Further study is necessary to clarify it. A quantitative XRD study used in
this study on fracture planes of the specimens rich in R-phases may help resolving the
issue.

CONCLUSIONS

We performed indentation-fracture testing for 6 mol% SrO-doped PZT ceramics,

Pbo.94Sro.o6(ZrxTil.x)03' in order to investigate R-curve behaviors as a function of x near
morphotropic phase boundary (MPH). Important findings from this investigation are as
following;

(1) The MPB where both rhombohedral and tetragonal phases co-exist was in the range x
= 0.51 - 0.57, and the. exact MPB where they exist in equal fractions was at x = 0.554.

(2) Strong R-curve hehaviors were observed with different critical indentation loads (or
crack lengths) depending on x. It suggests that the toughening mechanisms vary as x
changes.

(3) The analysis of the R-curves supplemented with indentation toughness results of
electrically polarized specimens showed that 90°-domain switching (twinning) is primarily
responsible for the R-curve behavior in the region rich in R-phase, but insensitive to the
composition of PZT.

(4) On the other hand, both microcracking and twinning were causing R-CUlve behaviors
in the region rich in T-phase. In particular, the toughness due to microcracking is strongly
dependent on the composition near MPH.

(5) The asymtotic values of toughness at the higher end of indentation load (or crack
length) were minimum at MPH as previously reported. However, contrary to the previous
results [4], they remained at the minimum as the composition moves toward R-phase field.

ACKNOWLEDGEMENTS

The authors thank to Korean Ministry of Commerce and Industry for finacial
assistance, and to G.M. Choi and S.T. Jun for helpful discussions throughout the study.

REFERENCES

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384
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Soc., 64[9]:539-43 (1981).
17. R.F. Krause, Rising Fracture Toughness from the Bending Strength of Indented
Alumina Beams, J. Am. Ceram. Soc., 71[5]:338-43 (1988).
18. J. Homeny and W.L. Vaughn, R-Curve Behavior in a Silicon Carbide Whisker/
Alumina Matrix Composite, J. Am. Ceram. Soc., 73[7]:2060-62 (1990).
19. G.G. Pisarenko, V.M. Chushko and S.P. Kovalev, Anisotropy of Fracture Toughness
of Piezoelectric Ceramics, 1. Am. Ceram. Soc., 68[5]:259-65 (1985).
20. J.W. Hutchinson, Crack Tip Shielding by Micro-Cracking in Brittle Solids, Acta
Metall., 35[7]: 1605-19 (1987).
21. G. Arlt and P. Sasko, Domain Configuration and Equilibrium Size of Domains in
BaTi03 Ceramics, J. Appl. Phys., 51[9]:4956-60 (1980).

385
CRACK-RESISTANCE CURVE AND CYCLIC FATIGUE

IN CERAMIC MATERIALS

Yiu-Wing Mai, Xiaozhi Hu, Kai Duan and Brian Cotterell

Centre for Advanced Materials Technology

University of Sydney
NSW 2006
Australia

INTRODUCTION

Despite their very high strength and high stiffness ceramics are usually quite
brittle and suffer from a lack of fracture toughness. In recent years there have been
considerable efforts to toughen these materials by promoting failure mechanisms that
would shield the crack tip from the applied stress intensity factor. Such mechanisms
include phase transformation, microcracking, localised grain brid~ng and fibre
bridging which normally give rise to long range crack-resistance (R) curves; other
mechanisms such as crack deflection, bowing and pinning only result in short range
R-eurves. Reviews on this subject have been given by Mai (1988; 1991) recently.
Also, the relationship between strength and toughness or R-eurve has been studied by
Mai and Lawn (1986), particularly in the range of short crack lengths.

Theoretical studies on the mechanics modelling of R-eurves in these ceramic

materials have provided some important clues to control the microstructures, such as
grain size, grain boundary interphase, residual stresses and heat treatment, etc., in
order to enhance the fracture toughness. Unfortunately, it is recently realised that the
same toughening mechanisms that impart a crack-resistance curve characteristic in a
ceramic material are also responsible for its weakness to resist accumulative damage
due to cyclic fatigue. The more pronounced the R-eurve the more severe is the
strength degradation. This observation applies to both phase-transformable and
non-phase transformable ceramics as well as ceramic matrix composites. However, the
connections between the R-eurve and cyclic fatigue are not clearly established yet;
though the failure mechanisms for coarse-grained aluminas have now been identified as
mainly due to the frictional degradation of the grain-bridges at the crack wake due to
repeated abrasions.

The present paper reviews the toughening mechanisms that are responsible for
the crack-resistance curves in a range of phase-transformable (e.g. zirconia containing
materials) and non-phase transformable ceramics (e.g. silicon nitrides and aluminas).
Sensitivity to cyclic fatigue is discussed with reference to the degradation of these
toughening mechanisms and particular attention is drawn to the differences between
short and long cracks as well as plain specimens containing distributed inherent
defects. A new theoretical analysis is also presented to determine the crack-bridging
stress when subjected to repeated loading in non-phase transformable ceramic
materials for which the main toughening mechanism is grain-bridging at the crack
wake.

Fracture Mechanics o/Ceramics. Vol. 9

Edited by R.C. Bradt et aI., Plenum Press, New York, 1992 387
CRACK SHIELDING, DEGRADATION AND
ENVIRONMENT-ASSISTED SLOW CRACK GROWTH
The concept of crack shielding to explain R-eurve characteristics in ceramics is
now well accepted. Crack growth occurs when the crack tip stress intensity factor K
t
is equal to the material fracture toughness K ' In truly brittle materials K is
o t
identical to the applied stress intensity factor K . But if there are such toughening
a
mechanisms as microcracking, grain-bridging or phase transformation, etc. that occur
near the crack tip or at its wake region, a negative shielding term -K will offset the
r
applied K so that at equilibrium crack growth
a
(1)

Since K is conventionally equated to the crack-resistance curve parameter K and

a R
since K is a function of crack length (a) the R-eurve is represented by
r

(2)

The evaluation of K is dependent on the precise toughening mechanisms that take

r
place. If these mechanisms extend over large crack lengths the R-eurve is both
specimen geometry and size dependent. Analytical methods to predict such effects on
R-eurves have been given by Cotterell and Mai (1988) and Steinbrech et al. (1990).

Non-equilibrium slow crack growth can occur in ceramic materials due to their
susceptibility to corrosion caused by moisture in the air and other aqueous solutions.
In general this behaviour is best described by the following power law equation (Atkins
and Mai, 1985)

da/dt = AK~ (3)

where A and n are numerical constants. Strength degradations due to static and
dynamic fatigue can be determined using Eqn. (3) by integrating from an initial crack
length a to a critical length a which is controlled by the condition K = K ' It is
o c t o
noted, however, that K = (K - K ) during this slow crack growth period.
t a r
Procedures for estimations of the time-dependent strength behaviour of zirconia-based
ceramics under static loading have been given by Duan et al. (1991a).
In cyclic fatigue the experimental crack growth rate measured is the sum of the
slow crack growth component inte~rated over the period (T) of the cycle and a true
mechanical fatigue component (da/dN)m normally measured in an inert environment,
i.e.

T
(da/dN)exp = ~ AK~ dt + (da/dN)m (4)

It is often assumed that (da/dN)m is negligible and that cyclic fatigue crack growth is
only a manifestation of the slow crack growth component (Evans and Fuller, 1974;
Evans, 1980). If there are any differences between the experimental and the integrated
crack growth rates this implies that a mechanical fatigue effect exists, i.e. (da/dN)m is

388
not equal to zero. The physical reason for the mechanical fatigue effect can be
interpreted in terms of the degradation of the shielding term during cyclic loading.
This causes K to increase compared to the case when the shielding effect is in full
t
operation. Consequently, the predicted crack growth rate becomes higher and the
lifetime to failure correspondingly shorter. The sensitivity to cyclic fatigue may also
be accentuated if the material toughness K in cyclic loading is less than that in
o
monotonic loading.

CRACK-TOUGHNESS CURVE AND CYCLIC FATIGUE CRACK GROWTH

Phase-Transformable Zirconia-Bearing Ceramics

Zirconia bearing ceramics have much higher fracture toughness values than
traditional ceramics because of toughening processes associated with the
microstructural change induced by the martensitic transformation of tetragonal Zr02
particles to monoclinic with an irreversible dilatant strain (Garvie et al., 1975; Porter
and Heuer, 1977; Porter et al., 1979; Evans and Heuer, 1980; Evans and Cannon, 1986;
Claussen, 1976; Claussen et al., 1977) leading to a pronounced R-eurve effect (Swain
and Hannink, 1984; Swain, 1983, 1986b). In connection with the R-eurve behaviour
these ceramic materials also exhibit a nonlinear stress-strain relationship which is a
precursor to sensitivity to cyclic fatigue (Swain, 1985; Kendall et al., 1986, 1987).
Consequently, there has been much recent interest in the crack growth behaviour of
zirconia bearing ceramics under cyclic stress.

Based on their microstructures, zirconia bearing ceramics are grouped into three
classes: (1) partially stabilized zirconia (PSZ) based ceramics; (2) ceramics containing
dispersed zirconia particles; and (3) complex zirconia systems (Claussen, 1984). We
review here the experimental results on fracture resistance and cyclic fatigue crack
growth of several class 1 ceramic materials including M8.-PSZ, Y-TZP and Ce-TZP.
This is followed by the zirconia toughened alumina (ZTA) of class 2.

PSZ is a two-phase zirconia ceramic stabilised by solutes, such as CaO, Ce02,

MgO and Y20 3, etc., whose microstructure and properties are affected significantly by
the crystal structure, morphology and distribution of the low solute content phase
dependent on the sub-solidus post-sintering heat treatment (Porter and Heuer, 1977,
1979; Porter et al., 1979; Hannink and Swain, 1982). This microstructural change due
to post-sintering heat treatment can induce different toughening processes giving
different R-eurve characteristics.
The transformation toughening mechanism in PSZ is often modelled by the
interaction between a main crack and the fracture process zone with dilatant strain,
OT. The shielding effect is obtained from Hutchinson's (1974) equation and the net
stress intensity factor K , which drives the crack, can be written as (McMeeking and
t
Evans, 1982; Budiansky et al., 1983)

K
t
=K +
a
EO
T
3.p1r(1 _ v)
f Jr r-3/ 2 cos ~~ ¢dA (5)
A

where the second term on the right-hand side represents the shielding term -K for
r
which the integral is taken over the transformed region A, which is determined by the
transformation condition. Because of the irreversibility of the transformation zone and
wake toughening behaviour of the dilatant strain, the shielding term increases with
increasing crack length. That is the fracture resistance (R) increases with crack
growth.

389
 Much experim~ntal work has already been performed on the tou~hening
mechanisms and R-eurve characteristics of PSZ ceramics such as Mg-PSZ (Swain,
1983, 1986b; Swain and Hannink, 1984; Swain and Rose, 1986; Marshall and Swain,
1988; Readey et al., 1987; Heuer et al., 1988), Y-TZP (Lai et al., 1989; Liu and Chen,
1990; Grathwohl and Liu, 1991) and Ce-TZP (Rose and Swain, 1988; Yu and Shetty,
1989, 1990; Tsai et al., 1990). Typical R-eurves of Mg-PSZ with two different heat
treatments are shown in Fig. 1. As shown by Swain and Hannink (1984) the
toughening mechanism associated with the R-eurves of a peak-toughness Mg-PSZ is
transformation toughening; but for the sub-eutectoid aged material of the same
Mg-PSZ this is due to microcracking. Also, combined transformation toughening and
microcracking mechanisms can be found (Rose and Swain, 1988) in some PSZ systems.
In the case of long cracks in specimens such as the double-cantilever-beams, crack
brid~ng also contributes to the crack-resistance curve (Swain, 1986b; Readey et al.,
1987). However, R-eurves for "natural" surface cracks are significantly different to
those of large cracks due to residual stresses (Marshall and Swain, 1988). Therefore,
there is no unique toughening mechanism for the R-eurves of PSZ ceramics. But the
single most important parameter is post-sintering heat treatment, and it is possible to
maximise toughness by optimisation of the heat treatment process.

It is now well recognised that Mg-PSZ does suffer mechanical fatigue when
subjected to cyclic stresses (Dauskardt et al., 1987, 1989, 1990a, 1990b; Sylva and
Suresh, 1989; Davidson et al., 1991). Other PSZ ceramics, such as Y-TZP and
Ce-TZP (Liu and Chen, 1989, 1990; Cardona and Beevers, 1990; Tsai et al., 1990;
Grathwohl and Liu, 1991a, 1991b) have also been shown recently to be sensitive to
cyclic fatigue. Systematic studies on cyclic crack growth in a range of Mg-PSZ
ceramics from the overaged to TS-grade have been conducted by Dauskardt et al.
(1987, 1989, 1990a, 1990b) in the compact tension geometry containing long cracks.
The experimental da/dt-~K data measured verify the existence of a true mechanical
fatigue effect in these ceramics under cyclic loading (see Fig. 2). Fractographic
analyses on crack closure and transformation zone size show that similar crack
toughening mechanisms are obtained for both monotonic and cyclic loading. It is
proposed that cyclic fatigue crack growth in Mg-PSZ ceramics is a mechanical
degradation process which may be accelerated by environmental effects. Although the
true fatigue mechanisms are not clear, recent work by Davidson et al. (1991) have
observed that the formation of slip bands prior to crack extension may be the precursor
to a true mechanical fatigue in Mg-PSZ ceramics. Cyclic fatigue crack growth in
3Y-TZP has been explained in terms of microcracking and related to damage
accumulation represented by the hysteresis loop in the applied stress-plastic strain
curve (Liu and Chen, 1989, 1990). It is suggested that the microcracking mechanism
causes plastic strain accumulation and reduces the elastic stiffness and that crack
growth rates are strongly dependent on the maximum stress O'max or maximum stress
intensity factor K . In Ce-TZP ceramics containing large cracks Tsai et al. (1990)
max
have suggested that enhanced fatigue crack growth is not due to reduced crack
shielding associated with the transformation zone. Rather, this is caused by a shorter
crack bridging zone and/or wedging by grain debris on the fracture surface as observed
in these materials. They have also shown that cyclic fatigue crack growth rates are
controlled by the crack resistance curve for any given stress intensity factor range ilK.
It is possible to increase the fatigue threshold by decreasing the transformation yield
stress or by preforming a crack-tip transformation zone by prior quasi-static loading.
Cyclic fatigue results of M~-PSZ containing surface indentation cracks have
been obtained by Lentz et al. (1990) at a frequency of 220 Hz and a stress ratio of 0.1.
When compared to the static fatigue data there is a slight but definite mechanical
fatigue effect. With unnotched plain specimens, however, it is shown that under
rotation bending the lifetimes to failure are much smaller than under static loading
(Swain, 1986c; Swain et al., 1991; Swain and Zelizko, 1988). This has led to the
conclusion that when tension-eompression cycles are involved the mechanical fatigue
effect is much enhanced. Whilst this is true it is necessary to assess the role of fracture

390
 14 c
c
c

12
~d
Q.

1: 10
++ +
+ + +
8

6
o 2 3 4
/:"0 (mmJ

Fig. 1. Effects of post-sintering sub-eutectoid heat treatment

on R-eurves of a Mg-PSZ ceramic in the DCB geometry.
o 8h/llOO • C; + 2h/llOO· C.

-2
"
-4 "
v
L>i!. ~
~ -6 0
A
.6
Q

-
Q
~o A " Q

0 A
::l2
ru -8
00
00 '" " Q

l' A'"
"0 v

0
CTI

-10 °0
0 i 1
-l
"
A

'"
-121 3 4 5 6 7 8
Kmox IMPavm)

Fig. 2. Log-log plot of da/dt against Kmax for a TS-grade Mg-PSZ

in a compact tension geometry. Sustained loading: v (air),
fJ. (water); cyclic loading: 0 (R = 0.1, air).

391
 300 r - - - - - - - - - - - - - - - - - - - - - - . . . ,
Tension
~
250
<?
0-
~200
(/)
(/)

~ 150
Ci5
C
~ 100
(\l
a.
a.
-< t t
50 I I
• •
200 400 600 800 1000 1200 1400
].J Strain
Fig. 3. Bending stress-strain curves in tension and in compression
for a ZTA ceramic.

8,....---------------------------,

0 0
0 0
0
0 6- 6
6* 6 6 6
*
~ 6 * 6
0
* 0 0
6 0* 'b 0 0 0 0
*
*
*
0

* DCB3
o DCB4
o DCB5
6 DCB6

2 4 6 8 10 12 14
Crack Increment,m(mm)
Fig. 4. Crack-resistance curves for a ZTA in the· double-eantilever-
beam (DCB) geometry.

392
statistics in plain specimens before a definite conclusion can be drawn. For example,
based on the statistical theory of time-dependent fracture by Hu et al. (1988, 1989),
the same lifetime data of Mg-PSZ obtained by Swain et al. (1991) can be predicted
quite accurately by the fracture data under dynamic loading (Duan et al., 1988).
However, it is questionable to assume zero crack growth in the compression half of the
cycle in the analysis because the crack shielding mechanisms may be degraded in
compression thus leading to enhanced crack growth in the tension half of the cycle.
However, this is not expected to be significant for small natural flaws. We return to
this point later in the paper about cyclic fatigue in unnotched plain specimens.

Zirconia-Toughened Alumina

Zirconia-toughened aluminas (ZTA) are made from an alumina matrix and

dispersed zirconia precipitates. Sometimes additives such as Y203' etc. are included.
The mechanical properties of these ceramics can be significantly improved by the
transformation of tetragonal Zr0 precipitates to monoclinic and other related
2
toughening mechanisms such as microcracking (Evans and Cannon, 1986; Wang and
Stevens, 1989). This improvement, however, is dependent on the microstructure,
Al 0 /Zr0 ratio and the stability of Zr0 (Lange, 1982; Becher and Tennery, 1983).
2 3 2 2
Transformation toughening from metastable tetragonal Zr0 to monoclinic can
2
increase both the fracture toughness and the tensile strength (Becher, 1981; Claussen,
1984); but microcracking only increases the toughness with a decreased strength
(Claussen, 1976; Claussen et al., 1977). Toughening from combined phase
transformation and microcracking has also been reported for ZTA (Kosmac et al.,
1985; Wang and Stevens, 1988).

Compared to the PSZ ceramics, relatively little work has been conducted on the
crack-resistance and cyclic fatigue behaviour of ZTA. The crack-resistance curve of a
sintered A1 0 /Zr0 composite made of an alumina matrix and dispersed monoclinic
2 3 2
Zr0 polycrystals has been measured by Garvie and Goss (1986) and explained by the
2
crack-bridging effect (Swain, 1986b). A systematic study. on the mechanical properties
of this particular A1 20 /Zr0 2 material containing 8 wt % zirconia has been conducted
3
by Duan et al. (1990a, 1990b, 1991c) which covers the stress-strain curve and the
R-eurve behaviours of large and indentation cracks as well as strength measurements
subjected to dynamic, static and cyclic loading. Figure 3 shows the tension and
compression stress-strain curves obtained in four-point bending. Apparently, both
curves show non-linearities though this effect is more obvious in tension than in
compression. It is suggested that the non-linearities are almost exclusively associated
with flaw growth and that microcracking is predominant in the tension surface of the
specimen giving rise to the offset/irreversible strain after completely unloading. Figure
4 shows the crack-resistance curve measured from a double-eantilever-beam with a
large crack. Although the precise toughening mechanisms have not been identified in
this material it is shown that crack branching (leading to crack bridging) and
microcracking in the frontal process zone (Fig. 5) may be important. Cyclic fatigue
crack growth data have been obtained from four-point bending of notched beams, Fig.
6. These results show that the crack growth rate depends strongly on the maximum
stress intensity factor K and the stress ratio for a given ilK. The effect of the
max
R-eurve on crack growth is reflected by the initial negative slope of the log da/dN
versus log ilK curve (see Fig. 14 later). In common with the observations of Sylva and
Suresh (1989) on Mg-PSZ, fatigue crack growth in this ZTA ceramic is discontinuous
and periodic crack arrest occurs after a small crack extension.

The lifetimes of plain specimens containing natural flaws under both static and
cyclic loadings have also been studied, Figs. 7 and 8. Using the Wei bull parameters
and dynamic fatigue data (Fig. 9) together with the statistical fracture theory

393
W
<D
~

Fig. 5. Photomicrograph of crack branching and microcracking processes

at the crack tip region in a ZTA ceramic.
 1E·06 r---------------------~

U
>.
~1E.07

z
u
Co 1 E·08
u
Q)

iU
a:
..c: 1E-09
3
e
CJ
-D 1E-1 0
~
()

1E-11 L . . - - - -_ _....L..- ..L- ..L-_ _---L_ _..J

3 4 5 6 7 s
Maximum Stress Intensity Factor, K"...(MPa Jm)

Fig. 6. Log-log plot of cyclic fatigue crack growth rate (da/dN)

against K for a ZTA ceramic in a notched bend geometry
max
containing large cracks. There is an approximate linear
relationship between da/dN and K max for the rising portion
of the data for all stress ratios. [R = 0.1 (*), 0.3 (0),
0.5 (6), 0.9 (0); frequency = 20 Hz.]

190
170

ro
a. 110
:2

70

2 3 4 5 6 7
Log Failure Time (s)

Fig. 7. Static fatigue data for a ZTA ceramic in unnotched plain

specimens. 0 represent unbroken data and - - are predicted
lines for different failure probabilities Pf

395
 190

---_-_----
170

<il
150
... ... ...
...
... ............
~130 ... ...
~ 110
(J)
'-
U5
E 90
::>
E
'x
Cil
:2 70

234 5 6
Log Failure Time (s)

Fig. 8. Cyclic fati~ue data for a ZTA ceramic in unnotched plain

specimens tR = -1.0 and frequency = 180 Hz). Experimental
data (~) are compared with theoretical lines for different P f

250

200 0
P, = 90%
0 t <90
(9
150 l 0
co
n-
0
co
P,= 50%
2
£
t
P,=10%
0>
c 100
~
Ci5

50 "--_-'--_ _-'--_--'-_--''--_ _.L..-_....I..-_---I..._ _- - ' - _ - - - - '

1 2 5 10 20 50 100 200 500 1000
Stress Rate (MPa/s)

Fig. 9. Dynamic fatigue data for a ZTA ceramic in unnotched plain

specimens. Theoretical lines for different P f are also shown.

396
developed by Hu et al. (1988, 1989) the static and cyclic results can be predicted and
compared to the experimental data. There appears to be a slight but definite
mechanical fatigue effect in small cracks. However, the experimental results by Guiu
et al. (1991a, 1991b) on an alumina containing 20 vol % Zr0 2 and 3 mol % Y203 show
a more significant mechanical fatigue effect in specimens with natural flaws.

Non-Phase Transformable Ceramics

Unlike zirconia ceramics, non-phase transformable ceramics, such as sintered

silicon nitrides and aluminas, do not have a significant crack tip fracture process zone.
Crack-tip shielding mainly comes from grain bridging at the crack wake. The
R-eurve owing to crack shielding can be readily modelled with the K--5uperposition
method (Foote, et al., 1986; Mai, 1988) under monotonic loading using Eqn. (2), Le.

(6)

where K is replaced by K (O"b) which is the shielding component due to the

r b
crack-interface bridging stress O"b. KR-eurves have been measured for a number of
coarse-grained alumina ceramics by Knehans and Steinbrech (1982), Swain (1986),
Swanson et al. (1987), Steinbrech et al. (1990) and Lathabai et al. (1991). The effects
of specimen geometry and notch depth on R-<:urves of aluminas have also been studied
and analysed (Steinbrech et al., 1990; Mai and Lawn, 1987; Mai, 1990, 1991).

In general, the existence of a R-<:urve in mon9tonic loading implies there is a

strong sensitivity to fatigue crack growth in cyclic loading. Cyclic fatigue crack
growth which cannot be explained in terms of the environment-assisted slow crack
growth mechanism alone has recently been observed (Reece, Guiu and Sammur, 1989;
Lathabai, Rodel and Lawn, 1991; Guiu, Reece and Vaughan, 1991). Unfortunately,
KR-eurves obtained in monotonic loading cannot be directly applied to cyclic fatigue
crack growth as it is II sub-<:ritical ll in contrast to the lI equilibrium ll crack growth in
monotonic loading. To explain cyclic fatigue crack growth it is necessary to determine
the mechanism for crack shielding degradation. As shown b~ Lathabai, Mai and Lawn
(1989), Hu and Mai (1991a,b), Lathabai, Rodel and Lawn 1991), crack-tip shielding
can be weakened by the frictional degradation of the grain ridges in the crack wake.
This argument is similar to that put forward by Tsai et al. (1990) for the Ce-TZP
ceramics in which crack bridging is observed. lio et al. (1991) have also shown that in
sintered silicon nitride the crack bridges developed in monotonic loading are fractured
during cyclic loading. This leads to a reduction in crack tip shielding so that the
material becomes sensitive to cyclic fatigue. Figures 10 and 11 show the cyclic fatigue
data for a coarse-grained alumina with large and indentation cracks, respectively.
Again these results show that in indentation cracks subjected to tension-tension
fatigue the mechanical effect is small but definite. In large cracks involving
tension-eompression fatigue the cyclic fatigue effect is much more prominent.

MECHANISMS OF MECHANICAL FATIGUE

AND MECHANICS MODELLING

Phase-Transformable Zirconia Bearing Ceramics

Cyclic fatigue crack growth rates can be described by Eqn. (4). If it can be assumed
that the mechanical fatigue component is negligible then the crack growth rate under
cyclic loading is given by

(7)

397
 u
~-5
1z -7 , ,
I

, I
"0
:g -8 ,
I
<.:)
, I

S -9 I

2 3 {, 5
Kmox (MPoIlTl)

Fig. 10. Cyclic fatigue crack growth in an alumina

(18 pm grain size). - - DCB geometry,
R = -(J.8 and frequency = 5 and 10 Hz;
- - - - static fatigue.

-
( \l
(l.
:2
250 .----r--.-----.-----.----.----r-~-_____,

...
I>
100 Hz
1 Hz
"-" 200
)(

'"
:E
t:>

.S:!
C3
>-
U 50
~
(\l
Q)
(l. OL-_.l...-_.l...-_.l...-_-L-_...L-_...L...:_-l-_--'
1 1 3 5 7
10. 10 10 10 10
Time to Failure, (5)

Fig. 11. Cyclic fatigue data for an alumina (35 pm

grain size) with surface indentation cracks.
Solid line is for static fatigue data.

3ge
 lE-05 , - - - - - - - - - - - - - - - - - - - - - - - - - ,

olE·06 As-Fired MS l',. - TS

:-/
>- l',.
u
E If

-•-
---,E·07 l',.

y
Z
~
l',.
l',.
"OlE-08 l',.
oJ
en l',.
l',.
~1E.09 '1
j 0 l',.
e 0

.
l',.
<.?lE-lO 0 Cb l',.
.:t:
u
C1l
OlE-ll
K~=1.8 MPa Jiff Predictions
lE-121-L..-----~2---3l....----5l....-----1....1.0--------l20

Stress Intensity Range, l'K (MPa .In)

Fig. 12. Cyclic fatigue crack growth rates for a range of Mg-PSZ ceramics
in the DCB geometry with different levels of phase transformation
toughening. Using the overaged data as a reference predictions are
given for the AF, MS and TS materials based on the slow crack growth
component only. Mechanical fatigue effect is more significant for the
tougher MS and TS ceramics.

K.....='2.3

u
>-
~
E
z
~
~1E-07 0 0 --------0
ro 0-
a: c
.s=
1:1E-11
e
<.?

e1E-15
.x

()

1E-19 L . . - - - - - - ' - ---' --L -----l

o 2 4 6 8
Crack Extension, La ( mm )

Fig. 13. Transient crack growth in the TS grade Mg-PSZ ceramic showing
crack growth following a load reduction and a single overload.
- - 0 - - 0 - - experimental data and - - theoretical predictions
based on the slow crack growth component alone.

399
In ceramics with phase transformation toughening the crack tip stress intensity factor
K must be replaced by the sum of the applied and shielding terms, K and K , Le.
t a r
Eqn. (5). When the cyclic fatigue data of Mg-PSZ are analysed in this way (Duan et
al., 1991a, 1991b) it is shown that the mechanical fatigue effect becomes stronger with
increasing toughness due to different heat treatment (Fig. 12). Crack growth rates due
to abruptly applied overloads durin~ cyclic fatigue can also be qualitatively explained
in terms of the R-eurve and Eqn. (7) even though the mechanical fatigue component is
again neglected (Fig. 13).

Theoretical modelling of cyclic fatigue crack growth in transformation

toughened ceramics is hampered by the fact that the mechanical fatigue mechanisms
are not yet clear. However, some empirical formulae have been introduced to predict
cyclic fatigue crack growth rates with varying degree of success. For example a power
law equation has been used by Dauskardt et al. (1987, 1990b)

da n
<IN = Ac . ~Kt
A
(8)

to describe cyclic fatigue in PSZ ceramics. Replacing the crack tip t:.K t by
(Ko/KC)K max or [Ko/(l - R)](t:.K/K C) a universal curve is obtained which is given
by

Kn n K n
da _ A.
<IN - C (1 _ R)n
0 . [t:.K] _ A [ 0] K n
KG - C KC max . (9)

Here R is the stress ratio and K is the saturation toughness on the R-eurve. Note
C
that Eqn. (9) describes the rising portion of the ZTA data in Fig. 6 fairly well and it
also predicts the R-ratio effect on da/dN as shown Fig. 14. Similarly, Liu and Chen
(1989, 1990) propose the following empirical equation:

(10)

Non-Phase Transformable Ceramics and

Frictional Degradation of Grain-Bridging
Analogous to a crack in a non-phase transformable ceramic under monotonic
loading, a long crack in cyclic loading is shielded by grain bridges in the crack wake.
Such a shielding effect normally increases the fatigue crack growth resistance. Indeed
this provides an explanation why in the early stage of fatigue crack growth da/dN
decreases with increasing t:.K. However, as pointed out by Lathabai, Mai and Lawn
(1989), frictional damage in grain bridges owing to cyclic loading eventually takes
place and this leads to enhanced crack growth as the crack-tip shieldin~ is reduced.
This has been frequently referred to as an extrinsic fatigue mechanism l e.g. Ritchie,
Dauskardt and Cox, 1991). Hence, the determination of frictional degradation in grain
bridges is needed to understand the mechanical fatigue in non-phase transformable
ceramics and to explain the essential difference between R-eurves measured in
monotonic and cyclic loading situations. This topic has been studied in earnest by
several investigators, e.g. Lathabai} Mai and Lawn (1989), Guiu, Reece and Vaughan
(1991), Lathabai, Rodel and Lawn t1991), and Hu and Mai (1991b). A simple method
has been proposed by Hu and Mai (1991b) to evaluate the grain-bridge degradation
from which the crack-tip shielding under cyclic loading can be determined.

400
Bridging-Stress Evaluation under Monotonic Loading

A fully develoyed bridging zone X is shown in Fig. 15. The area under the
(Tb-w curve, Fig. 15la), is defined as the specific fracture energy G The bridging
f
stress (Tb decreases from its maximum value (Tm at the crack tip a to zero at the
critical crack opening wc' Fig. 15(b). The magnitude of the bridging stress (Tb(x) at a
position x behind the crack-tip is controlled by the crack face opening w. Such a
description of the (Tb-w relationship is adequate for many quasi-brittle materials such
as aluminas. Hence, a power law (Tb(w) function proposed by Foote, Mai and Cotterell
(1986) is convenient to describe the relationship of (Tb-w, i.e.

(11)

and it follows that the fracture energy G is given by

f

(12)

If (Tm' wc and the exponent n are determined, the KR-<:urve of alumina ceramics can
be predicted with the K-superposition method (Foote, Mai and Cotterell, 1986; Mai,
et al., 1988).

Because of the crack-tip shielding effect of the bridging stresses the compliance
of a specimen with a bridged crack is different to that of a specimen with a
traction-free crack of the same length. Let Cu be the measured unloading compliance
and C{a) the ideal elastic compliance without any crack-tip shielding. It follows that

C(a) > Cu (13)

The above inequality indicates that if C = C(aeff), aeff < a. In other words, the true
u
crack length a is underestimated if the conventional compliance method is used to
measure crack length. This underestimate is entirely due to the crack-interface
bridging. Therefore, the inequality C(a) > Cu provides a measure of the bridging
stress influence. Indeed, a general method for the determination of bridging stresses in
terms of compliance measurements has been recently developed by Hu and Mai
(1991a), which relates the far field compliance C(a) and C to the local bridging stress
u
(Tb adjacent to the crack tip. The relevant analysis is summarised below.

Crack face opening in quasi-brittle materials like ceramics is normally small

because of the relatively high Young modulus and its profile is approximately linear
(e.g. Foote, Mai and Cotterell, 1986; Rodel, Kelly and Lawn, 1991). Hence, it is
reasonable to assume a linear crack profile within the bridging zone X shown in Fig.
15(b). Based on this assumption, it has been proven (Hu and Wittmann, 1989, 1991)
that

401
 1E-06 r - - - - - - , . - - - - - - - - - - - , . - - - , - - , . - - - - ,

u>-
.521 E-O?

Z
E
~
I
-0 1
Ci31 E-08 \
-0
Q)
1
~ rn
~
((
.J:: 1E-09 ,0
~
e ,0
C)
.::t:
,
I

(..) 1E-l 0
~ ~O 0
o 01

lE-11 .
03 0.5 1 2 3 5 10
Stress Intensity Range ~ (MPa Jm)

Fig. 14. R-ratio effect on cyclic fatigue crack growth in a ZTA ceramic
with the notched-bend geometry. R = 0.1 (*),0.3 (0), !J. (0.5)
and ZTA ceramic with the 0.9 (0). - - predictions based on
Eqn. (9) and data in Fig. 6. - - - -lines indicating the
initial negative da/dN versus ~K effect.

~~ .. _---_._- O'm
,,
,
,

r- x
,
,
o
---a

(a) (b)

Fig. 15. Schematics showing (a) the specific fracture work for the crack bridges and
(b) the crack bridging stress distribution in a non-phase transformable ceramic.

402
 2
I1b (x) C (a) C~(x)
--=---.~ (14)
11m C'(a) Cu(x)

where C'(a) and dC(a)/da and C~(x) = dCu(x)/dx, and that

(15)

These two equations are originally derived for a consecutive sawcutting experiment on
cementitious materials with large bridging zones (Hu and Wittmann, 1989, 1990) and
Cu(x) is the unloading compliance measured after the sawcut has proceeded to the
position x within the bridging zone X. The validity of these equations have also been
confirmed with a finite-el.ement computer simulation experiment (Alvaredo, Hu and
Wittmann, 1989). However, the application of consecutive sawcutting cannot be easily
applied to ceramics with small bridging zones. A method to relate directly the
unloading compliance C without sawcutting to the bridging stress I1 is needed.
u b

Let a be the initial notch length and a crack extension equal to ~a (= a - a )'
o o
Before a bridging zone is fully developed, i.e. ~a < X, there is stress transfer at the
notch tip. Such an unsaturated bridging zone is analogous to a fully developed
bridging zone then partially re-notched. Therefore, the bridging theory developed for
the consecutive sawcutting experiment can also be used to determine the bridging
stress at the initial notch tip a '
o

Hu and Mai (1991a). With Eqns. (11) and P4)

The left-hand side of Eqn. (15) has been defined as a compliance ¢>-function by
they have proven the ¢>-function
determined by C and C(a) is valid even i a bridging zone has not been fully
u
developed, i.e.

(16)
~a<X

Hence, if crack-interface bridging is the predominant toughening mechanism in a

ceramic material ~ is a monotonic increasing function of the crack extension ~a,
starting with zero and reaching its plateau after the bridging zone is fully developed.
Hence, with a kurve obtained under monotonic loading we can determine both the
exponent n for the power law bridging stresses and the length X of a fully saturated
bridging zone.

Measurements of the unloading compliance C and corresponding crack length a

u
are required to experimentally determine ~, from which both X and n can be
evaluated. One example is shown in Fig. 16 for a compact tension specimen of a
coarse-grained alumina with an average grain size of 23 pm (Lathabai, Rodel and

403
Lawn, 1991). The always positive if> in this figure proves that grain-bridging is the
major toughening mechanism for the crack-toughness KR-eurve. The exponent n
determined is about 2.8.

It is worth pointing out that the application of the Hu-Mai bridging theory
(and the associated ¢>-eurve) is not confined to ceramic materials. It has been
successfully used for the analysis of stable crack growth in short fibre-reinforced
cements (Mai and Hakeem, 1984) and mode-I delamination of carbon fibre/epoxy resin
composites (Hu and Mai, 1991c). Recently, a number of coarse-grained aluminas and
zirconia-bearing ceramics have been tested and the results analysed in accordance with
the Hu-Mai bridging theory (Hu, Lutz and Swain, 1991).

Frictional Degradation of Bridges under Cyclic Loading

Under cyclic loading the crack-tip shielding effect from existing bridges is
reduced owing to the accumulative damage of these bridges in repetitive abrasion
(Lathabai, Mai and Lawn, 1989; Reece, Guiu and Sammur, 1989; Lathabai, Rodel and
Lawn, 1991; Hu and Mai, 1991b; Guiu, Reece and Vaughan, 1991). However, for
mechanical equilibrium, new bridges must be established with every fatigue crack
growth increment and the total crack shielding effect is increased. To incorporate this
complex crack-tip shielding effect into a cyclic fatigue crack growth analysis it is
imperative to know independently the frictional degradation process of existing bridges
behind the crack tip. The frictional degradation of grain bridges with crack growth has
been analysed briefly with the ¢>-function (Hu and Mai, 1991a). Fatigue crack growth
plus the degradation process is further studied by Hu and Mai (1991b) using
experimental results obtained for a coarse-grained alumina ceramic. Their analysis
can be extended from the ¢>-eurve approach presented in the previous section.

Separation of the frictional degradation of crack-interface bridges from cyclic

fatigue crack growth is possible in experiments. Initially, a bridging zone (and
preferably a saturated zone) behind a long crack needs to be established in a specimen
with monotonic loading. To study the degradation of these bridges in cyclic fatigue
the applied maximum tensile stress O'max should be controlled to limit any fatigue
crack growth so that no new bridges can be developed. Thus, any reductions in the
unloading compliance is directly related to the frictional damage experienced by the
existing bridges. This damage process is illustrated in Fig. 17. After the fully
saturated bridging zone X is established with monotonic loading, cyclic loading is then
applied. As the maximum cyclic loading O'max is smaller than the critical monotonic
loading under which the crack with the bridging zone X extends, the bridging stress at
the crack tip a is smaller than O'm at an early stage of the cyclic fatigue experiment.
This stress is gradually increased when degradation of the bridges accumulates. When
it reaches O'm the crack grows under cyclic loading to maintain overall mechanical
equilibrium. Obviously, the whole degradation process is dependent on the cyclic
stress range, i.e. (O'max-O'min) and the stress ratio R( = O'min/O'max)' It should be
noted that grain-boundary micro-fracture processes in front of the crack tip, if any,
are not included in the present analysis, i.e. K in cyclic fatigue is the same as in
o
monotonic loading.

Let N indicate the number of fatigue cycles elapsed for a given cyclic stress
system (O'max'O'min)' Under the condition that a is kept constant, only the unloading
compliance Cu in the ¢>-function will be influenced by the frictional degradation.
From Eqns. (15) and (16) it can be shown that

404
 7 2.0

-=---.---.•
6

-• .........• •
1.6
~....

••
5
~
c:l ~. _ 0'- -00-
Q.. 1.2 E
L:: 4
,0 ' E
0
3
~
0::
/ 0 0.8 B-
0
, 0
2 /
/
00
K •
/ 0.4
/ ep 0

,q<:O,
.. 6 0
00
0 0
0 2 3 4 5 6 7 8

!::.a mm
Fig. 16. K and if; curves for an alumina ceramic in the compact tension
R
geometry. (Grain size = 23 Jl.'ID and bridging stress power law exponent
=
n 2.8.)

Fig. 17. Schematic showing the crack-interface bridging stress

distribution before and after cyclic loading. Note that
wc (N) < wc and X (N) < X.

405
 (17)

The frictional degradation reduces the magnitude of the bridging stress O"b(N) , the
critical crack opening wc(N), and hence G~N) the area under the O"b(N) - wc(N) curve
(see Fig. 17). Since only the magnitude of the bridging stress, and not the bridging
mechanism, is changed during the frictional degradation process, it is reasonable to
assume in Eqn. (11) that the exponent n is constant. Thus, both wc(N) and G~N) are
reduced proportionally during cyclic fatigue and the G~N)/wc(N) ratio is constant, i.e.

Gf(N) G f
WJNJ=w ' (18)
c

Equation (17) also shows that the change in the compliance Cu(N) or the
~(N)-function after N fatigue cycles is directly related to the diminution of the
bridging zone X.

If the maximum tensile cyclic stress O"max is smaller than the critical stress to
cause crack growth in a traction-free crack of the same length a, crack extension does
not occur even after all existing bridges are destroyed. Let Nc be the critical number
offatigue cycles elapsed for given O"max and O"min' If N = Nc' X(N) = 0 and Cu(N) =
C(a). Let ~~(N) = ~(a) - ~(N). Thus from Eqns. (16) and (17),

~~(N) = ~(a) - ~(N)

C 2
(a) {1
=C'{aJ" ~-~
1}

(19)
N>N
- c

By comparison of Eqns. (16) and (19), it is clear that ~(a) and ~~(N) are similar
curves with the same plateau value X/(n + 1) when ~a ~ X or N ~ N ' A ~~(N)-
c
curve for a given fatigue system (O"max'O"min) therefore provides vital information on
the bridge degradation process in the non-phase transformable ceramics.

The variation in bridging stresses during cyclic fatigue is another important

aspect as it indicates the change in the crack-tip shielding. The length of the bridging
zone X(N) during cyclic fatigue can be determined from either Eqns. (17) or (19), i.e.

X(N) = (n + 1) . ~(N)

=X-(n+ 1)· ~~(N) (20)

406
 120

~100
/
....
C
.~ / N<6.5Xl0'
a.
E
80
o / . .. . . . &
()
,,60
Q) S
.!:! /N:4.3Xl0
roE 40 .
o
Z 20
/ N:;O

o
0.2 0.3 0,4 0.5 0.6 0.7 0.8
a/W

Fig. 18. Normalised compliance results for a coarse-grained

alumina in the tapered DCB geometry as a function of
normalised crack length. Crack growth is zero for
5
N less than 4.3 * 10 cycles but the compliance
increases thus indicating the degradation of crack
bridges due to repeated loading.

3 N=O H<a.5XtO •
E
E 2

-e-
"
N= 4.3)('0 •
o '---~--~--~---'
o 4 6
c.a mm
Fig. 19. ¢-t::.a curve for the experimental fatigue crack growth-eompliance
results given in Fig. 18. Notice that 4J decreases from 2.96 to 0040 when
t::.a = 0 showing the degradation of the grain-bridges. 4J increases with t::.a
subsequently but at t::.a ~ 4 mm 4J decreases and increases periodically
indicating the nature of discontinuous crack growth and crack arrests.

407
According to the linear crack profile assumption, the critical crack opening wc(N)
during cyclic fatigue is given by:

W
c
wc(N) = r· X(N)

= c . (n * 1) . 4>(N)

*
W

=wc . [1_(n 1l.~4>(N)] (21)

The corresponding bridging stress distribution during cyclic fatigue shown in Fig. 17 is
obtained from Eqn. (11), Le.

(22)

A comparison between Eqns. (11) and (12) for a given stress level indicates
quantitatively how existing bridges are degraded because of repetitive abrasion during
cyclic fatigue so that a suitable lT -w function can be found for the cyclic fatigue
b
analysis.

4>(N) has been evaluated with Eqn. (17) from the compliance results (Fig. 18)
obtained by Guiu, Reece and Vaughan (1991a) for a coarse--grained alumina before
fatigue crack growth and shown in Fig. 19. The reduction in 4> with cyclic fatigue
clearly indicates the frictional degradation in the grain bridges.

Fatigue Crack Growth under Cyclic Loading

In practice fatigue crack growth and the frictional degradation of bridges occur
concurrently during cyclic fatigue. Hence, the crack shielding effect from bridging
stresses under cyclic loading is different to that measured under monotonic loading.
To study the shielding influence upon cyclic fatigue crack growth it is crucial to
measure the bridging stress under cyclic loading. Again, the ¢>--eurve approach can be
extended for this purpose (Hu and Mai, 1991b; Hu, Mai and Lathabai, 1991).

For a given cyclic stress range (ITmax-ITmin) and stress ratio (ITmin/ ITmax) the
¢>-function defined in Eqn. (17) has a steady state value smaller than X/(n + 1)
because of the degradation of bridges. Equation (17) can be rewritten as:

4>(N,~afc) = 8~(l) . {cu(~~Alfc) -I} (23)

Gf(N,~afc) 1
= IT W (N lia ). X(N,~afc) = n+r . X(N,~afc) (24)
m c ' fc

~afc indicates the fatigue crack growth while N denotes the number of fatigue cycles
associated with the bridge degradation. Hence, during cyclic fatigue a
4>(N,~afc)-eurve can be constructed with Eqn. (23) which measures the net crack-tip
shielding due to the new bridges established with fatigue crack growth and the existing
bridges which suffer accumulative frictional degradation.

408
 X/(n·1)

ep monotonic

cyclic

o
Fig. 20. Schematic ¢r-~a curves for monotonic and cyclic loading.

0.8 1 7 - - ' \ ; \ - - - - - - - - - - - - 1

0.6 ~,---\-'I~--,-------____4
O"b

0" m 0.4 1-':-------\~___r'-------____1

0.2 t----'.~---"""'.....>..,;:__----____4

\'. wc(N)/wc
o L-..---:..>.L-_--'-_---J._-=:::~ _ _l

o 0.2 0.4 0.6 0.8

W/Wc
Fig. 21. Crack-interface bridging stress distributions for two coarse-
grained aluminas under both monotonic and cyclic loading. Notice
the dramatic reduction of the bridging stress in cyclic loading.

409
 If fatigue crack growth initiates from a notch the 4>(N,6.afc)-<urve starts from
zero and increases with crack extension until a steady state value is reached for the
given cyclic fatigue system (0'max'O'min)' As shown in Fig. 20 this value is less than
that indicated by Eqn. (16) for monotonic loading because X(N,6.afc) < X. Thus if
Eqn. (16) represents the crack-tip shielding effect under monotonic loading conditions,
Eqn. (24) then specifies the shielding effect under cyclic loading conditions. As such,
the crack tip shielding is hence weaker in cyclic fatigue than in monotonic loading.

The cyclic fatigue results of Guiu, Reece and Vaughan (1991a) have been
analysed with Eqn. (23) (Hu and Mai, 1991b) and shown in Fig. 19. It can be seen
that 4> is increased with fatigue crack growth as the crack-tip shielding is increased.
However, if the increment in 4> due to new bridges is not enough to compensate the loss
due to the degradation of the old bridges, the overall 4> is reduced. A local instability
thus occurs resulting in a discontinuous crack growth. Crack arrest takes place when
more bridges are encountered as it jumps forward. This kind of crack behaviour has
been reported for ZTA and other non-phase transformable ceramics. For comparison,
the steady state 4> value obtained under monotonic loading with asimilar alumina (Hu,
Lutz and Swain, 1991) is also shown in this figure. The bridging stress distributions
under both monotonic and cyclic loading determined by Hu and Mai (1991b) are given
in Fig. 21.

CYCLIC FATIGUE OF PLAIN SPECIMENS

AND INHERENT FLAW SIZE DISTRIBUTION

Experimental Results of Phase Transformable

and Non-Phase Transformable Ceramics
As distinct from large cracks, which are not representative of ceramic
engineering components, plain specimens containing a distribution of "natural" or
inherent flaws are considered in this section. Crack growth in these specimens require
a more sophisticated statistical fracture mechanics analysis. The timHependent
strength phenomenon including cyclic fatigue can only be fully analysed if both the
slow crack growth and cyclic fatigue crack propagation rate equations are known.
However, since these equations may be different for small "natural" cracks compared
to large cracks, accurate predictions of timHependent strengths and failure lifetimes
are difficult. Further, the mechanical fatigue crack growth component is usually not
available.
Predictions of cyclic fatigue crack growth rates in plain specimens therefore
usually make the assumption of a predominant single crack which controls the lifetime
to failure. This assumption leads to errors because in a non-uniform stress field, such
as in rotational bending, the largest crack is not necessarily subjected to the largest
stress. The growth of each crack has to be considered in accordance with the single
crack growth equation. This problem has been considered in detail by Hu et al. (1988,
1989) for single phase brittle materials. Extension to two-phase materials has also
been given recently (Hu, Mai and Cotterell, 1991).

Cyclic fatigue has been studied extensively with plain smooth surface specimens
for Mg-PSZ (e.g. Swain and Zelizko, 1988; Zelizko and Swain, 1988), 3Y-TZP (e.g.
Liu and Chen, 1991), Ce-TZP (e.g. Liu, 1990) and aluminas (e.g. Krohn and
Hasselman, 1972; Guiu, Reece and Vaughan, 1991a). These results are usually plotted
in the form of applied stress range versus lifetime to failure as shown in Fig. 22(a)-(c).
It is noted that for an alumina with an average grain size of 18 Jilll, a zirconia
toughened alumina (ZTA) (Guiu, Reece and Vaughan, 1991b) and a Mg-PSZ (Swain,
Schneider and Zelizko, 1991) the lifetimes under cyclic loading are consistently shorter
than those under static loading of the same amplitude. This implies
that these ceramic materials are sensitive to cyclic fatigue and the
mechanical fatigue crack growth component may be significant. Based

410
a

..

~-71-~0'------1';--~2'------*3-----;4L...--75­
Log tf (min!

Fig. 22(a)

b 3

d
a.. 0 <D
0 0
L:

b 2
<J
" --.,
-
g
C'l
0 -1 0
....J
R= 0
-0-

0.5 -.-
0.8 -0-
2 3 4 5 6
Log Nf

Fig. 22(b)

411
 C <n

'"
~
N .. x .x x •
roo
0- N x
x • x
x x
Eo,.,....
'~
o~

g~
-'
;g
......
IJ"l
2 3 4 5 6
Log Nf

Fig. 22. Cyclic fatigue data for unnotched plain specimens.

(a) Mg-PSZ (. static loading; rotational bending and R =
-1.0 and 15.5 Hz (11) and 200 Hz (0)); (b) 3Y-TZP (push-
pull at 1 Hz and varying R-ratio); and (c) coarse-grained
alumina (push-pull at 5 Hz and R = -1.0. X cyclic, • static).

2.4

o
0..
::E:

b
0\
o
2.3
-J

2.2 '-----'----'---------'----'-----'----'---
-1 o 2 3 4 5 6
Log t f (sec)

Fig. 23. Static fatigue data for an alumina ceramic in rotation bending.

412
on an empirical cyclic fatigue crack growth equation obtained
from experiments S-N curves have been constructed for a 3Y-TZP ceramic by Liu and
Chen (1991). They show that pre-existing processing cracks act as fracture origins in
the plain specimens subjected to uniaxial tension-eompression fatigue and that the
fatigue lifetime is primarily controlled by crack propagation.

Statistical Fracture Models and Comparison with Experimental Data

Statistical fracture theory for distributed cracks. Taking the fracture-site

transition into consideration Bu, Mai and Cotterell (1988, 1989) have developed a
statistical fracture theory for quasi-brittle materials with distributed pre-existing
flaws under non-uniform stress fields. Both monotonic and cyclic loading conditions
are considered assuming only the environment-assisted slow crack growth mechanism
to operate. The assumptions and main results are summarised below. Interested
readers may refer to the original papers.

Following Bunt and McCartney (1979), the Weibull strength distribution in an

inert environment is related to a Pareto distribution for pre-existing cracks (Bu,
Cotterell and Mai, 1985). The failure probability F of a specimen with volume V
under a non-uniform stress field is given by:

F = 1-exp {-l fID q(a)da· dV} (25)

V a(a(x,y))

and the pre-existing flaw size distribution q(a) is given by:

a (M+2)/2
q(a) = Pf . ~.
.t<a [-.Q]
a a>- a0 (26a)
o

(26b)

where Pf is the density of the pre-existing cracks, M Weibull's modulus and a a

o
reference crack. It can be easily proven with Griffith's theory that a( a(x,y)) =
[K IC /(Ya(x,y))]2 and that the usual Weibull strength distribution equation can be
obtained from Eqns. (25) and (26).
In accordance with Eqn. (25), the failure probability at time t due to an applied
non-uniform stress field and the environment-assisted slow crack growth of these
pre-existing flaws is given by:

F(t) = 1- exp {- 1V fIDa( a(x,y)) q(a,t)da· dV} (27)

where the flaw size distribution q(a,t) is timHependent owing to the slow crack
growth. It has been proven (Bu, Mai and Cotterell, 1988) that the pre-existing flaw
size distribution q(a) can be used to replace q(a,t) so that:

F(t) = 1-exp {-lV fIDa/ a(x,y ),t) q(a)da· dV} (28)

413
where ar(O'(x,y)) is related to a(u(x,y)) by

(29)

As a can be evaluated for various stress conditions, such as a constant stress or stress
r
rate (e.g. Bu, Mai and Cotterell, 1988; Duan, Mai and Cotterell, 1988) and constant
amplitude cyclic stresses (e.g. Bu, Mai and Cotterell, 1989), lifetimes for a given
failure probability can be predicted with the statistical fracture theory. This has been
done for the ZTA data given in Figs. 7 to 9. It is noted that if q(a) is a surface flaw
size distribution the volume V should be replaced with the surface area S and the
analysis is still valid.

It should be emphasized again that the statistical fracture theory given above
considers not only fractures at different positions, but also the fracture site transition
due to the time-dependent slow crack growth. This analysis is therefore different to
the single--erack approach even though a Weibull strength distribution has been
included. As shown previously (Bu, Mai and Cotterell, 1988) the application of the
statistical theory in lifetime predictions is not difficult and correction factors to the
single crack analysis for various loading conditions and volume or surface distributed
flaws have been tabulated.

Comparison with Sintle--erack analysis. It is of interest to compare the

theoretical ratio of lifetimes or rotation bending to constant sustained stress for both
the single crack and the statistical fracture multiple crack approaches. Table 1
compares these results for a range of Weibull moduli (M) and slow crack growth
exponent (n) values. Some interesting information emerges. The single crack
predictions are not dependent on M and are only a function of n. Also, the cyclic
fatigue lifetimes are always larger than those for sustained stress. On the other hand,
the statistical fracture approach shows that the predicted lifetime ratios are dependent
on both M and n and that the cyclic fatigue lifetimes can be smaller or larger than the
static fatigue lifetimes. For many brittle ceramics the (M,n) values for glass and
alumina are typically (5, 15) and (20, 50) so that the lifetimes in cyclic fatigue are
always less than in static fatigue. It would therefore be dangerous to draw any

Table 1. Ratio of Lifetimes for Rotation Bending to Constant Sustained

Stresses for the Single and Statistical Multiple Crack Approaches

M n Single Crack Statistical

Theory Fracture Theory

5 10 8.13 0.41
5 20 11.40 0.016
5 40 16.00 "'0.00
10 10 8.13 1.4
10 20 11.40 0.24
10 40 16.00 0.005
15 10 8.13 2.26
15 20 11.40 0.68
15 40 16.00 0.045
20 10 8.13 2.94
20 20 11.40 1.22
20 40 16.00 0.15

414
a 5

uOJ
4 .
. -. - . _. ---.
F=0.9
- - - . -... - - -

~ 3 i ~ F=0.5
...........
: !
.I I F=0.1
C'l 2
0
-.J I
- - - - - - - - - - - - - - - - - _e _

o 10 20 30 40 50
Frequency f (Hz)

Fig. 24(a)

b 5
. F=0.9

u
OJ
4

3
. _._._._------
F= 0.5 ..
~

...........
2
C'l
0
-.J
1

o 10 20 30 40 50
Frequency (Hz)

Fig. 24(b)

415
 c 5 /F= 0.9
4 ._-----_/_------_.
u F=0.5
OJ
III 3 I ~
..... I = :
----)--------! /.------,----
~
F 0.1 :
01
2
0
-'

o 5 10 15 20 2~

Frequency f (Hz)

Fig. 24. Cyclic fatigue failure lifetimes plotted against rotation

frequency for the same alumina ceramic as in Fig. 23. (a)!::.(J =
10.7 MPa, (b) !::.(J = 20.7 MPa and (c) !::.(J = 40.4 MPa. The
maximum cyclic stress is kept constant 227 MPa. Theoretical
lines for different failure probabilities are predicted from
the statistical fracture mechanic multiple crack analysis.

single-cr.ack theory

_. I
.. )::.::-
2.0

d ..
a...
E
stu tistjcul theory
b 1.5
c>

.
0
---'
constun stress
1.0 0 cyclic stress. f=14 r.p,m.
cycti c stress. f= 10,000 r.p.m.
""

0.5
a 2 3 4 5 6
Log tf (sec)

Fig. 25. Cyclic fatigue data for a soda-lime glass in static and
rotation bending. Single crack analysis overestimates the
lifetimes to failure which show good agreement with the
statistical fracture mechanics analysis.

416
conclusions that a ceramic is sensitive to cyclic fatigue simply because the lifetimes are
shorter than under sustained stress.

The static and cyclic fatigue results of a polycrystalline alumina (Krohn and
Hasselman, 1972), and a soda-lime glass (Gurney and Pearson, 1948) are chosen to
illustrate the differences between the statistical and single--<:rack theories. Detailed
analysis of these results have already been given by Hu, Mai and Cotterell (1988).

The static fatigue results for the alumina are given in Fig. 23 and used to find
the necessary parameters for lifetime predictions under cyclic loading. If cyclic fatigue
is only due to environment-assisted slow crack growth then the lifetime is independent
of test frequency as may be predicted theoretically. If a mechanical fatigue mechanism
due to ~K does exist, the predicted lifetimes are overestimated at both high
frequencies and large amplitudes. For all the cyclic fatigue results shown in Fig. 24 the
maximum stress is kept constant at 227 MPa. In Fig. 24(a) the cyclic stress amplitude
is 10.7 MPa, no obvious mechanical fatigue effect is detected for cycling frequencies up
to 40 Hz. However, when the cyclic stress amplitude is increased to 20.7 MPa the data
at 40 Hz clearly show a sensitivity to cyclic fatigue, Fig. 24(b). With a higher cyclic
stress amplitude of 41.4 MPa, the influence of a true mechanical fatigue effect becomes
obvious even at 10 Hz, Fig. 24(c). The theoretical lines in Figs. 23 and 24 are
predicted from the statistical fracture theory for failure probabilities of 0.1, 0.5 and
0.9. These results confirm that in plain alumina specimens sensitivity to cyclic fatigue
depends on cyclic frequency and stress amplitude. It is likely that the degradation of
grain bridges in aluminas is more effective at high frequencies and large amplitudes.

The soda-lime glass static and cyclic fatigue results are given in Fig. 25 along
with predictions from both the statistic and single--<:rack theories. In line with the
theory given by Hu et al. (1988) and Table 1 the statistical multiple crack analysis
gives shorter lifetimes in rotation fatigue than static fatigue. This prediction is in
agreement with the experimental data obtained.

CONCLUDING REMARKS

The connection between crack-resistance (R) curves and cyclic fatigue crack
growth is given for both phase transformable (e.g. the partially stabilised zirconias)
and non-phase transformable coarse-grained (e.g. aluminas and silicon nitrides)
ceramic materials. The presence of non-linearities in the stress-strain curves of these
ceramics (particularly the zirconia-based materials) is a good indication that they
have a crack-resistance curve behaviour. For such non-linearities are associated with
crack-tip shielding processes which lead to a toughening of the material. Efforts to
promote more pronounced R-{;urves in ceramic materials are met with the problem of
increasing their sensitivity to mechanical fatigue. It is postulated that any physical
mechanisms that lead to cyclic fatigue must result in a degradation of the crack
shielding processes. Thus, in the phase transformable ceramics this can be a reduction
in the crack-bridging zone (for Ce-TZP) or accumulative damage due to
rnicrocracking (for 3Y-TZP). It appears that the usual phase transformation-induced
shielding mechanism is unaffected by cyclic loading. In the non-phase transformable
ceramics clear indications have been given of the frictional degradation of the
grain-bridges due to repetitive abrasions (for coarse-grained aluminas) and the
fractures of the grain bridges in the crack wake region (for silicon nitrides). Another
reason for the strength degradation that has not been much studied is the plausible
reduction of the toughness term K in cyclic loading relative to static loading.
o

A simple analysis has been given to measure the crack-bridging stress in the
wake region of non-phase transformable aluminas in both monotonic and cyclic
loading using an experimental compliance method. It is demonstrated that frictional
degradation of the grain bridges has caused much reduction in the bridging stress
leading, therefore, to a sensitivity to mechanical fatigue. It is expected that the

417
degradation of the bridging stress in cyclic loading is controlled only by the
stress-ratio, cyclic stress range and number of elapsed cycles but not by specimen size
and geometry. Simple experiments can be performed to verify this proposal.

Cyclic fatigue crack growth in the ZTA and other ceramics with R-eurve
characteristics is discontinuous with periodic crack arrests due to the heterogeneous
nature of these materials. Initial crack growth is characterised by a negative slope in
the da/dN versus ~K log-log plot for both small and large cracks. Like in metals and
polymers, the crack growth rates and hence the lifetimes to failure are determined by
the test frequency, stress ratio and cyclic stress amplitude, for they control the
magnitudes of degradation of the crack shielding processes. In small cracks involving
tension-tension cycling the shielding degradation process is not as much as in large
cracks. And for both small and large cracks the degradation is more severe in cyclic
loading involving tension-eompression, i.e. a negative stress ratio, than
tension-tension only.

Attention is drawn to the practical significance of plain specimens with

distributed inherent flaws. From the statistical fracture mechanics theory presented, it
is shown that the conventional single crack analysis in non-uniform stress fields (such
as in rotation bending) is inaccurate and it may lead to erroneous conclusions
regarding mechanical fatigue effect in ceramic materials, if simply because failure
lifetimes in cyclic loading are smaller than in static loading.

Except for the coarse-grained aluminas the cyclic fatigue mechanisms for many
other ceramic materials remain largely undiscovered and until these become fully
understood it seems premature to put up any theoretical fatigue crack growth models.
In particular it appears that much more work should be directed towards
understanding the elevated temperature R-eurve and cyclic fatigue behaviours.

ACKNOWLEDGEMENTS

The authors wish to thank the Australian Research Council (ARC) for the
continuing support of this work. Parts of this review are also funded by the DITAC
New Materials Technology (GIRD) grant. X-Z.H. is supported by an ARC National
Research Fellowship and K.D. by a CSIRO/Sydney University Postgraduate Research
Scholarship. The zirconia-toughened alumina (ZTA) materials reported in Figs. 3 to 6
are developed by the late Dr. R. Garvie of the CSIRO Division of Materials Science
and Technology. Thanks are also due to S. Bennison, F. Guiu, S. Lathabai, B.R.
Lawn, T. Liu and J. Rodel for contributions in the form of original data and many
useful discussions.

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422
EFFKTS CF CRACK SIZE CN CRACK PRCFAGATICN BB-lAVICR AND EXPERIMENTAL

VFRIFICATICN CF CYOJC FATIGUE MIllIANISM CF SINTERH> SIUCCl'ol NJ1RIIE

Akira Ueno*, Hidehiro Kishimoto*, and Hiroshi Kawamoto**

*Toyota Technological Institute, 2-12-1, Hisakata, Tempaku-ku

Nagoya 468, Japan
**Toyota Motor Corp., Higashifuji Technical Center 1200
Mishuku, Susono 410-11, Japan

ABSTRACT

In order to investigate the effects of crack size on the crack propagation behavior of a
sintered silicon nitride, crack propagation tests were carried out under cyclic loads and static
load. Two kinds of small semielliptical surface crack were introduced by Knoop indentor.
By polishing the surface layer, the residual stress around the Knoop indentation was
completely removed. The crack propagation rate of small cracks (35~m, 2oo~m) was lower
than that of long cracks obtained with a CT specimen. On the other hand, by measuring and
analyzing the crack opening displacement (COD) of 350~m crack, we were able to determine
the quantity of the true stress intensity factor Kltip' Kltip was defined by the following
equation

in which Klmax is the stress intensity factor calculated by the applied stress and the crack
length. K s is the stress intensity factor shielded by bridging effects. Furthermore, we found
that COD after cyclic loading was larger than that before cyclic loading. It was evident that the
increase in COD after cyclic loading was attributed to the reduction of bridging force with
cyclic fretting at the bridging sites. Under the cyclic loads, the reduction of bridging force
resulted in an increase in Kltip which, in tum, accelerated the crack propagation rate.

INTRODUCTION

As the stress varies with time in machine structure, it is important to study the fatigue
life behavior of ceramics under cyclic loads to achieve reliable design. There have been some
reports \.') that showed life reduction by cycling load for ceramics, such as sintered silicon
nitride. On the other hand, as the ceramics fracture almost always initiates from the
manufacturing defectsl~ such as pores or inclusions, the mechanisms of cyclic fatigue with
small cracks should be studied. However, there are only a few reports discussing the
behavior of small crack propagationl\'l~
In this study, we c1ari fied the effects of crack size on the crack propagation rate using
the small semielliptical surface crack. Furthermore, we determined the quantity of the
bridging effects on small cracks, and the cyclic fatigue mechanism of ceramics was verified
by analyzing the crack opening displacement.

Frtulure Mechanics of Ceramics. Vol. 9

Edited by R.C. Bradt el ai.. Plenum Press. New York, 1992 423
 Table I. Mechanical properties of sintered silicon nitride.

Bending strength Young's modulus Poisson's ratio Fracture toughness

alb (MPa) E(GPa) v K c (MPa.m)

710 310 0.27 5.57

SPECIMEN AND EXPERIMENTAL PROCEDURES

The material used in this study was a sintered silicon nitride doped with Ah03 and
y 203. The mean grain size of this material was about 0.48Jlm and the mean aspect ratio of the
elongated grain was 6.8 14 • The mechanical properties are shown in Table 1. Fatigue
specimens were machined into the shape shown in Fig.l, after which the specimen surface
was buff-finished using Ah03 powder. In order to compare the propagation behavior of
small-cracks with that of long-cracks, these specimens were cut out from the CT specimen as
shown in Fig.2. A small semielliptical surface crack was induced at the narrowest part of the

2a

t-·~:oC]
Section A - A ()

C')
N

30 t~0.9

Fig. 1. Configurasion and dimensions of Fig. 2. Cutting position of fatigue

fatigue specimen. specimen.

Normalized surface removal

2 3 4 5 6 7 8 9 10

Knoop indentation
8:-
~ -500 ~</)=(J
I

1/>=90'
0: I/>=rf
.:1/>=90'
(ij . -. : ResidJai stress
::J
"0 on lapp:ld surface
'iii
OJ
a: -100
OL..-_..L-_......._ ........_-'-''--....L._.....J
o 10 20 30 40 50 60
Surface removal/), lim

Fig. 3. Relationship between residual stress and surface removal.

424
fatigue specimen, as shown in Fig.l. This crack was induced by Knoop indentor. Two
different sizes of crack, crack length 2a of 350/lm and 200/lm, were induced with indenting
loads of 98N and 34N, respectively. The residual stress around the Knoop indentation were
measured by the X-ray diffraction method. The residual stress of the 98N indentation is
depicted in Fig.3 as a function of the surface removal of the specimen. The surface removal
was normalized by the depth of the Knoop indentation. The residual stress tends to decrease
with increase in the surface removal until the value of normalized surface removal reaches
about 7 times the depth of the Knoop indentation. The residual stress was almost completely
eliminated by polishing the specimen surface, as shown in Fig.3.

(j)Specimen
®Load cell
@Mean stress adjustor t8~ '1
r--=

F= ! ~
"!.,, I "..,

"SS'~ rib,
f,J.., ~~
Ij
,,=., ;;::: I!I ;;::: ;::;
a
rn
! '"
..,...
I
"'r
I

1
<6. .,;,
$V. i
@-~. ~
4-4r
y.$-
4-+
-<p--0-

240 ~

Fig. 4. Electromagnetic bending fatigue testing machine.

Distance from center d, mm

-1.0 -0.5 0.0 0.5 1.0

Crack front
0.5
configuration
- - - - : Initial shape
- - : Final shape
1.0
Fig. 5. Simulated configuration of propagated crack.

425
 The crack length 2a' and crack depth c' after surface removal were calculated by eq.(1).

a'=a ~ 1- 82 (1)
a2 ·Aspect 2

c' =a-Aspect - {)

in which 2a and c refer to the original crack length and original crack depth, respectively. c
indicates the surface removal of each specimens. The mean values of 2a' and c'/a' are 346llm
and 0.61 with 98N indentation, 2031lm and 0.61 with 34N indentation, respectively.
Fatigue tests were carried out by an electromagnetic bending fatigue testing machines, as
shown in FigA. A cyclic fatigue test under 60Hz sinusoidal wave-form and a static fatigue
tests were performed. The crack length was measured by using a metallographic microscope
and the crack depth values c' after crack propagating were estimated by using the simulation
program while the crack depth values c' corresponding to 2a' were indicated graphically, as
shown in Fig.5. The stress intensity factor was calculated by Raju-Newman's equation lS ,
substituting the measured 2a' and estimated c' values into this equation.

EXPERIMENTAL RESULTS AND DISCUSSIONS

Comparison of Propagation Rate of Small Crack with that of Long Crack

Figures 6(a) and 6(b) show the relationship between maximum stress intensity factor
Klmax and the crack propagation rate under static and cyclic loads, respectively. The crack
propagation rate measured through the CT specimen is also represented by solid lines. Arrows
indicate the stress intensity factor when 200llm cracks started propagating. This value is
nearly equal to the threshold stress intensity factor. Under static load, the propagation rate of
350llm cracks was lower than that of long cracks (CT specimen). The stress intensity factor
Klmax which started the 200llm crack propagating was lower than that of 350llm cracks. This
Klmax is almost equal to that of long cracks. Under cyclic loads, the propagation rate of
350llm cracks was the slowest, that of 200llm cracks was in intermediate range, and that of
long cracks were the fastest. As shown in Fig.6(b), the crack length varied from 200llm at
initial condition to 400llm at final condition in the case of 200llm crack, and from 350llm at
initial condition to 600llm at final condition in the case of 350llm cracks. The difference
between crack propagation rate of 200llm cracks and 350llm cracks tended to smaller as the
200llm crack grew larger.

Interaction of Crack Surfaces

In order to investigate the effects of crack size on the crack propagation behavior, the
difference in the crack opening displacement (COD) of each size crack was studied. Figures
7(a) and 7(b) show the COD of long cracks and small semielliptical surface cracks,
respectively. As shown in Fig.7(a), the COD of long cracks was larger than the mean grain
size. Therefore, the debris of Si3N4 grains can enter between the crack surfaces, which can
induce crack closure and wedge effects. On the other hand, the maximum COD of 350llm
crack was about 0.1 211m as shown in Fig.7(b). As this COD was smaller than the mean grain
size, the debris-induced crack closure could not occur in small crack. In contrast to this
phenomenon, grain bridging was observed in the range of small COD, as shown in Fig.8.
Arrows indicate the grain bridging sites. Figure 9 represents the schematic diagrams of grain
wedging and grain bridging. At the sites where COD was larger than grain size, wedging
occurred. At the sites where COD was smaller than grain size, bridging occurred. Wedging
is thought to affect the stress intensity factor at the minimum load during cyclic loading while
bridging is thought to affect the stress intensity factor. The true stress intensity factor Kltip at
maximum load is expressed by the following equation 16

426
 3/2
K lmax ' kgf/mm
a 10 12 14 16 18 20
104 rr--r-r--rj---.....--,---rr-1"T"""1 1
Key I Creek ",el"ml I
o 0.1
1-
350
3l 10 5 I

fi
OOngICT) -

IFinal 2a.55011m >•

-.. I
E
I I I
10-6~=i=±~~~~~"--r}'"'
g
Final 2a.60011m K"V
i5
~ I I
~
7
10 t--1--t--j--

ia.
10 8t---+-+--+
I
~
-
K 9 Iinilial 2a.35011m)'
.:.r: 10 I --
5 101('---'------'-...L-~
~V:.......J.----'---J
nn 1--
3 4 5 6
Stress intensity factor K lmax ' MPalm

3/2
K lmax' kgf/mm

b -41"110_-r-"'12...--r_1-r4,--1,.6---,1r8..,
10 Ir --;;;;;"lrr.;:;;,;I;;:;;;;;;-
Key Crack siZ9Wml
-++-1

4 5 6
Stress intensity factor K lmax ' MPalm

Fig. 6. Relationship between maximum stress intensity factor and crack propagation rate:
(a) Under static load, (b) Under cyclic load.

427
 E 7r--------------,
: 6 ~ Applied load = 441 N
['o-o--q
I:
~ 5 ~ K 1= 3.09MPaJffi

~ a=7262mm

: "0'0-0
.§
Q)
2 '0-0
Q.
o 1 Mean grain size (0.5Jlm)
.::t:- ...................................... .. "

U
~
o1.--.-.1_--'-_-'-_........._ ' - - - - ' - _..........-'--'
o 012345678
Distance from notch tip d, mm
(a) In the case of long crack (CT specimen).

0.08
Applied be~ding strain E a= 880JlE

E 0.06 o -+- 0-
K 1= 3.2MPaJffi

e
::1.
o 0 0 I
(,Q

ci 0.04
0 8 0
~ 0-8
cj
cj 0
0
o
B
0
~
T""
0.02 6'-

0.00 ~ ~

-200 -100 o 100 200

Distance from center , J.lm
(b) In the case of small semielliptical surfce crack. Crack length 2a'=340J.lm.

Fig. 7. Examples of COD measurements.

where, K s is the stress intensity factor originated from stress shielding by bridging. The
correlation between the K s and the crack propagation behavior in relation to crack size is
discussed in the following section.

Effects of Wedging on Stress Intensity Factor

Grain wedging effects were analyzed by FEM. The mesh model of 1/4-CCT specimen
is shown in Fig.IO where crack length 2a=lOmm, and specimen width B = 40mm. The
debris was replaced by constrained displacement at the nodes. The values of constrained
displacement were IJ.lm and O.5J.lm, which were determined on the basis of the debris size
observed on the fracture surface2.~ The stress intensity factor was calculated based on the
stress (Jy ahead of the crack tip. The results of FEM analysis is shown in Fig.ll. The solid
line indicates the stress intensity factor without debris and the circle symbols indicates that

428
Fig. 8. Microphotograph of 350~m crack. Arrows indicate grain bridging sites.

• COD>Grain size; Wedging

••
t COD<Grain size; Bridging

~
t
Fig. 9. Schematic disgrams of grain wedging and grain bridging.

429
 Delail of part B O.5mm

Detail of parI C 50Jjm

Detail of parI D 5Jjm

Fig. 10. Mesh model of 1/4 - CCT specimen.

Key Debris si2eljJml

1.0 0.5
1.0

10 0
~
~ 0.5 f 0- -000 I
--j----+-t
:.:

o. 0 L.o............'-'-~.....................J....J
0.0 0.5 1.0
PIP"".

Fig. 11. Results of FEM analysis.

430
with wedging. Although the stress intensity factor Klwedge with wedging was higher than that
without wedging, Klwedge does not exceed the maximum stress intensity factor Klmax. It was
concluded that the wedgmg increased the minimum stress intensity factor Klmin and decreased
the effective stress intensity factor range L1Keff. It was evident from our previous study that
the decreased L1Keff lowered the crack propagation rate under cyclic loads 2•

Effects of Grain BridiPn& on Stress Intensity Factor

In order to verify the effects of grain bridging, the crack opening displacement (COD)
of 350J.tm cracks was measured by SEM. Figure 12 shows the measurements of COD. This
COD was measured on the surface of a cracked specimen, to which a bending strain of 880lJ£
was applied. The bending strain was detected by a strain gauge attached to the back-surface of
the specimen. In order to estimate the stress intensity factor of this small crack affected by
grain bridging, Torii et al.'s method)7 was applied to the measured COD. This procedure is
summarized as follows:

J7
0.08 r - - - - r - - - - - ; - - - - - - - r - - - - - - ,
Approximated curve

: 0.06t-----+-- ~~ 0 '0
ci 0.041-----· o'S -----I

~ v~,~
~ 0.02 1Y

0.00 L..-Q-"---.l..--"--_.L...._"---_L....-_'--{")-J
-200 -100 o 100 200
Distance from center , 11m
Fig. 12. COD measurements on 350llm crack.

(l) Measured COD were approximated by a polynomial of third degrees and equation
(3). The approximated function was denoted with VI of polynomial and V2 of eq.(3)

() ( ' ) 1/2 + (3('

V2x=aa-x a-x )3/2 (3)

in which a' is the half length of the surface crack, and x is the distance from crack center.
(2) The crack opening stress <Jyy was calculated by substituting these functions of VI
and V2 into eq.(4)

in which V is the approximated function of VI and V2. E' is the modified Young's modulus,
which is equal to E/(I - v2) for plain strain. We used 310GPa of E, and 0.3 of Poisson's
ratio v.

431
 300
_______ .l _________ _________I. _______
~

Applied bending stress

ell 0a =270MPa
~ 200

o
·200
~
o ·100 100 200
Distance from center , 11m
Fig. 13. Relationship between crack opening stress <Jyy and distance from crack center.

(3) The stress intensity factor of the surface crack was calculated by substituting the <Jyy
into eq.(5).

In Fig.12, solid line shows the approximation of VI and V2. We obtained the
following equations for VI(X) and V2(X).

VI (x) = -5.663 X 1O- 13x 3 • 6.022 X 1O- 6x 2 + 1.836 X 1O-9x + 0.108 (6)
oflm :s; x :s; 38.30 flm
V2(X) =7.327 x 10- 3 (c - x)1/2 + 8.247 X 10-6 (c - x)3/2 (7)
38.30 flm :s; x:s; 170.0 flm

Providing functions VI and V2 are symmetrical to the origin, and substituting VI and V2 into
eq.(4), we obtained the crack opening stress CJyy as shown in Fig.13. The maximum CJyy of
about 70MPa was thought to be applied to this crack. In Fig.13, the dashed line indicates the
applied bending stress CJa. The ratio of CJyy/CJa was about 0.25. This discrepancy between CJyy
and <Ja is thought to originate from two causes. One is the boundary condition of the
semielliptical surface cracks stressed in bending and the other is the effects of the bridging
force distributed on the crack surfaces. Torii et al. 18 discussed issue of the boundary
condition and reported that the ratio of CJyy/CJa was about 0.8 in the case of a semieIliptical
surface crack under tensile stress. Nevertheless, they showed that the estimated stress
intensity factor from eq.(5) coincided with the value obtained through Raju-Newman's
equation. It was thought that the stress intensity factor obtained by eq.(5) was not affected by
the boundary condition.
The estimated stress intensity factor Klesti obtained by substituting the distribution of
C}yy into eq.(5) was about 0.7MPavrn. The stress intensity factor Klmax calculated by Raju-
Newman's equation was 3.2MPavrn. The difference in these two values (KImax - KIesti) is
attributed to the stress shielding effects of grain bridging. We believed that grain bridging
distributed the frictional force over the crack surface thereby closing the crack surface.

432
 0.2
E Key I Loading/unloading
:t
-x 01 Unloading ~
I Loading
'E"
f- •

(,CJ
I
ci 0
0 0.1
0 •

i
E
:J
E
'x
co
~
0.0
o 500 1000 1500
6
Applied bending strain £a' X10·
Fig. 14. Relationship between applied bending strain fa and maximum COD Omax.

5 1 1
Key I Loading/unloading

4
01 Unloading
.1 Loading

~-

'::£.(J) 2 • 0
eo

o i
0.0 0.1 0.2
Maximum C.O.D. 8max ' Ilm
Fig. 15. Relationship between Omax and Ks.

433
The Behavior of Grain Bridging Effect Ks.

If K s originated from the frictional force at the grain bridging sites, the direction of
bridging force during loading was opposite that during unloading. In order to clarify the
bridging effects, we measured the COD of 350~m crack under bending strain and calculated
Ks• Bending strain was applied in the following sequence: 1200~€ - 850~€ - 488~€ - O~€ -
488~€ - 850~€ - 1200~€. The stress intensity factor Klmax at 1200~€ was 4. 39MPa"fii.
Figure 14 shows the relationship between the applied bending strain Ea and the maximum
COD Omax at the crack center. The Omax value measured during unloading was larger than that
measured during loading at bending strain of 850~. It is obvious that this difference was due
to the difference in the direction of the bridging force. During loading, the bridging force
prevented the crack from opening, and during unloading, the bridging force promoted crack
opening. Figure 15 shows the relationship between Omax and K s. K s increases as omax
increases in this range of COD.

(a) At first loading cycles. O} =0.160~m, <52=0.160~m, 03=0.193~m.

Fig. 16. SEM microphotographs of crack path.

Effects of Cyclic Load on Grain Bridging

In order to verify the effects of grain bridging on the fatigue mechanisms of ceramics,
the analyzing method as stated above was applied to the crack under cyclic loads. The COD
was measured after 106 cycles with Klmax=4.0MPa"fii, stress ratio R=O.l, and measured
again after 5xl06 cycles with Klmax=4.1 MPa"fii, R=O.1. The applied bending strain was
equal to 1200~€ in each case. SEM micrographs of crack-path are shown in Figs.16(a)-
Fig.16(c). Figure 16(a) shows the crack profile before cyclic loading. The arrows in
Fig.16(a) indicate the measuring positions of COD, O}, <52 and 03. O} =0.16~m, <52=0.16~m
and 03=0.19~m. After 1Q6 cycles, as shown in Fig. 16(b), O}', <52' and 03' were larger than
Ob <52 and 03, respectively. After 5x106 cycles, as shown in Fig.16(c), the COD apparently
increased as compared with Fig.16(b). The whitened layer on the crack surface were
observed, as shown in Fig.16(b) and Fig.16(c). The thickness of this layer tended to
increase with increase in the number of cycles. We considered that this layer might consist of
powder produced by cyclic fretting wear.

434
(b) After 106 cycles. oJ '=O.235Ilm, fr}. '=O.145Ilm, c5:3 '=O.260Ilm.

(c) After 5XI06 cycles. 01 "=O.259Ilm, fr}."=O.210llm, 03"=O.272llm.

Fig. 16.(continued) SEM microphotographs of crack path.

435
 400
. I I I
.............................. - .................................................................
Applied bending stress Key Number of cycles

11l 300 ~ cra = 358MPa - 0 1

a.. 0 10'
~ [:, 10 + 5X10'

en
en

~~-
~
ij) 100

o
-200 -100 o 100 200
Distance from center , 11m
Fig. 17. Crack opening stress CJyy before/after cyclic loading.

5 r=;:::::::;::::;::::;::=:::::r:;::::=--~-------,

4
Key

o
•
o
[:,
Number 01 cycles

1 (unloading)
1 (loading)
10
10 +SX10
T
3 ~====+=7=-- ~--;
* 2 !---------1y-,r- - - - - 1 - - - - - - - 1

,z • /4-~ •
"/. ~
01'..--""""---J.---------L------.1
o 500 1000 1500
Applied bending strain fa , X10·6
Fig. 18. Relationship between applied bending strain fa and Klesti.

The crack opening stress CJyy derived by using the COD of each of the three loading
cases is shown in Fig. 17. CJyy also increased as COD increased. Figure 18 shows the
relationship between applied bending strain fa and Klesti which was estimated through eq.(2)
with CJyy. Klesti is believed to be the true stress intensity factor KItip. Compared to the
precyclic load values, the KItip increased by 1.1 MPavrn after 106 cycles and the Kltip after
SX106 cycles increased by 1.7MPa..JiTI. It was evident that the reduction of bridging force
made the Kltip increase under cyclic loads 19 and that the degree of degradation of bridging
force dependent on both the magnitude of applied Klmax and number of cycles. As stated
above, it was concluded that the degradation of the grain bridging effects with cyclic fretting
was responsible for the KItip increase which, in turn, accelerated the crack propagation rate
under cyclic loads.

Influence of Crack Size on the Crack Propagation Rate

We tried to explain the crack propagation behavior shown in Figs.6(a) and 6(b), on the
basis of the above mentioned fatigue mechanism. In the range of bmax in Fig.IS, it can be
thought that K s decreases with decrease in bmax. Therefore, under static load, the KItip of

436
350llm cracks was lower than the Kltip of 200ilm cracks. Under cyclic loads, the crack
propagation rate of 200llm cracks was hIgher than that of 350llm cracks. This difference was
attributed to the difference in the K s of 350llm cracks and 200ilm cracks. After cyclic load, it
was thought that the Klti of 200ilm cracks was higher than that of the 350llm cracks. As the
200llm cracks lengthened and approached the size of the 350llm cracks at the final stage of the
crack propagation test, the effects of bridging tended to be almost identical and the
discrepancy in crack propagation rate of both cracks almost vanished.
The COD of long through cracks (CT specimen) increased parabolically, the area of
bridging was localized in the narrow space near the crack tip. Consequently, the bridging
effects on the Kltip of the long cracks was smaller than that of the 350llm cracks, because
grain bridging occurred everywhere on the crack surfaces in the case of 350llm cracks. The
propagation rate of the long cracks was thought to be almost the same as that of the 200llm
cracks, in which slight grain bridging took place. The bridging effects on the micro-cracks
initiated from pores and inclusions is an important topic, but it is beyond the scope of this
study.

CONCLUSIONS

The major conclusions obtained in this study are summarized as follows:

(1) Under static and cyclic loads, the crack propagation rate of the 350llm cracks was
slower than that of the 200ilm cracks. Although the 200ilm cracks started propagation at the
lower stress intensity factor than that of the 350llm under cyclic loads, the crack propagation
rate of the 200ilm cracks tended to approach the crack propagation rate of the 350llm cracks
with increase in the crack length.
(2) The wedge effects resulted in a decrease in the range of the true stress intensity
factor Kltp,.
(3) B'y analyzing the COD of 350llm crack, we obtained the true stress intensity factor
Kltip' We also estimated the stress intensity factor component of stress shielding K s, by
comparing the Kltip with Klmax obtained by Raju-Newman's equation.
(4) Kltip of 350llm crack is thought to be lower than that of 200ilm crack, on the basis
of the relationship between COD and Ks in 350llm crack (Fig. 15).
(5) We found that the COD before cyclic loads was smaller than that after cyclic loads.
Consequently, Kitip before cyclic loads was lower than Kltip after cyclic loads.
(6) It was evident that the increase in COD after cyclic load was attributed to the
reduction in bridging force with cyclic fretting at the bridging sites. Under cyclic loads, the
reduction of bridging force led to an increase in Kltip which in turn accelerated the crack
propagation rate.

ACKNOWLEDGMENTS

The authors are grateful to Mr. Y.Yamanaka of NIPPONDENSO Co. Ltd., for
assistance with experimental work.

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the Japan Society of Mechanical Engineers, A-57: 746 (1991).
19. G. Grathwohl, Ermudung von Keramik unter Schwingbeanspruchung, Mat.-wiss.
u. Werkstofftech., 19: 113 (1988).

438
FATIGUE CRACK PROPAGATION AND FAILURE PREDICTION FOR TOUGHENED CERAMICS

UNDER CYCLIC LOADS

Akira Okada and Toshio Ogasawara

Central Engineering Lab., Nissan M::>tor CO., Ltd.

1, Natsushima-cho, Yokosuka 237 Japan

ABSTRACT

An investigation was made of the possibility for the lifetime of

corrponents made of toughened ceramics to be shortened under cyclic loads.
calculations were made of cyclic fatigue crack propagation and failure
prediction under the assurrption that the crack velocity was governed by both
time-dePendent and cycle-number-dePendent rates as a function of crack tip
stress intensity. Time-dependent crack propagation is shown to govern the
region of high crack tip stress intensity, while cycle-number-dependent crack
propagation governs the low stress intensity region. The frequency of stress
and the stress intensity at the crack closure are shown to affect the crack
velocity in the region governed by the cycle number. The contribution of
intrinsic and extrinsic mechanisms to fatigue crack growth and the resulting
cyclic fatigue behavior are discussed in comparison with experimental data.

INTRODUCTION
The excellent mechanical properties of advanced ceramics have led to
the application of structural ceramics to autorrobile engine corrponents, such
as turbocharger rotors, in the last decade. During this time the design
methodology for applying brittle materials to mechanical parts has been
developed to avoid catastrophic failure and thereby assure corrponent
reliability. Finite and boundary element methods have been used to achieve
designs for reducing the maximum tensile stress corrponent, consisting of
mechanical and thermal stresses, resulting in a low probability of component
failure. The small dimensions of processing flaws in ceramic corrponents made
quality control difficult, which gave rise to a wide range of strength
distribution arrong components. This made it necessary to eliminate
corrponents with low strength levels. Proof testing,1-6 a destructive testing
method of applying a constant stress to cause fracture of weak corrponents,
has generally been used for this purpose.

Since fracture of ceramic components in service must be avoided,

failure prediction7- 11 has been employed to assure sufficient durability for
the required service life. Delayed failure is generally predicted on the
basis of the subcritical crack growth velocity from a pre-existing flaw.

Fracture Mechanics of Ceramics, Vol. 9

Edited by R.C. Bradt et ai., Plenum Press, New York. 1992
439
Flaw generation under service conditions can also contribute to delayed
failure, for which several mechanisms are known. These include chemical
reaction at the surface such as oxidation12 ,13 and corrosion,14-16 surface
crack formation such as impact damage 17- 19 caused by foreign particles
striking rotating corrponents, and contact damage due to local contact of
ceramics which results in high local stress. 20 The design of ceramic
corrponents must also avoid strength degradation which occasionally occurs
during use as a result of flaw generation. One of the problems encountered
in making failure predictions based.on the subcritical crack growth velocity
is uncertainty originating in the extrapolation of component lifetime from
experimental data on short time failure. This uncertainty stems from the
lack of a clear understanding of the phenomena that occur under low stress
intensity. The assumption that a crack propagation law in the high stress
intensity region of a short lifetime can apply to the region of a low stress
intensity with a long lifetime may provide a Jrore reliable estimation, if a
threshold value 21- 27 for subcritical crack growth exists or if crack tip
blunting28 ,29 and crack healing30 - 32 occur in the lower stress intensity
region. However, in cases where cracks coalesce in the initial stage of
propagation,33-35 and crack propagation is governed by cyclic fatigue in the
region of low stress intensity,36,37 this assumption may yield unreliable
estimations because a greater crack extension rate may occur than expected in
the region of low stress intensity. In the present study, an analysis was
made of the possibility for component lifetime to be shortened by cyclic
fatigue.

CRACK PROPAGATION AND FAILURE PREDIcrION IN CERAMICS

The fracture strength of ceramics is virtually governed by the flaw

distribution induced during the production process. Fracture under cyclic
loads also results from rapid crack propagation of a pre-existing flaw when
the critical stress intensity of the worst crack reaches the fracture
toughness of the material. This mechanism differs greatly from that of
metals, in which the Jrovement of dislocation leads to an increase in surface
roughness, resulting in formation of a surface notch. Crack extension
initiating from the notch occurs as a function of the stress intensity range.
Therefore, a trace such as striation, which is generally observed in metals,
has not been observed in ceramics, and phenomena derived from the Jrovement of
dislocation such as stress hardening and the coaxing effect have not been
reported in ceramics. Accordingly, fatigue in ceramics has been thought to
be caused by the accumulation of static fatigue due to stress corrosion
cracking. Failure prediction has therefore been based on analysis of time-
dependent crack growth.

Subcritical crack propagation in ceramics is generally given by38

da/dt =A KIn (1)

where A and n are parameters describing subcritical crack growth, and KI is

the applied stress intensity. This expression was shown to be dimensionally
strange because the dimension of A was given as a function of n. 39
Therefore, an inproved expression was proposed: 40

da/ dt = Vo (KI/ Ke) n (2)

where Ke is the fracture toughness of the material and Vo = A Ken. Failure

prediction of ceramics has generally been based on the expression for
subcritical crack growth velocity. Time to failure, t s , under a constant
stress of as is calculated from Eq. (1) as follows: 2

440
 (3)

where Si is the fracture strength in the inert environment, g-1 = Ay2 (n-2)
Kcn-2 / 2, and y is a geometrical factor dependent on the crack
configuration. Similarly, fracture strength under a constant stress rate is
given b y41

(4)

where crf is the fracture strength and is is the stress rate. Time to failure,
t e , under cyclic stress can be calculated in a similar manner 42 .

(5)

where crav is the average applied stress and A. is the period of cyclic
loading.

Recent studies 43 - 45 suggest that the expression for failure prediction

needs to be rocxiified because toughened ceramics exhibiting steep R-curve
behavior have been reported to display degradation due to cyclic loading. R-
curve behavior in ceramics generally occurs as a result of stress transfer
behind the crack tip. This stress transfer can be classified into two types.
One is a direct stress transfer such as sliding pUll-out 46 and grain bridging
mechanisms,47 and the other is a process zone wake such as stress induced
transformation 48 ,49 and stress induced microcracking. 50 Wake in the process
zone produces compressive stress at the crack interface through volume
expansion of the process zone, resulting in reduction of the stress field
near the crack tip. This indicates that the applied stress intensity
required for rapid crack propagation is given by the total of the additional
stress intensity due to stress transfer and the critical stress intensity of
the material at the crack tip.

As indicated by Lawn,51 crack propagation is virtually governed by crack

tip stress intensity. An improved expression achieved by using a crack tip
stress intensity factor was reported for subcritical crack growth of sintered
silicon nitride, which exhibited R-curve behavior. 52 A rising KR
characteristic was shown to result in a shift of the v-Kr relationship to the
high Kr region.

In corrosion fatigue of metals, where cyclic stress accelerates the

subcritical crack growth velocity due to stress corrosion cracking, crack
propagation is virtually governed by the stress intensity range. Considering
that the stress corrosion cracking mechanism, however, contributes to both
static and cyclic fatigue, a combined effect should be taken into account.
Wei and Landes 53 proposed an expression for the combined effect consisting of
the two terms of time-dependent and cycle-number-dependent crack growth.
Cycle-number-dependent crack propagation was recently reported in
ceramics. 36 ,43-45 Crack propagation in zirconia under cyclic loads displayed
cycle-number dependence,43,44 and silicon nitride exhibited cycle-number
dependence under a low stress level whereas time-dependent crack growth was
reported at a high stress level. 36 It should be noted that these toughened
ceramics, exhibiting steep R-curve behavior, show cycle-number dependence for

441
fatigue crack growth. Therefore, an evaluation of the effect of the stress
transfer at the crack interface on fatigue crack propagation is regarded as
an irrportant factor in predicting the ti.Jre to failure of toughened ceramics.

CYCLIC FATIGUE AND CRACK PROPAGATION MECHANISMS

Subcritical crack growth in ceramics has been considered to be caused

by stress corrosion cracking due to a surface reaction with water rrolecules
at the crack tip. Extensive study was focused on subcritical crack growth in
glass. It was reported that there were three stages in crack propagation: 54
the lowest crack propagation rate in stage I was governed by the reaction
with water rrolecules at the crack tip, thus the crack velocity was controlled
by the partial water vapor pressure in the ambient atrrosphere; the crack
growth in stage II was governed by the diffusion of water rrolecules toward
the crack tip, thus the crack velocity was independent of the water vapor
pressure; and the highest crack growth velocity in stage III was independent
of the water vapor pressure in the atrrosphere. Arrong these stages, stage I
was thought to be the rrost irrportant for determining the ti.Jre to failure.
Another rrechanism of subcritical crack growth was reported to be due to grain
boundary sliding at high temperatures resulting from softening of the grain
boundary phase. 55

Although the cyclic fatigue of ceramics has been thought to be caused

by the accumulation of ti.Jre-dependent crack growth, recent research on cyclic
fatigue of toughened ceramics has indicated that cyclic stress increases the
crack propagation rate. The rrechanism of cyclic fatigue crack growth can be
classified into two types. 44 One is an intrinsic rrechanism which causes
damage in the region near the crack tip, and the other is an extrinsic
rrechanism such as the crushing of grains at the crack interface where stress
is transferred. Kishirroto et al. 36 ,56-58 examined the crack velocity of
sintered silicon nitride under various stress ratios. They reported that the
crack velocity was significantly greater in the low Krrrax region when the
stress ratio was low. They concluded that an increase in the crack growth
rate was reflected by the acceleration of stress corrosion cracking due to
chemical activation of the crack tip by cyclic stress. In the fracture
surface experiencing cyclic stress, debris fracture was reported to result
from cyclic contacts of asperity along the crack interface. 56 Increased
crack extension in silicon nitride under cyclic loads was reported for a test
of crack extension from an indentation flaw. The cyclic stress was found to
extend the crack at a low stress level, whereas a static load caused
virtually no crack propagation. Dauskadt et al. 43, 44 examined the fatigue
crack growth behavior of transfonnation-toughened zirconia. They reported
that the velocity was governed by the stress intensity range, and that the
rreasured m value was 24. This value was much greater than the value for
rretals, which is generally in a range of 2 to 4. They concluded that an
intrinsic rrechanism such as microcracking near the crack tip governed the
extension. Suresh et al. 59 - 64 reported that cyclic compression resulted in
crack propagation, and that crack extension occurred during unloading due to
non-linear defonnation in the vicinity of the crack tip. This compressive
crack extension slowed as the crack interface was filled with the debris
produced by the cyclic compression, while the velocity increased as the
debris was rerroved from the interface.

The results of a cyclic fatigue test using srrooth specirrens showed that
the application of cyclic stress led to a shorter lifetirre. Krolm et al. 65
conducted a four-point bending cyclic fatigue test of alumina, and found that
an increase in frequency resulted in a shorter lifeti.Jre. Shorter fatigue
life was also reported in push-pull tests of alumina than in static load
tests,66 where damage due to cyclic defonnation was thought to have occurred

442
because it was difficult to explain the results by the environmental stress
corrosion cracking mechanism. High temperature fatigue tests, however,
indicated that cyclic loads produced slower crack propagation than static
loads. Fett et al. 67 concluded a cyclic fatigue test of hot pressed silicon
nitride at 1200ce under four-point bending and reported that the specimen
life was ten times longer than the calculated lifetime based on time-
dependent crack growth. Reduction of the effective stress at the crack tip
due to the adhesive force resulting from the grain boundary glassy phase at
high temperatures was thought to be responsible for the results. Horibe 68
performed a cyclic fatigue test of sintered silicon nitride, and found that
the fatigue strength under a stress ratio of R = -1 was lower than that of
static loading in the region of stress cycles greater than 103 cycles. He
observed surface spalling in the failure origin, and proposed the following
m::x:iel for crack generation under cyclic stress. Debonded particles were
trapped in the pre-existing surface flaw and produced a plastic deformation
zone surrounding the crack when compression stress was applied; a lateral
crack was generated during unloading. M3.suda et al. 69 conducted a push-pull
fatigue test of sintered silicon nitride, and reported that strength in the
fatigue test of R = -1 was significantly lower than that in a static fatigue
test. Their proposed mechanism at room temperature was the accumulation of
microcracking and the coalescence of a nain crack with grain boundary
microcracks. On the other hand, they also proposed a mechanism of crack
healing due to coopression for cyclic fatigue at high temperatures. They
reported that the fatigue behavior at 800ce with R = 0.5 coincided with an
estination nade from static fatigue data while cases of R = 0 and R = -1 led
to a shorter lifetime than expected. At 1000ce with R = -1, fatigue lifetime
became shorter with increasing frequency. This result was consistent with
the study done by Fett et al. 67 Takatsu et al. 70 reported the results of a
fatigue test for a variety of sintered silicon nitrides at frequencies of 250
Hz and 550 Hz. They concluded that a greater KC value for silicon nitride
resulted in a higher rate of cyclic fatigue crack growth.

In an effort to reduce scattering in the fatigue strength of ceramics

reflecting large scatter of fast fracture strength, tests have been conducted
using specimens with indention flaws. A cyclic fatigue test of sintered
silicon nitride having Vicker's indentation flaws was conducted at a load of
9.8 N and a frequency of 10 Hz, which was chosen because a higher frequency
resulted in greater scatter in the time to failure. 71 Analytical results of
the static fatigue behavior were consistent with cyclic fatigue data obtained
under stress higher than 460 MPa, while tests conducted under stress lower
than 420 MPa led to a shorter lifetime than expected. Reactivation of a
crack arrested under static loading was proposed for the mechanism of fatigue
crack growth. Yanauchi et al. 72 reported a cyclic fatigue test of hot
pressed silicon nitride having Knoop indentation flaws. With a Knoop
indentation load of 49 N, a narrow distribution of fatigue strength was
achieved, and an n value of 40 was obtained under a stress ratio of R = O.
It should be noted that this n value was much snaller than the value of n =
85, which was obtained from a fatigue test of R = 0 using specimens that had
survived proof testing. 72 Residual stress generation during indentation and
a surface flaw dimension greater than that of a natural flaw were proposed to
explain the inconsistency.

Niwa et al. 73 examined the effect of crack dimensions on cyclic fatigue

behavior. They reported that the relationship between the naximum stress and
the effective time to failure for smooth specimens was independent of
frequency. However, fatigue behavior for specimens having a Vicker sI

indentation flaw with a dimension of 180 ~, from which residual stress was
relieved, differed from that observed in static loading. The cyclic fatigue
behavior exhibited a reverse S-shaped fatigue curve, and an n value of 27 was

443
reported for R = 0.1 and f = 10 Hz. From plots of the data obtained for
fatigue strength versus the cycle number, it was observed that crack
propagation was governed by the cycle number. FurtheLmJre, small cracks were
concluded to have a negligible effect on accelerating the cyclic fatigue
crack growth velocity compared with static fatigue behavior for crack
dimensions of 40 jlm and 20 jlm.

ANALYSIS OF FATIGUE CRACK PROPAGATION IN CERAMICS

As described in previous section, it has been observed that the cycle

number governs crack growth behavior in toughened ceramics. Considering that
the toughening of ceramics is achieved through stress transfer at the crack
interface resulting in a reduction of the stress field near the crack tip,
the effective stress intensity at the crack tip, Kt, which virtually governs
crack propagation, is lower than the applied stress intensity factor Ka.
Accordingly, the crack tip stress intensity, Kt, can be expressed as follows:

(6)

where ~s is the additional stress intensity due to stress transfer at the

crack interface. Fast fracture then occurs when Kt reaches Ktc:

Ktc = KR - ~sc (7)

where KR is crack growth resistance depending on the extent of crack advance,

and ~sc is the critical value for the additional stress intensity when fast
fracture occurs. Assuming that ~s is proportional to Ka, the following
expressions are derived:

~s = ~sc (KaIKR) for Ka ~ ~l (8a)

~s = ~sc (Kcl/KpJ for Ka < Kcl (Bb)

where Kcl is the stress intensity at which crack closure occurs. Therefore,
Ktcanbe expressed as

Kt = Ka (1 - ~Ksc/KR) for Ka ~ ~l (9a)

Kt = Kcl (1 - ~scIKR) for Ka < Kcl (9b)

Provided that the crack growth velocity under the cyclic stress depends
on both time and the cycle number, the following expression can be derived

cia I dt = (oalot) + f (oaloN) (10)

where f is the frequency of the cyclic stress. Considering the contribution
of stress transfer at the crack interface, the equation for crack propagation
should be rewritten by using the crack tip stress intensity:

(11)

(12)

where ~t = Ktnax - Ktrnin.

444
 In the case of sinusoidal stress, Ka is given by

Ka = [(1 + R) + (1 - R) sin (21tft)] ~ / 2 (13)

where R = ~ / ~.

Substituting Eq. (13) into Eq. (11) and rearranging the result leads to
an expression for an average crack growth velocity in a single stress cycle,
<iJa/dt>:

(14)

Q = .1.
1t
[f8' (~)n
K max
d() + f."12 (~)n d()]
• K max
- n/2 e

where sin ()* = [2R' - (1 + R)] / (1 - R) for ~ > Kel >~, ()* = - 1t/2
for ~ ~ Kel, and ()* = 1t/2 for Kel ~~. Here, R' = Kel / ~.
Similarly, Eq. (12) yields

(15)

where n= (1 - for ~ > Kel > ~, n= (1 - for ~ ~ Kel, and

°for Kel
R,)m R)m

n= ~ ~.

RESULTS AND DISCUSSION

Assuming that fatigue crack growth can be expressed as Eqs. (14) and
(15), the slope obtained from plots of log v against log (~/KR) coincides
with the n value for the case that da/dt » f(da/dN) with a constant Q value.
Figure 1 shows the Q value against Kel/~ for n = 80. The Q value rapidly

0.9 for the case of R = °

decreases with a smaller R' to reach a constant value in the region of R' <
and R = -1. This indicates that the crack closure
has a negligible influence on the time-dependent crack growth rate when ~
is much greater than Kel. Figure 2 shows the constant value of Q against R
for a variety of n values. As the value of n increases, the constant value
of Q decreases. When a fatigue test is conducted under a constant stress
ratio, the n value is constant when ~ > Kel or Kel >~. Therefore, the
slope obtained from the relationship between log v and log (~/KR)
coincides with the value of m when f(da/dN) »da/dt except for the case of
~ < Kel <~. Consequently, when Kel < %n, the slopes in the regions of
da/dt » f(da/dN) and of da/dt « f(da/dN) give n and m, respectively. Figure
3 shows a sample calculation of the fatigue crack growth for a variety of
frequencies, where m = 20, n = 80, Vs = O.Ol/KRn, Vc = O.OOl/K~, Kel = 0, and
R=O.l.

Figure 4 shows the relationship between log v and log (~/KR) for
various values of Kel in the region of %n < Kel < ~, where R = -1, m =
20, n = 80, Vs = O.Ol/KRn , Vc = O.OOl/KRm, f = 0.1 Hz, R' = 0, 0.25, 0.5, and
0.75, An increase in the value of Kel leads to an increase in the crack
growth velocity in the region of da/dt « f(da/dN) , while no influence is
observed in the region of aa/at »f(aa/aN) as preViously described.

445
 1.0
R = 1

0.8

Q)
:l
.-i
0.6 -
I1l
:>
01
0.4

0.2 - R
=~1=\ J
I
0.0
0.0 0.2 0.4 0.6 0.8 1.0

R' value
Figure 1. Q values vs. R' values for n = 80 and various R values.

1.0

Q)
:l
0.8
.-i
I1l
:>
0.6
01 n = 20
+J
c:
I1l 0.4
+J
Ul
c:
0
u 0.2

0.0
-1.0 -0.5 0.0 0.5 1.0
R value
Figure 2. Constant Q values vs. stress ratio, R, for various n values.

446
 -4
C/l
....... -6
E

:::. -8
0'>
0
.-l
-10 f
,
>0
.IJ
.,-i -12
u f
0
.-l
Q) -14
>
0
~
u -16 0.01 Hz
co
~
u -18
-0.5 -0.4 -0.3 -0.2 -0.1 0.0

Applied stress intensity, log (Krnax /KR)

Figure 3. calculation of the fatigue crack velocity for a variety of
frequencies, according to Eqs. (10-15) where m = 20, n = 80,
Vs = 0.01/J<Kl, Vc = O.OOl/Rifl, KCl = 0, and R = 0.1.

-4
C/l
.......
E
-6
:::.
0'>
0 -8
.-l
,
>0
.IJ -10
.,-i
U
0
.-l
Q)
-12
>
~
u -14
co
u
~ 0.75
-16
-0.5 -0.4 -0.3 -0.2 -0.1 0.0

Applied stress intensity, log (Krnax /K~

Figure 4. Relationship between log v and log (~/~) for various values of
KCl. calculation was nade for R = -1, m = 20, n = 80,
Vs = O.Ol/~n, Vc = O.OOl/~m, f = 0.1 Hz, R' = 0, 0.25, 0.5, and
0.75.

447
 The value of KCl was reported to be given as a function of the stress
ratio for aluminum alloys.74 In ceramics, however, the cyclic contact at the
crack interface during unloading and application of compression results in
crushing of the asperity. Consequently, an increase in the compressive
stress accompanying a number of cyclic contacts would lead to a decrease in
KCl. Figure 5 shows the plots of KCl against ~ for silicon nitride
obtained from the report by Kishimoto et ai. 36 Although the effect of the
cycle number is excluded from the consideration, the relationship indicates
that the value of KCl increases with an increase in ~ for a positive value
of ~, while the KCl value remains constant for a negative~. The
following relationship can therefore be derived.

KCl/KC = 0.18 for ~ :5 a (16a)

KCl/KC = 0.18 + 0.8 ~/KC for ~ > a (16b)

It is noteworthy that KCl ~ ~, which indicates that the crack velocity in

the region of da/dt » f(da/dN) is governed by ~/KC independent of the
frequency and the KCl value, while the crack velocity in the region of daldt
« f(daldN) is accelerated by an increase in the frequency and a decrease in
the KCl value.

Furtherrrore, considering the decrease in the KCl value due to an

increase in the cycle number, the effect of overloading on crack extension
can be evaluated. Crack velocity just after rapid crack extension due to
overloading would decrease because the KCl value is large, and further
application of cyclic stress to the crack would cause a gradual increase in
the crack velocity due to a decrease in the KCl value. This analysis is
consistent with the results of an experimental study done on Mg-PSZ having
peak toughness. 44

The analytical result described above was normalized by the I<R value.
However, as a crack advances, an increase in the area of the crack interface
contributing to the stress transfer results in an increase in the value of
I\R. It should be noted that an increase in the KR value also occurs during
the failure process due to crack extension from a natural flaw. An increase
in the value of M sc as an indication of crack advance can be approximated as

for 0 < ~a < ~asat (17a)

for ~a ~ ~asat (17b)

where Msat is the maximum value of M sc ' ~asat is the maximum distance from
the crack tip contributing to the stress transfer, and b is a parameter for
determining the shape of the R-curve. In general, b > 1 for a straight
through crack whereas a chevron notch gives an apparent b value near 1 with
~asat approaching infinity. It should be noted that crack propagation
behavior from a natural flaw is similar to that from a chevron notch because
an extension of a crack from a natural flaw leads to expansion of the front
length of the crack.

The relationship between log v and log ~ for toughened ceramics

exhibiting a steep R-curve can change depending on the measuring method used.
When crack propagation is measured from a small Kr region to a large Kr
region for crack advance such as crack propagation from a natural flaw, the

448
 0.6

~ 0.5
.......
.....
~ 0.4
~

Q)
~
~ 0.3

••
CIl
0
.-l
u 0.2
~
u
ro .-...
••
.~
....
u
l-l
0.1 •
0.0
-2 -1 a 1

Minimum applied stress intensity, Kmin/Kc

Figure 5. Plots of KCl against J<min for silicon nitride reported by

Kishimoto et al. 36 The value of KCl increases with an increase in
J<min for a positive value of J<min while KCl remains constant for a
negative value of J<min.

>,
~ U
·rl
CIl ~
h <]
................................... --- --- --- .... _..... ----- Static

.,
Q)
oW l-l
" /1K static
h
....
Q)
·rl
CIl
sat
CIl h
CIl ro cyclic
Q) l-l /1K
~ oW sat
oW
CIl CIl
CIl
C clic
r4 Q)
ro ~
h oW
0 CIl
cyclic
·rl static
oW 0 /1a /1a
·rl oW sat sat
11 I
"0
"0 Q)
~ ~
"0

Crack advance, /1a

Figure 6. Schematic comparison of R-curves under static and cyclic crack

growth. The reduction in M sat and /1a sa t occurs as a result of
cyclic contact at the crack interface.

449
 ,
:>.
.jJ
.,-i
u
o
.-l
(j)
::-
..I<:
u
11l
~
U
Intrinsic effect
of cyclic fatigue

Applied stress intensity, log Kmax

Figure 7. Schematic indication of Rmax versus fatigue crack growth velocity

under static and cyclic loads.

effect
fatigue

Time to failure, log t

Figure 8. Relationship between ~ and time to failure calculated from the
v-K relationship in Figure 7.

450
slope should be gradual and can even be negative. On the other hand, a steep
slope should be obtained when measured from the high Kr region to the low Kr
region as a crack advances. A negative n value was obtained from propagation
of a small crack in a measurement of static crack growth for Mg-PSZ,75 while
a large n value of 95 was obtained for the same material using an applied
rroment double cantilever beam technique.

Cyclic fatigue crack extension comprises intrinsic crack growth

dependent on Mt and the extrinsic effect on crack propagation as a result of
a decrease in Msc . The latter effect accelerates time-dependent subcritical
crack growth. Because the extrinsic contribution to cyclic fatigue crack
growth is caused by the fracture of the asperity at the crack interface,
application of cyclic stress would result in a decrease in both M sat and
6asat. Figure 6 shows a schematic cooparison of R-curves between static and
cyclic crack growth. A reduction in Msat and 6asat would occur with an
increase in the cycle number and a decrease in the stress ratio. Figure 7
shows a schematic indication of the Fm:tx versus v curve under static and
cyclic loads. The crack velocity under cyclic loads is greater due to the
intrinsic effect which decreases the value of M sCt while no change occurs in
the slope in the comparison nade for crack velocity under static loads. The
intrinsic effect gives the v-Fm:tx curve a different slope in the region of
low stress intensity. The presence of the extrinsic effect was suggested by
measurements for silicon nitride, which showed a rronotonic increase in the
crack velocity in the region of daldt » f(daldN) .36,56,57

Figure 8 shows a schematic indication of the relationship between ~

and the time to failure calculated from the v-K relationship presented in
Figure 7. In the region of high applied stress, the slope is gradual with a
gradient of -lin because the mechanism governing crack propagation is time-
dependent crack growth, while the slope in the region of low stress is -11m
and is governed by cycle-number-dependent crack growth. It is noted that the
extrinsic effect shortens the time to failure and an increase in the
frequency results in a further shortening of the time to failure in the
region of low stress. According to a cooparison made of the shortening of
the time to failure due to cyclic loads and that due to static loading at the
same amplitUde of the naximum stress for alumina, 66 a sudden drop in strength
occurred in the range of 3,000 to 30,000 cycles in a push-pull test under 10
Hz, while the strength change was insignificant in the region of less than
3,000 cycles and in the region over 30,000 cycles. This may suggest that a
change in governing effect occurs at 3,000 cycles from time-dependent to
cycle-number-dependent crack growth. Although the reason for the slope
change in the region near 30,000 cycles remains unclear, it may correspond to
the fatigue limit. Such a reverse S-shaped curve of ~ versus t c was also
reported for silicon nitride, in which the reverse S-shaped fatigue curve due
to a sudden decrease in fatigue strength occurred in a four-point bending
fatigue test 69 of R = 0 and in a test using C-type specimens. 68

While it has been pointed out that cyclic fatigue crack growth was
accelerated in the case of large crack dimensions,73 the role of cyclic
fatigue crack growth is important in predicting failure. This is because
some toughened ceramics having no artificially induced cracks exhibit the
characteristics of cyclic fatigue such as a reverse S-shaped cyclic fatigue
curve, and a significant strength degradation caused by the application of
cyclic stress. The occurrence of cyclic fatigue crack growth in the low
stress region may be attributed to the fact that the crack length responsible
for the long lifetime is large. Analytical results suggest that failure
predictions based on subcritical crack growth may lead to unreliable

451
estimations when cycle-number-dependent crack growth occurs. Thus, it is
essential to take into account the effect of cyclic fatigue crack growth in
order to obtain reliable lifetime predictions.

CONCLUSIONS

Failure prediction of toughened ceramics under cyclic loads was

analyzed. Crack propagation was assumed to be governed by both time-
dependent and cycle-number-dependent terms as a function of crack tip stress
intensity.

The analytical results indicated that time-dependent crack propagation

virtually governed the region of high stress intensity, and that cyclic loads
increased the growth rate as a result of the crushing of grains at the crack
interface where the stress was transferred, thereby shielding the crack tip
stress field from the applied stress. The intrinsic effect on cycle-number-
dependent crack propagation was shown to govern the region of low stress
intensity, where increasing the frequency of the applied stress and
decreasing the stress intensity at crack closure increased the crack
propagation rate. These results were consistent with experimental data.

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454
TENSILE FATIGUE CRACK GROWTH OF

POLYCRYSTALLINE MAGNESIA

Takeshi Ogawa

Department of Mechanical Engineering

Gifu University,
1-1 Yanagido, 501-11 Gifu, Japan

ABSTRACT
Fatigue crack growth in polycrystalline magnesia has been investigated at room
temperature using a combined loading technique, in which a compressive load is
applied to the uncracked ligament of the compact specimen in order to stabilize the
crack growth. Mcasurcment of the crack length is performed continuously by a surface
film tcchnique, in which changes in crack length are monitored by a thin layer of
carbon on a surface area which encompasses the region of fracture. The propagation
of a crack leads to a break in the carbon film which is atomically bonded to the
surface of the specimen. The crack advances in a stable manner under cyclic tension
with the maximulll stress intensity factor K max lower than the maximum fracture
toughness K cs . Initially, the growth occurred in each cycle, however, it later became
discontinuous. The continuow; monitoring of the crack length revealed that the crack
grew quickly in a single cycle at K max over several tens of microns and became arrested
until the ncxt growth occurred. Based on the experimental results of the crack growth
and thc fracturc surface observation, a mechanism for fatigue crack growth in terms
of wake effects is discussed.

INTRODUCTION

Fracture mechanics has been applied to the crack growth characterization in ce-
ramics under monotonic and cyclic loading conditions. Recently, the evidence for
fatigue crack growth in ceramics under cyclic loading has been provided at room
temperature,I-4 where limited plasticity exists. It is significant to investigate the
effect of cyclic loading on the crack growth behavior for engineering applications.
However, experimental data are limited because ceramics are so brittle that the con-
ventional techniques developed for fatigue experiment in metals arc not applicable.

Crack growth control and crack length measurement are the major difficulties
for crack growth experiment of brittle materials. In order to test crack growth in
ceramics under cyclic loading, it is difficult to obtain stahle crack growth condition,
because the cracks grow in an unstable manner with a sIIlall increase of crack driving
force. Experimental tecllIliqucs to stabilize crack growth could be classified into three
categories involving (i) rigid fixed grip, (ii) specimen geometry and (iii) combined
loading. Method (i) is not suitable for the experiment under cyclic loading. The use
of tapered DCB specimen cnables the crack to be stabilized by the method (ii), but
the specimens are expensivc. Method (iii) has the possibility to investigate the char-
acteristics of stable nack growth under cyelic loading in britt.le materials. Another
experimental difficulty is to measurc crack length, because the crack tip location is

FrQt:llUe Mechanics of Ceramics. Vol. 9

Edited by R.C. Bradt el aI.• Plenum Press. New York, 1992 455
obscure due to the limited amount of plasticity at the crack tip. The author has
developed a indirect method to measure the crack length in ceramics,5 which enables
continuous monitoring of crack length during cyclic loading.

In the present stuJy, fatigue crack growth has been investigateJ using the com-
bined loading technique for stabilizing crack growth and surface film technique for
monitoring crack length. Fractographic observations are performed using scanning
electron microscope (SEM) with the aiJ of image processing, which enables the three
dimensional observation using a stereo pair of SEM micrographs. Based on these
results, the crack growth medmnism in terms of a wake effect of fatigue cracks and
the role of cyclic loading in the crack growth of ceramics are discusseJ.

MATERIAL AND EXPERIMENTAL PROCEDURES

The material investigated in this study is a polycrystalline magnesium oxide,
MgO, which is commercially available from Custom Technical Ceramics, Arvada,
ColoraJo. The main impurity added as sintering aid is 2.3% yttria (Y 2 0 3 ). The
sintering temperature is 1560°C. The material properties provided by the supplier
are as follows: flexural strength=227 MPa, Young's modulus=258 GPa, grain size=2
Ilm( 60%), 6"'-'8 lun( 40%), Jensity=3.40 g/cm 3 .

Crack length was monitored successively by the surface film technique which is
described in detail clsewhere. 5 In this method, changes in crack length in ceramics are
monitored by sputter-depositing a layer of carbon on a surface area which encompasses
the region of fracture. The propagation of a crack in the ceramic leads to a break in
the carbon film which is atomically bonded to the surface of the solid. The carbon
layer is connecteJ to an electrical cireuit where an increase in crack lcngth is reflected
as a change in the electrical voltage. Detailed calibration and evaluation are given in
the literature. 5

Quasi-static crack growth experiments were performed to evaluate the fracture

resistance curve (R-cnrve) in a screw-driven test machine on both compact type (CT)
specimens and single edgc notched (SEN) specimcns. The specimen dimensions were:
CT - width, W =25 nun, thickness, B=5 mm, height, H =30 nun and notch length
a ll =I1.6 mm, SEN - ~V=lO mm, B=5 mm, H=50 lIun and a ll =4 mm. For the SEN
spccimcns, three types of loading systems werc chosen, i.e. uniaxial tension (SENT)
by pin loading with holes machined near the ends of SEN specimen, 3 point bending
(3PB) with a span of 40 lIun and 4 point bending (4PB) with an outer span of 40
nun and an inner span of 20 mm. The specimens were loaded in an uniaxial cyclic
compression to introduce a mode I fatigue precrack. 6 Then quasi-static tensile load
was applied to the specimens under stroke control with the displacement rate of 2.54
11m/min.

Tensile fatigue testing was done in a servo-hydraulic testing machine under load
control with cyclic frequency f of 0.1 Hz on a CT specimen with W=25 mm, B=5
mm, H =30 lIun and an =9 mm, which wa.'i precracked in cyclic compression. In this
experiment, a combined loading technique was used to stabilize crack growth. When
a compressive load P emp is applied to the ligament of a CT specimen together with a
tensile load PIn .• to the loading pins, stress intensity factor K can be analyzed by the
superposition principle as shown in Fig.l, and is expressed as;

K = KIllS - Kemp (1)

KIllS = ::;WFllIs((a/W)li p) (2)

Kemp = Pe~Femp((a/W)liP,(l/W)ernp) (3)

BvW
where (a/W)lip and (l/W)emp are normalized crack length and compression location,
respectively. The stress intensity factor, KIllS, due to the tensile load is given in

456
Srawley.7 While Kemp-calibration has not been obtained, Femp values are determined
by the finite element method using the commercially available code ABAQUS. 8 De-
tails of the calibration are shown in APPENDIX. Fem was applied statically using a
C-shape clamp equipped with a load cell. For the tensife fatigue experiment, the max-
imum load P",ax (= PIns in Eq.(2)) and P emp values were chosen so that maximum
stress intensity factor K max was approximately constant with crack growth. The
relationship between the tensile load ratio R p (= P min / P max ) and stress intensity
factor ratio Rs Ifi- is expressed by the following equation

(4)

where P min and Kmin are minimum load and minimum stress intensify factor, re-
spectively. The tensile fatigue experiments were performed under constant Rp value
of 0.1, thus RSf fi' value decreased with the crack growth.

RESULTS
Crack Growth 'Under Monotonic Loading

The crack growth resistance curves (R-curves) obtained for CT, SENT, 3PB and
4PB are shown in Fig.2. Rising R-curves are observed for all cases, and they depend
strongly on the specimen gcometry and loading system. CT has the largest stable
crack growth before instability occurs. For the SEN specimens, SENT has 3 times
larger stable crack growth than 3PB or 4PB do. These results indicate that the
R-curve increases more rapidly when the stress gradient in the specimen is larger.
This anomalous behavior is controlled by the cohesive stress in the wake of crack tip.
Details of the investigation of this behavior is shown elsewhere. 9 Unstable fast fracture
initiated at the samc stress intensity factor of 2 MPaJill regardless of the specimen
geometry and loading system. This value corresponds to the saturated condition of
the wake effect, thcn it is evaluated as saturated fracturc toughness K es .

Crack Growth 'under Cyclic Loading

The crack growth bchavior under cyclic tension loading was investigated using
the combined loading technique to facilitate the observation of crack growth. The
compressive load was applied for the ligamcnt at (l/W)cmp of 0.7 with P cmp / PIns of
4.2, which resulted in approximately constant K max value of 1.7 MPaJill regardless
of the crack growth. Figure 3 shows the relationship between K and ~a under cyclic
tension loading. In thc first cycle, the crack grows on the R-cll1've up to ~a=0.45

Pins Pcmp

(a/W) lip

o
+ o

Fig. 1 Superposition principle to analyze the stress intensity factor 1D combined

loading technique.

457
mm. The crack grows continuously until t:.a=0.6 mm, followed by a discontinuous
growth behavior involving arrest for several cycles and intermittent growth. Figure
4 is an example of the 'relationship between K and t:.a during the number of cycles
N between 65 and 75 cycles showing the discontinuous crack growth. It is important
to note that the crack grows abruptly over t:.a=40 Jim around K =Kmax in a single
cycle of N =70, and is dormant in the remaining cycles.

Another important implication of the continuous monitoring of crack length is

crack closure behaviour. Decrease in t:.a for the surface film technique corresponds
to the decrease in resistance of the surface film, which indicates the physical contact
between the crack faces on the side surface of the specimen. Thus, the closure stress
intensity factor KcI is evaluated by a K value below whicht:.a decreases and is about
0.8 MPaJffi in the case of FigA. The significance of crack closure in tensile fatigue
crack growth in ceramics has been demonstrated by Kishimoto et aI. I and Tanaka

2.5

~
'"
c..
:>: 2.0

'"' 1.5

~
>, 0 CT
'"<: 1.0 /),.
SENT
'"
.....
c
0 3PB

..'"
'"'"
.....
Vl
0.5 0 4PB

0.0
0.0 0.1 0.2 0.3 0.4 0.5 0.6

Crack extension lla mm

Fig. 2 R-curves for different specimen geometry and loading system.

2.0
f = 0.1 Hz
..
ll;:
~ 1.5

'"' 1.0

.....>,
'"c 0.5
2c
1\
N ~ 0 - 40 cycles
'"'" 0
.....'"
L
Vl

-0.5 +---,----,------r--.---..,......--.----.--j
o 0.1 0.2 0.3 0.4 0.5 0.6 0.7 O.B
Crack ex tens ion
"'"
Fig. 3 The relationship between K and t:.a showing the crack growth behavior
under cyclic tension loading.

458
et al. 2 based on back face strain (BFS) method. However, the measured K cI has a
different meaning between BFS method and the present investigation. As mentioned
above, physical contact of the original crack faces is detected in surface film technique,
while the non-linear stress-strain response induced by the contact stress in the wake
of crack tip in BFS method.

The relationship between 6a and N is plotted in Fig.5, showing the character-

istics of arrest and intermittent crack growth. Each plot represents the ~a value of
each one cycle. This figure also present the minimum ~a value, ~amin obtained by
surface film technique in each cycle. The difference between 6a and 6a m in may cor-
respond to the significance of crack closure and increases with increasing Nand/or
6a.

It is also seen in Fig.5 that the number of cycles between intermittent crack
growth increases with increasing N. Similar growth behavior continued until fla

l.l;;
'"
a..
xc 1.5- fb~CSi
CtJ~ DC
oDJ Ei ClcCOJ
"" 1.0- cP 83J OJ§Jo

ocPCbBJ §qjo
...
>,

CSJB=bo
0.5 - ~ClJ
...'"'"
c:
c: Des s:m cmCID 0
'"'" 0
On; ldn
...'"
I-

V'l 13m 0 COO c:QJo

o~o
-0.5 § DO
I I
~~
I
0.68 0.70 0.72 0.74 0.76
Crack extension Aa rrm

Fig. 4 Magnified plot of Fig.3 showing the discontinuous crack growth and crack
closure.

0.8-r----------------------,

·i 0.7
'"
.
<3

'"
<3

c:
0.6
o
'"c:
~
o lla
~ 0.5 , • llamin
'"I-
U

0.4 +--r--,---r-...,--,-----,---r-,---,---i
o 20 40 60 80 100
Number of cycles II

Fig. 5 a vs. N plot showing intermittent crack growth and the closure response in
surface film tedlilique.

459
became 1 nun at N of 700 cycles, then the crack arrested completely. Because of this
anomalous crack growth, the growth rate, da/ dN depends strongly on its definition.
When da/dN is defined for one cycle, it is either a few tens of 11m/cycle or zero.
In many of the literature, da/ dN is defined as an average crack growth rate over a
number of cycles, which can conceal the discontinuous crack growth behavior. K max
value is maintained constant in the present experiment (Rs I F is slightly decreased,
and thus stress intensity factor range 6.f{ increased, cr. Eq. (4)), however, da/ dN
attains a wide range of valucs. Therefore, the conventional fracture mechanics plot
of da/ dN vs. K max or 6.K can not characterize the tensile fatiguc crack growth in
the prcsent expcriment.

Fraetography

Fractographic observations were performed using scanning electron microscope

(SEM) with the aid of image processing. Figure 6(a) shows debris formed on the frac-

Crack growth direction

..

View

Fig. 6 Fractographic observation by SEM on the fracture surface where crack has
grown discontinuously. (a) SEM image. (b) Topographic feature recon-
structed based on stcreo matching t,echnique.

460
ture surface where the tensile fatigue crack lias grown discontinuously. Based on the
stereo matching teclllliqllc, the topop;raphic feature of the fracture surface is analyzed
by using a digital image processing systcm, which investigates the corresponding loca-
tions of a sterco pail' of SEM images and reconstructs the 3-dimensional expression. 10
Figure 6(b) is the three dimensional appearance from the "view" shown in Fig.6(a).
These figures reveal that debris is formed from a break down of asperity and it accu-
mulates in the valley on thc fracture surface. This appearance is frequently seen in
thc discontinuous crack growth region, however, debris is hardly seen in the region
where the crack has grown in the first cycle. This region corresponds to crack growth
under monotonic loading. Similarly, Kishimoto et al. reported debris formation on
the fracture surface where tcnsile fatip;ue crack had grown for silicon nitride. I Except
the existence of debris, transgranular fracture is dominating in all the regions and no
significant differencc in fracture mechanism is seen.

DISCUSSION
The rising R-curves caused by the wake effect would be expressed by the following
expressIOn;
K u = K;nt + Kwake (5)
K wake = F(D wk )
(6)
where K R is the crack growth resistance of a material, K jnt is an intrinsic fracture
toughness, K wake is the shielding of the wake effect and D wk is an area where wake
effect occurs. Schcmatic illustration of this model is shown in Fig.7. Under monotonic
loading, Dwk equals crack extension ~a. If toughening does not increase in front of
crack tip with crack growth, K int is considered to be constant for the material tested.
However, F(D wk ) may <lepend strongly on specimen geometry and loading system,
and leads to the depcndence of R-curve on those factors, as shown in Fig.2.

From the experimental results, the mechanism of intermittent crack growth under
cyclic loading can be explained as follows. In the first cycle, the crack grows on
the monotonic R-curve according to the Eqs.(5) and (6), where D wk corresponds to
~a. However, because of a higher loading rate than the quasi-static experiment, ~a
may be smaller than D wk in the first cycle. Thus, in the following continuous crack
growth regime( N =2", 10 cycle, ~a=0.45", 0.6 mm), ~a approaches D wk and the crack
becomes dormant for several cycles. Cyclic loading develops a fretting damage in the
wake of crack tip, as schematically illustrated in Fig.8, and causes a micro-fracture
of asperity. The micro-fra.cture produces debris, as is seen in Fi/!;.6, and releases the
shielding strcss in t.he wake, which is expressed by the decrea.se of !{wake due to the
decrease of D wk . Thcn t.hc crack grows abruptly to compensate K wake so that Kil
cqllilibrates to K rrwx in the cyclic loads. This behavior is expressed schematically in
Fig.7.

R-curve
Asperity fracture

Q)
u
C
«l
.~
en
Q)
a:

Fig. 7 Wake tOllghening model for R-curvc and fatigue crack growth.

461
 t ~
Toughening

t
Frictional
stress
~

Crack tip

Micro·fracture of
(a) K=Kmax
t t t

Debris induced crack closure Roughness induced crack closure

(b) K=O

Fig. 8 Schematic illustration of tensile fatigue crack growth mechanism due to the
fretting damage in the wake of crack tip.

CONCLUSIONS
It has been demonstrated that cracks grow in a stable manner under cyclic load-
ing in polycrystalline magnesia. Based on the continuous crack growth monitoring
and fractographic observation, it is suggested that the fatigue crack growth has the
same mechanism with the crack growth on the monotonic R-curve except the fretting
damage in the wake region. Similar fatigue crack growth mechanism is predicted for
the other ceramics and ceramic composite whose wake effect is significant.

Acknowledgements - This work was performed at Brown University. The author

thanks Prof. Suresh for invaluable discussions and Murata Machinery Co., Japan, for
providing a fellowship which sponsored his visiting appointment at Brown University.

REFERENCES
1. H. Kishimoto, A. Ueno and H. Kawamoto, Proc. Fatigue 90, 2:727(1990).
2. T. Tanaka, N. Okahe and y. Ishimaru, J. Soc. Mat. Sci., Japan, 38:137(1989),
in Japanese.
3. S. Horibe, Proc. Fatigue 90, 2:753(1990).
4. L.A. Sylva and S. Surcsh, J. Mat. Sci., 24:1729(1989).
5. T. Ogawa and S. Suresh, Engng Fracture Mech., in press.
6. L. Ewart and S. Suresh, J. Mat. Sci., 22: 1173(1987).
7. J.E. Srawlcy, Int. J. Fract., 12:454(1976).
8. ABAQUS User's Manual, Version 4.7, Hibbit, Karlson and Sorensen Inc., Provi-
dence (1988).
9. J. LLorca and T. Ogawa, Fract. Mech. Ceram., 9-10:(1991).
10. T. Ogawa and K. Tokaji, Trans. Japan Soc. Mech. Eng., 54A:2188(1988), in
Japanese.

462
 Table AI. Coefficients Bi,j of Eq.(A2)

Bi,O Bi,1 B i,2 B i ,3 Bi,4

0 9.78566 -11.8148 6.2779 -10.3469 5.39516

1 -70.9308 37.9321 -50.4234 212.751 -128.751

2 331.718 -130.84 -250.866 -186.347 226.735

3 -596.871 229.66 923.012 -615.989 71.6484

4 431.353 -221.916 -690.502 687.761 -213.385

APPENDIX
The Fcrnp values in Eq.(3) were determined by finite element method using
ABAQUS. The mesh uscd for this calculation consists of 8 nodes, isoparametric ele-
mcnts. The total number of nodes and elements are 937 and 288, respectively. Fig.Al
shows the variation of Fcrnp value as a function of both (a/W)ti and (1 /W)crnp. Solid
lines are calculated by the following equat,ions determined by the least squire method
of the FEM results.

Coefficients Aj(i = 0 '" 4) are expressed as:

The coefficients Bi,j( i, j =0"'4) are given in Table Al with an accuracy of better than
0.5%. Fcrnp values were also analyzed for distributed load with a width of 0.5W. Load
distribution has no effect on Fcrnp value, when the central (l/W)crnp is considered.

Fig.A2 shows the variation of normalized K value evaluated by the present anal-
ysis as a function of (a/W)tip for different Pcmp / Ptns and (l/W)cmp values. As shown
in this figure, it is feasible to have any kinds of change in K value with increasing
(a/W)tip using the combined loading technique.

25.0
(a/W)cmp
20.0 •... 0
0.25

15.0 T
• 0.5
0.75
0. • 1
E 10.0
u
u.
5.0

0.0

-5.0
0.3 0.4 0.5 0.6 0.7
(a/W)tiP
Fig.Al Fcrnp values determined by finite element method.

463
 25.0
(1/W)cmp = 0.6
20.0
lJ)
c
.....
0- 15.0

~
CO 10.0
~

5.0

0.04-----.r---""'----.-::::......--..------l
0.3 0.4 0.5 0.6 0.7
(a/Whip
(a) (l/W)cmp = 0.6.

25.0 - , - - - - - - - - - - - - - - - ,
(lfW)cmp = 0.7
20.0
lJ)

.....c 15.0
0-

~CO 10.0
~

6.0

0.0 +------,---~---~----::""---l
0.3 0.4 0.5 0.6 0.7
(a/Whip
(b) (l/W)cm/I = 0.7.

Fig.A2 Examples of the variations of normalized K as a function of (a/W)tip for

different Pcmp / Ptn. and (1 /W)cmp values.

464
FATIGUE BEHAVIOUR OF STRUCTURAL CERAMICS

Yukihiko Yamauchi, Tatsuki Ohji, Wataru Kanematsu,

Shoji Ito and Katsushi Kubo

Government Industrial Research Institute, Nagoya

I-I, Hirate-cho, Kita-ku, Nagoya, 462 Japan

Abstract
4-point bending static and cyclic fatigue tests are carried out on
several structural ceramics both at room and elevated temperatures.
Measured fatigue behaviours are compared with the lifetime predicted from
the dynamic fatigue properties and cyclic loading effects on delayed
failure are discussed. Experimental results indicate that a delayed
failure of ceramics under a cyclic loading is caused mainly by extension
of a pre-existed flaw and the lifetime is substantially predictable from
a subcritical crack growth behaviour estimated under a static or quasi-
static loading condition. It is also pointed out that at elevated tem-
peratures the crystallization of glassy phase at grain boundaries extends
the lifetime and that a crack growth is accelerated by compressive stress
if grain (cluster) bridgings and/or crack interlockings are formed on a
crack surface. Humidity controlled stress corrosion of a glassy phase at
grain boundaries and mechanical fracture through the grain boundaries due
to softening of the glassy phase are considered as main crack growth
mechanisms at room and elevated temperatures, respectively. From these
results it is concluded that the fatigue behaviour of ceramics is strong-
ly affected by the properties of grain boundaries.

Introduction

High performance ceramics is a promising structural material due to

its high strength at high temperatures and high corrosion resistance. A
prerequisite for the reliable use of ceramics in structural applications
is the understanding of its mechanical properties. In particular the
knowledge of the fatigue behaviour of ceramics is important with respect
to life time prediction of components. In this context a lot of reports
dealing with the fatigue properties of structural ceramics have been
presented 1 - 3 l> but the essential fatigue mechanism has not been under-
stood yet. The authors have studied on the subcritical crack growth
behaviours of several structural ceramics and a ceramic composite by
dynamic fatigue tests etc. 36-38.

In this paper static and cyclic fatigue behaviours of ceramics

both at room and elevated temperatures are studied. Measured fatigue
behaviours are compared with fatigue lives predicted from dynamic

Fracture Mechanics afCeramics, Vol. 9

Edited by R.C. Bradt et ai., Plenum Press, New York, 1992 465
fatigue properties and the effects of cyclic loadIng on delayed fail-
ure of ceramics are discussed.

Experimental procedure and lifetime prediction

Materials and specillen

The materials for this experiment are 3 kinds of silicon nitride and
2 silicon carbIde ceramics. Their chemical compositions and densities
are listed in Table 1. The sintering additives are N2: MgO, Ce02, SrO
and Zr02, N3: AbOs and Y20 S , Cl: AbOs and C2: Band C, respectively.
The bending strength and the fatigue parameters of the materials
estimated by dynamic fatigue tests S8 • ST are shown In Table 2.

Specimens are cut from sintered bodies made from the same batch
using a diamond blade of 0.5mm thickness and their surfaces are
ground parallel to the longitudinal direction by a diamond wheel of
mesh number 400 for silicon nitride ceramics or of mesh number 600 for
silicon carbide ceramics. The corners of all specimens are chamfered
by a diamond disk of mesh number 1000. The final shapes of the speci-
mens are shown in Fig.1.

Fatigue tests

4-point bending static or sinusoidal cyclic load is applied to a

specimen and time to failure Is measured. Outer and inner spans of the
4-point bend in the static and the pulsating fatIgue tests (tensIon-
tension cyclic loading) are 30mm and 10mm and those in the alternating
fatigue tests (tensIon-compression cyclic loading) are 130mm and 60mm,
respectively. The frequency of the cyclic load is 0.1 or 5Hz. The
stressing rate R, whIch is the rate of the applied minimum and maximum
stress U mt.n/U max, is 0.25 (pUlsating fatigue test) or -1 (alternating
fatigue test). Tests are conducted at a room temperature in an air and
at elevated temperatures up to 1500 C in a vacuum of less than 10- 4 Torr.
In the tests at elevated temperatures the testing system including upper
and lower molybdenum rods, the 4-point bending jig made of silicon car-
bide ceramics and the specimen is heated by a tungsten resistance heater
with a heating rate of 30°C/min. Before starting the test the system is
kept at the testing temperature for 1 hour to achieve a uniform tempera-
ture distribution. The tests are interrupted after around 10 6 sec. The
testing conditions are summarized in Table 3.

Lifeti.e prediction
To clarify cyclic loading effects on lifetime of ceramics, fatigue
lives predicted from dynamic fatigue properties are compared with experi-
mentally obtained ones. The lifetime prediction is carried out under the
following asssumptions.
(1) Delayed failure of ceramics is caused by a propagation of a pre-
existed flaw.
(2) Crack is extended only by tensile stress. The subcritical crack
growth behaviour is expressed by the following equation.

dadt = VO' (Kk

1e
1
)"
(1)

Where a is a crack length, KI is a stress intensity factor at a

466
 Table 1. Chemical compositions and densities of the materials for
the static and cyclic fatigue tests.

Contents (wt%) Density

Material
AI Y B Mg Ce Zr Sr Free C 0 (g/cm 3)
Nl(RS-Si3 N4) O. 032 O. 003 1. 81 2. 68
N2 (NS-S i 3N 4) o. 08 2. 08 3. 60 2. 18 O. 65 5. 80 3. 21
N3(HP-Si3N4) 1. 08 2.33 O. 003 3. 38 3. 25
Cl (NS-Si C) 2. 24 2. 70 3. 20
C2(HP-SiC) o. 125 3. 36 4. 22 1. 12 3. 17
RS Reaction Sintered NS Normal Sin tered HP Hot-Pressed

Table 2. Bending strength and fatigue parameters of the materials

estimated by the previous dynamic fatigue tests 3 6 . 3 7 •

20·C 800 ·C 1000·C 1200 ·C 1300 ·C 1400 ·C 1500 ·C

Material . , ,
n :
·, (j 8 n : (J B n a B n a B n a B n , a B n ·,, a B
, ,
·,
Nl 256 219 130
··: ··: ·: :
* ,, , * , * ,
N2 76 885 16 : 508 12 419
,, ,,
·:, · ·:,
,
··, ·
N3 110 , 960 , 50 I
994 32 ·,, 786 16 I
416 I

I I , I
I I
·,,
, I I
Cl 95 88
·,
448 47 401 33
·, 244
,, 515 , I I , I
,,
I I
C2 , 390 ,,
, ,
·· , 633 ,, ,
·, 676
* ·· * ·· ·· *
.". n Fatigue parameter. a B : 3-point bending strength (MPa)
Ol Subcritical crack growth is not observed (n~150).
-..J *
 ,~ Er

r
N

l 40

(a) For static and pulsating (b) For alternating fatigue test
fatigue tests

Figure 1. Shapes of specimens for (a) static and pulsating and

(b) alternating fatigue tests.

Table 3. Summary of testing conditions.

Testing conditions
Material
Temperature Atmosphere R (0' mini 0' max) Load frequency
20°C Air o. 2 5 5 H z
N1
.. _________ 00 ___

------------ ------------------- .... ----------_ .. _--

1200°C Vacuum o. 2 5 5 H z
O. 2 5 5 H z
20°C Air -- .. _------_ .. _------ --- .. --_ .. ---------
- I 5 H z

N2
1000°C Vacuum O. 1 H z
O. 2 5
5 H z

O. 2 5 5 H z
20°C Air
- 1 5 H z
N 3 -------------- ------------ ------------------- -----------------
1200°C Vacuum
O. 2 5 5 H z

20°C Air O. 2 5 5 Hz
C 1 1
1400°C Vacuum
0.25 5Hz
O. 2 5 5 H z
20°C Air
C2 -15Hz

1500°C Vacuum O. 2 5 5 H z

crack tip, KIc is a critical stress intensity factor, t is time from

the start of a loading and Vo and n (fatigue parameter) are con-
stants.
(3) The relationship between stress intensity factor KI and applied
stress 0' is written by following equation.

468
 (2)

Where Y is a shape factor of a crack.

(4) Change of shape factor Y with crack propagation is negligible.
(5) A crack length at fracture ac is large enough compare with an
initial crack length ao .
• -2
a~ -~- ~ a; -~-
,,-2

(3)

Under these assumptions a dynamic fatigue behaviour, that is the

relationship between the stressing rate if and fracture stress a 1', can
be wr it ten by

uj+1 2(n + 1) - .. :~ y-n K n

- iT
- = n-
2 ' ao • . vo '
-1
. Ie
(4)
= C (con,t.)

When an applied cyclic stress is expressed by

u(t) = um .... · F(21rft) (f j load frequency) (5)

the relationship between lifetime t1' and applied maximum stress a max is
written by
41r - .!!j1 -1 1
f:1< Fn(~)d~
-n -n
u~a .. . t = -n---2' ao . Vo . y . K le .

21rC 1 (6)
= n + 1 . f:1< Fn(~)d~

In the equation (6) the integral must be calculated for tensile

stress period of one cycle. Then lifetime under a static or a cyclic
loading can be calculated if the values nand C are known from a dynamic
fatigue behaviour. In the actual fatigue life predictions stress levels
are corrected using an effective volume based on Weibull statistics.

Results and dIscussion

Roo. te.perature fatigue property
The measured fatigue behaviours at a room temperature are shown in
Fig.2 (a)-(e). In the figures dotted and dash-dotted lines show the
pulsating and alternating fatigue behaviours predicted from the dynamic
fatigue property, respectively. The results are summarized as follow-
ings.
(1) In the materials N1 and C2 delayed failure is not observed.
(2) The pulsating fatigue data of N2, N3 and C1 and the alternating
fatigue data of N2 are distributed around the respective predicted
lines.
(3) In the alternating fatigue data of N3 the degradation of the life
compared with the predicted line is observed in low stress level.

From the results of the previous dynamic fatigue tests 36 it is

concluded that at a room temperature a subcritical crack growth in ceram-

469
 3OO..--r--~-""""---'---..-----r--.....,....---,
~ 6 0
~ l:>
~ 0
~ 200
~
I:
:;
E
'So. HI
20'C
~ R-0.25, I-5Hz
100 L.....lo.,-_........,.._----'-."....-_"-:-_.........._---'-:--_......,.............
10' 10' 10' 10' 10' 1cf 10·
Time to failure,s
(a) Nl

1000 ,......--~- ........ -__r--.--..,.....-.....,....--,

~ 900 (p<Ma11ng) PredietMi lif. til'M

~
wi 800 1
_.:!}--:.i'!:~--_=-~~~_~_~_ ~ e ..
~ ~ ; - -'T-.':A---
predICted lit. time
.;; 700 (oltomoUngl
E
~

.~ 600 H2
III
20'C
~ 0; R-0.2S, I-SHz
e; R--l ,1-SHz
SOO L...I..-:--_"-;-_....I..;-_----'-;-----''-:-_--'-;-_~---'
10· 10' 10' 10' 10' 10' 10'
Time to failure. s
(b) N2

1100 """"''''''--""T""---'--""T""---,---r--......,.-...,
If
~_1000
l
t
~ /} ••• _ predieted lif. time
~ -Q:"-..e-·.~._.e? ~ 0 (pulsating)
ti 900 " 0rtIP.e-e.O-----o.-. . 0
E l:> e (I)iii-- e__ -------
~ predic'od lifo limo e e eil--e-
E 800
'i(
H3 (o.ltomoting) • .~
20'C
~ o ; R -0.2S, 1= SHz
. ; R=-I. I=SHz
700 L....I--.......,..----'-:--.......,..----'-:---....L..;----l.-:-~
10· 10' 10' 10' 10' 10' 10'
Time to failure , 5

(c) 3

Figure 2. Results of fatigue tests at a room temperature.

470
 600 ,..,.--""T'"""-----.--""T'"""-----.--""T'"""-....,.-..,
~
::E
~500
l:l o 0
l!! -----_.0
o 0
--------00 _ 0
ti ----~ 0
E400 predicted ~,; -tT,.;.
:::s
E
·x C1
III
20'C
::E R.O.25 ••• 5Hz
300 L.....I.":""""_~-"""""-::__-'-:--""""":_----I._;__-~---I
10' 10' 10t 10' 10' 10' 10'
Time to failure I S

(d) Cl

500 ,..,.--.....-----.---....--.........----r--.....----,
,:.
::E 4oo
III •
!
ti 300 ~
E 6
:::s C2
E 20'C
.~ 0 ; R.o.25•• • 5Hz
::E 200 .......'"::._;_R_._-1,,-:-'._._SHz
.........-:--_"""'--:-_---"...,..-_........,,....-_.l....:-___I
10' 10' 1et 10' 10' 10' 10'
Time to failure I S

(e) C2

Figure 2. (Continued)

ics is caused by humidity controlled stress corrosion of glassy phase at

grain boundaries. Nl and C2 have almost no glassy phase at their grain
boundaries and by their dynamic fatigue tests subcritical crack growth is
not confirmed 36 . In the present experiments delayed failure of these
materials is not observed. On the other hand, delayed failure which
agrees with the line predicted from the dynamic fatigue property is
observed in the results of pulsating fatigue tests on N2. N3 and CI. In
these materials the existence of glassy phase has been confirmed by TEM
observation 39 . 4o . This result suggests that the pulsating fatigue beha-
viour of ceramics is also controlled by the extension of a pre-existed
flaw due to stress corrosion of glassy phase.
A difference is observed between the alternating fatigue behaviours
of N2 and N3. that is. the lifetime of N2 agrees with the fatigue life
predicted from the dynamic fatigue property while in N3 the degradation
of lifetime compared with the predicted one is observed especially in low
stress level.
In silicon nitride ceramics an acceleration of a crack extension
and/or a degradation of a fatigue life by cyclic loading has been report-
ed10.11.17.18.20.28.32.41.42. One of the possible mechanism is that
grain bridgings and grain interlockings formed on a crack surface are
destroyed by a compressive stress 32 or that even in compressive stress
periods tensile stress is generated at a crack front due to the lever
effect of fallen off grains on a crack surface or of crack surface asper-
ities and the crack propagates throughout a tension. compression
cycle6.10.28.42.

471
 Assuming the lifetime degradation mechanism, following conditions
are necessary to an appearance of cyclic loading effect on fatigue life.
(1) a crack must be propagated by a loading.
(2) grain bridgings, interlockings and/or crack surface aspcrities etc.
must be formed on a propagated crack surface.
In C2 specimen crack extension does not occur because of an absence
of glassy phase at the grain boundaries. Therefore above mentioned condi-
tion (1) is not satisfied. This may be the reason why a cyclic loading
effect on the fatigue property is not observed in C2. The subcri tical
crack growth in N2 has been confirmed by the dynamic fatigue tests at a
room temperature 37 (condition (1) is satisfied) while the cyclic loading
effect does not appear in its fatigue behaviour. In this case, probably
the condition (2) is not satisfied. Fig. 3 shows the SEM photographs of
Vickers cracks introduced on the polished surfaces of N2 and N3. The
Vickers indentation is conducted in water. An indentation load and
keeping time of a loading are 30kgf and 10min, respectively. In the
photograph of N3 many grain (cluster) bridgings and crack surface asperi-
ties are observed. But in the photograph of N2 such phenomena are not
remarkable and a crack propagates comparatively straight. Therefore the
condition (2) is not satisfied and thus the fatigue mechanism considered
here does not affect in N2.
Considering the fatigue mechanism, the compression load effect on
lifetime is negligible when a crack extension is small. Therefore the
degradation of life time by alternating load is observed only in a low
stress level in N3.
From these considerations it is concluded that a delayed failure of
ceramics under an alternating load at a room temperature is also caused
by an extension of pre-existed flaw but conditions of propagated crack
surface affect the lifetime. When the grain bridgings or interlockings
are formed on the crack surface they may be destroyed by compressive load
resulting in the lifetime degradation. The present experimental results
can be explained by this mechanism.

lIigh te.perature fatigue property

The measured fatigue behaviours at elevated temperatures are shown
in Fig. 4 (a)-(e). In Fig. 5 the pulsating fatigue data points of N2 are
plotted on number of cycles to failure. The results can be summarized as
followings.
(1) In Nl and C2 delayed failure is not observed.
(2) The pulsating fatigue data of N2 (except the data measured at load
frequency of 5Hz), N3 and Cl agree with the respective predicted
fatigue lives.
(3) The pulsating fatigue behaviour of N2 is slightly affected by load
frequency. At the same stress level the lifetime measured under
higher load frequency condition is longer.
(4) If pulsating fatigue data points of N2 are plotted on number of
cycles to failure, a difference of two data sets measured at load
frequency of 0.1 and 5Hz is enlarged.
(5) In the results of static and cyclic fatigue tests on N2 delayed
failure is not observed in the lifetime range of longer than 10 5 sec.
By the previous high temperature dynamic fatigue tests of the mate-
rials the facts that ceramics which has almost no glassy phase at the
grain boundaries does not show the crack growth behaviour, that the
active crack growth through the grain boundaries is observed when glassy

472
 (a) N 2
crack front

( b) N 3
Figure 3. SEM photographs of Vickers cracks introduced on polished surfaces
of (a) N2 and (b) N3 specimens.

~
-..I
W
 300 r-r---r-----..,.---r--.....,.---r--.....,.-...,
t!!
::E

111200
~
'lii •
E
:l
E
Nl
~ 100 L....,,-:-_........_
1200'C
R= 0.25. '-5Hz
..........,--_"'-:-_-"-_----"-:--_""'"':---'
10' 10 ' 10' 10' 10' 10' 10'
Time to failure. s
(a) Nl

500 ,.......,--.,...-----..,.---r-----..,.--.,...----,.-...,
~ 400
::E
- 300
j
ell
E 200 N2
::l
lOOO'C
E .. ;R=l (static) predicted We time
')( (.l.tlc)
o ;R-0.25, '-O.IHz
'"
::E • ;R=0.25, '-5 Hz
100 ......-::--...1..;------"-::---"""";------"-;--....1..;----'-;--......
10· 10' 10' 10' 10' 10' 10'
Time to failure, S

(b) 2

1000 ,.......,--.....,-----,,---.-----,--"'T""'"---,.-....,

~ 800
~
'lii
E 600
::l
E N3
1200'C predicted life time
4;R-l (static) (stltic)
o ; R = 0.25, ,- 5 Hz
400 L......I-:--....l..;-----''-:----'--;----'-;--.....L..;----'-:-......
10' 10' 10' 10' 10' 10' 10·
Time to failure, S

(e) N3

Figure 4. Results of fatigue tests at elevated temperatures,

474
 300 ~--.----,.....---.---,--~-"""T""---'

t
~200
'ti

Cl
1400'C
& ; R=l (stalic)
• ; R=O.25, I-5Hz

(d) Cl

700 r"'T--..---"""T""""---.---.---......-----.----.

~-600
~
~
•• •
§ SOO
E
'x I::> C2
i lSOO'C
R-U5, !-5Hz
400 .......-;---'7----'-;-----'--:---.o..,--.......,..---'---.J
10' 10' 10' 10' 10' 10' 10'
Time to failure. s
(e) C2

Figure 4. (Continued)

SOO r---.--~---r-""T"""-.---"""'T'"-~---r-"""T"""--.
If

.....
400
~
- 300
~ ~.)
'ti2QO o a.~
E
~ H2
'x 1DOO'C
III O;R"O.25,I_O.1Hz
~ .:R"O.25, 1-5 Hz
100 l....-......-:-"""""-;_"""-:-_....,........._-'-,_......,...................---'-_...J

10' 10' 10· 10' 10' 10' 10' 10' 10'

Number of cycles to failure

Figure 5. Cyclic fatigue data of N2 plotted on number of cycles

to failure.

475
phase exists at the grain boundaries of ceramics. and that the sUbcriti-
cal crack growth behaviour of ceramics at elevated temperatures is af-
fected by the composition of the glassy phase have been proved 3B • From
these results it is concluded that the subcritical crack growth of ceram-
ics at high temperatures is mainly due to softening of the glassy phase
and the concomitant degradation of the grain boundary strength.
The fact that both the static and the cyclic fatigue behaviours can
be explained by the dynamic fatigue properties suggests that substantial-
ly a fatigue life under a cyclic loading at elevated temperatures is
controlled by a subcri tical crack growth due to softening of glassy
phase. Fig. 6 shows the SEM photographs of fracture surfaces of N2, N3
and C1 specimens which have been failed by pulsating fatigue tests at
elevated temperature and have had comparatively long lives. On all the
fracture surfaces trace of a subcritical crack growth is observed. In
the subcri tical crack growth region of all the specimen intergranular
fracture is predominant while in the unstable fracture region transgranu-
lar fracture is observed. This result also supports that the delayed
failure by cyclic loading at elevated temperatures is caused by subcriti-
cal crack growth through the softened glassy phase at grain boundaries.
The pulsating fatigue life of N2 specimen tested at load frequency
of 5Hz is longer than that tested at load frequency of O.lHz if data
points are plotted on number of cycles to failure (Fig. 5). This differ-
ence can be roughly explained by the rate of the load frequency values.
This result indicates that the pUlsating fatigue life of N2 at high
temperatures does not depend on the number of cycles but on the loading
time.
Fig. 4(b) shows fatigue data points of N2 plotted on time to fail-
ure. In this figure a slight difference is still observed between two
pulsating fatigue data sets. The pulsating fatigue behaviour measured at
load frequency of O.lHz agrees well with the lifetime predicted from the
dynamic fatigue property but that measured at load frequency of 5Hz is
slightly sifted to higher lifetime range. This result suggests that the
subcri tical crack growth behaviour of ceramics at elevated temperatures
may be affected by the stressing rate. A possible explanation of this
phenomenon is that the resistance to crack propagation may increase at
high load frequency due to the elastic-plastic properties of glassy phase
at grain boundaries.
In static and cyclic fatigue tests of N2 specimen delayed failure is
not observed in the lifetime range of longer than 10 5 sec. The crystalli-
zation of the glassy phase at grain boundaries is considered as the cause
of the fatigue life extension. Then the X-ray diffraction patterns of
as-machined and heat-treated (lOOOoC in vacuum, keeping time: 24hours)
specimens are measured. Results are shown in Fig. 7. In the X-ray
diffraectin pattern of heat-treated specimen clear peaks of MgSi0 3 ,
MgSi0 4 • Sr2Si04 , Sr02. CeO.7SZrO. 2S02, Zr02 etc. are observed while in
that of as-machined specimen those peaks are broad and their intensities
are low. Almost all the elements contained in the crystals are the same
ones of the sintering additives. Therefore they can be considered as
main elements of the glassy phase at grain boundaries. This result
confirms the crystallization of the glassy phase by the heat-treatment.
The crystallization of the glassy phase may induce an improvement of
grain boundary strength and following extension of lifetime. Hence a
fatigue fracture is not observed in the lifetime range of longer than
10Ssec (about 24hours). Bending strength of heat-treated specimen is
measured at 1000 C to validate the effect of crystallization on strength.
After the heat-treatment bending strength level increases to 1.1 to 1.2
times.

476
 N2

T =IOOO'C
a max=250MPa
R =0. 25
f =511z
t =20. 730scc

N3

T =1200'C
a max=560~Pa
R =0.25
f =511z
t =32. 860scc

C1

T =1400'C
a max=180MPa
R =0.25
f = 511z
t = 2. 570 sec

Figure 6. SEM photographs of fracture surfaces of N2, N3 and Cl specimens failed by

~
-..J pulsating fatigue tests at elevated temperatures.
-..J
 20 30 40 50 55
2 8 (Cu KQ)
(a) As-machined specimen

, ; 5;3 ....
Z ; IiIg510:l
3 ; 1ilu25iO.
4 ; 5r02
5 ; 5'2510.
, ; Ceo15I 'O.25Oz
7; Z,Ot
...
It,

20 30 40 50 55
28 (Cu Ked
(b) Hcat-treated specimen

Figure 7. X-ray diffraction patterns of (a) as-machined and

(b) heat-treated specimens.

Conclusion
Static and cyclic fatigue tests of 3 kinds of silicon nitride and 2
kinds of silicon carbide ceramics have been carried out both at room and
elevated temperatures. Results are summarized as followings.
(1) Static and pulsating fatigue behaviours at every testing temperature
are predictable from the dynamic fatigue behaviours.
(2) The alternating fatigue life of the hot-pressed silicon nitride at
the room temperature is shortened in a low stress range. This
degradation of lifetime is probably due to the
destruction of grain bridgings and/or grain interlockings formed on
the propagated crack surface by compressive stress or due to lever
effect of crack surface asperities.
(3) Fatigue life of ceramics at elevated temperatures depends on the
loading time.
(4) Load frequency dependency of the cyclic fatigue life at an elevated
temperature is observed in a silicon nitride ceramics. The stress-
ing rate dependency of the subcritical crack growth behaviour af-

478
 fee ted by the elastic-plastic properties of glassy phase at grain
boundaries is considered as a cause of this phenomenon.
(5) At elevated temperatures the crystallization of the glassy phase at
grain boundaries causes an improvement of fatigue life.
From these results it is concluded that the delayed failure of
structural ceramics under the static and cyclic loading both at room and
elevated temperatures is caused by mainly the propagation of a pre-exist-
ed flaw and substantially the fatigue behaviour is predictable from the
subcritical crack growth behaviour estimated under the static or quasi-
static loading condition. Humidity controlled stress corrosion of glassy
phase and the mechanical fracture of grain boundaries due to softening of
glassy phase are considered as a'subcritical crack growth mechanisms at
room and elevated temperatures, respectively. Thus the properties of
grain boundaries is essential for the fatigue behaviour of ceramics both
at room and elevated temperatures.

Acknowledge.ent
The authors gratefully acknowledge the experimental assistance of
Mr. M. Ito and the specimen preparation of Mr. S. Sakai.

References
1. D.A.Krohn and D.H.P.Hasselman, J. Am. Ceram. Soc., 55, 208(1972)
2. C.P.Chen and W.J.Knapp, Fract. Mech. Ceram., 2, 691(1973)
3. R.Kossowsky, J. Am. Ceram. Soc., 56, 531(1973)
4. T.M.Yonushonis and K.E.Hofer, Proc. 1977 DAPPA/NAVSEA Ceram. Gas
Turbine Dem. Eng. Prog. Rev., 235(1978)
5. F. Guiu, J. Mat. Sci., 13, 1357(1978)
6. A.G.Evans, Int. J. Fract., 16, 485(1980)
7. Y.Matsuo, Y.Hattori, Y.Katayama and I.Fukuura, NATO Adv. Stu. Inst.
Ser. E., 65, 515(1983)
8. M.Kawai, H.Fujita, Y.Kanki, H.Abe and J. Nakayama , Proc. Int. Symp.
Ceram. Compo Eng., 269(1983)
9. T.Yamada, T.Hoshide and H.Furuya, J. Soc. Mat. Sci. Jap., 33,
28(1984)
10. Y.Yamauchi, S.Sakai, M.Ito and S.Ito, Proc. 27th Jap. Congo Mat.
Res., 27, 235(1984)
11. Y.Yamauchi, S.Sakai, M.Ito, T.Ohji, W.Kanematsu and S.Ito, J. Ceram.
Soc. Jap., 94, 631(1986)
12. T.Sakai and K.Fujitani, J. Soc. Mat. Sci. Jap., 35, 1371(1986)
13. H.N.Ko, J. Mat. Sci. Letters, 5, 464(1986)
14. H.N.Ko, J. Ceram. Soc. Jap., 95, 472(1987)
15. T.Tanaka and A.Sakaida, J. Jap. Soc. Mech. Eng., A53, 1566(1987)
16. T.Kawakubo and A.Goto, J. Soc. Mat. Sci. Jap., 36, 1253(1987)
17. M.Masuda, T.Soma, M.Matsui and I.Oda, J. Ceram. Soc. Jap., 96,
277(1988)
18. T.Kawakubo and A.Goto, J. Soc. Mat. Sci. Jap., 37, 939(1988)
19. M.Takatsu, H.Kamiya, K.Ohya, K.Ogura and T.Kinoshita, J. Ceram. Soc.
Jap., 96, 990(1988)
20. K.Saruki, K.Ogawa and T.Asano, J. Jap. Soc. Mech. Eng., A54,
2082(1988)
21. K.Ohya and K.Ogura, J. Soc. Mat. Sci. Jap., 38, 44(1989)
22. K.Ohya, K.Ogura, T.Takatsu and H.Kamiya, ibid., 38, 144(1989)
23. M.Masuda, N.Yamada, T.Soma, M.Matsui and I.Oda, J. Ceram. Soc. Jap.,
97, 520(1989)
24. H. N. Ko, ibid., 97, 599(1989)
25. M.Masuda, T.Soma, M.Matsui and I.Oda, ibid., 97, 612(1989)

479
26. M.J.Reece, F.Guiu and M.F.Sammur, J. Am. Ceram. Soc., 72, 348(1989)
27. S.Lathabai, Y.W.Mai and B.R.Lawn, ibid., 72, 1760(1989)
28. M.Takatsu, K.Ohya and M.Ando, J. Ceram. Soc. Jap., 98, 490(1990)
29. T.Ohji, Y.Yamauchi, W.Kanematsu and S.Ito, ibid., 98, 521(1990)
30. T. Tanaka , S.Yamamoto, N.Okabe and H.Nakayama, J. Soc. Mat. Sci. Jap.,
39, 318(1990)
31. T.Tanaka, N.Okabe, H.Nakayama, Y.Ishimaru and T.Imamichi, ibid., 39,
694(1990)
32. T.Niwa, K.Urashima, Y.Tajima and M.Watanabe, J. Ceram. Soc. Jap., 99,
296(1991)
33. T.Ogasawara, Y.Akimune and K.Yoneda, ibid., 99, 489(1991)
34. M.Reece and F.Guiu, J. Am. Ceram. Soc., 74, 148(1991)
35. G.Grathwohl and T.Liu, ibid., 74, 318(1991)
36. Y.Yamauchi, S.Sakai, M.Ito, T.Ohji, W.Kanematsu and S.Ito, J. Ceram.
Soc. Jap., 96, 885(1988)
37. Y.Yamauchi, S.Sakai, M.Ito, T.Ohji, W.Kanematsu and S.Ito, ibid., 98,
250(1990)
38. Y.Yamauchi, M.Steen and J.Bressers, Proc. 4th Int. Confer. Creep and
Frac. Eng. Mat. Struct., 449(1990)
39. T.Ohji, S.Sakai, M.lto, Y.Yamauchi, W.Kanematsu and S.Ito, J. Ceram.
Soc. Jap., 94, 1056(1986)
40. Y. Murase, private communication
41. H.Kishimoto, A.Ueno, H.Kawamoto and Y.Fujii, J. Soc. Mat. Sci. Jap.,
38, 1212(1989)
42. T.Tanaka, N.Okabe and Y.Ishimaru, ibid., 38, 137(1989)

480
FATIGUE BEHAVIOR OF NON-OXIDE CERAMICS AT ELEVATED TEMPERATURE

M. Masuda, T. Makino, Y. Nakasuji, and M. Matsui

NGK Insulators, Ltd.

Suda-cho, Mizuho-ku, Nagoya, 467 Japan

ABSTRACT

Cyclic and static fatigue tests were carried out using tensile
specimen to clarify the fatigue behavior of silicon nitride and silicon
carbide. The cyclic fatigue strength of silicon nitride on 10 7
alternating cycles is about 60% of the original mean tensile strength at
room temperature. With increasing temperature, the cyclic fatigue
strength decreases due to slow crack growth and creep deformation. The
static fatigue strength of silicon nitride also degraded with increasing
temperature. In slow crack growth failure without creep deformation, the
power law for crack growth rate controlled the strength degradation. In
creep deformation regime, the modified Larson-Miller parameter was
applicable to life prediction under static stress. On the other hand,
the cyclic fatigue phenomenon in silicon carbide is observed at elevated
temperature, but not at room temperature. The difference of fatigue
behavior between silicon nitride and silicon carbide was caused by
microstructure characteristics.

INTRODUCTION

Silicon nitride (Si)N,) and silicon carbide (SiC) are currently being
considered for use in gas turbine engine components" 2, because of high
mechanical strength and high heat resistance. Design of high-temperature
system frequently requires consideration of fatigue damage as well as
fracture strength.

In recent work by the authors, accelerated fatigue tests were made by

the resonant bending method to accumulate fatigue data up to 10'0 cycles
for silicon nitride, and to clarify the effects of frequency on cyclic
fatigue at room temperature. Degradation in strength of the silicon
nitride by cyclic fatigue at room temperature depended mainly on the
number of cycles rather than on time.) The tension-compression and
tension-tension axial cyclic fatigue tests at room temperature were
carried out to study the effect of mean stress and stress amplitude on
fatigue strength. The modified Goodman line agreed well with the results
of fatigue test at room temperature.'

The objective of the present work is to investigate the fatigue

Froclure Mechanics of Ceramics, Vol. 9

Edited by R.C. Bradt el ai.. Plenum Press. New York, 1992 481
behavior of silicon nitride and silicon carbide at elevated temperature.
Cyclic fatigue test and tensile stress rupture test were carried out using
tensile specimen. The effects of stress state on fatigue behavior at
elevated temperature were discussed.

EXPERIMENTAL PROCEDURE

Specimens

Three kinds of sintered Si 3 N_ (SSN-A, SSN-B, and SSN-C) and a hipped

SiC (HIP-SC) were studied. Mechanical properties of these materials are
shown in Table 1. A comparison of the tensile strength measured for the
used material in this work versus temperature is shown in Fig. 1. Tensile
strength measurements were made according to JIS R1606. The SSN-A showed
a decreasing in tensile strength at BOO°C or more, to 60% and 25% of the
strength at room temperature, at 1000 and 1200°C, respectively. The
SSN-B had higher heat resistance than SSN-A, occurred no strength
degradation up to 1200°C. However, the effect of temperature on the
tensile strength measured for SSN-B were significantly more severe than
for SSN-C. The SSN-C had higher average tensile strength than was
measured for HIP-SC from room temperature to 1400°C. However, the
tensile strength of SSN-C was more susceptible to the effects temperature
than was that of HIP-SC.

Table 1 Mechanical properties of silicon nitride and silicon carbide

Materials Density Four-point Fracture Young's

(g/cm 3 ) bending toughness 'b)
modulus")
strength") (MN/m 3 / 1 ) (GPa)
(MPa)

SSN-A 3.28 860 6 275

SSN-B 3.25 970 6 300
SSN-C 3.52 650 7 300
HIP-SC 3.15 610 3 415

(a):According to JIS R1601.

(b):Chevron notch method.
(c):According to JIS R1602.

The button head type tensile specimen cut from sintered cylindrical
blocks was also used in the fatigue test. The surface of the gauge
length area with 6 mm diameter was finished using 600-grit diamond
wheels. The maximum surface roughness, Rm •• , was less than 3.2 ~ m.
All specimen were inspected with liquid fluorescent dye penetrant and
radiographed (X-rays) to detect surface flaws and internal cracks. Only
those specimens free from surface damage and internal cracks were used
for testing.

482
 800
Tensile Strength

SSN-D

e:'"
.<;
600

~1lJ' '00 ~ - '\-- ~ ~~ -c

.•
~ r---/-lIP---S- C- - - - ' 1-2-~~-Q
200
• SS1l-A
• SSN-8 \SS ~A
o HIP-SC
• SSN-C
I2U \

Temperature. 't

Fig. 1. Tensile strength of used material. Tensile strengths were

measured up to 1500°C in air according to JIS R1606.

Cyclic fatigue test

Cyclic fatigue tests were carried out using the electro-hydraulic

testing machine equipped with a self-aligning grip system. A sprit
collet chuck with spherical bearings was used because it can both align
the axis accurately and facilitate the testing easily. The chuck was
designed to be self-aligning. The accuracy of the alignment for this
technique was verified by measuring the bending stress component, using
the strain gauge in the center of the gauge length. The percentage of
bending stress component was less than 5 %for each specimen, in both
static and cyclic loadings.

Cyclic fatigue equipment includes a high-intensity infrared image

furnace. s The infrared image furnace can heat the gauge of specimen up
to 1500°C. The temperature of the specimen was measured by three
thermocouples attached to the gauge portion, The temperature gradient
within the gauge portion was kept less than 10°C by controlling the
shadow of infrared ray.

In the cyclic fatigue test, the specimen were subjected to a sinusoidal

cyclic stress at 20 Hz and stress ratios (minimum stress / maximum
stress) were -1 (tension-compression loading) and 0 (tension-tension
loading) .

Tensile stress rupture test

Tensile stress rupture test was made to evaluate the static fatigue
behavior and to compare the static fatigue strength with cyclic fatigue
strength. The button head specimens were loaded with static tensile
stresses using both the lever type and the electro mechanical tensile
creep-rupture testing apparatus, heated either by an infrared image
furnace or electro resistance heating furnace using molybdenum disilicide
elements. 6

483
RESULTS AND DISCUSSION

Cyclic fatigue behavior in silicon nitride

Cyclic fatigue data for SSN-A with a glassy grain boundary phase at
800, 1000°C, and room temperature were plotted in a log-log plot of
stress versus number of cycles to failure, as shown in Fig. 2 (a). The
mean tensile strength of 6-mm diameter button-head specimens at room
temperature, 800, and 1000°C were 585, 560, and 360 MPa, respectively.
The arrow pointing to the left indicates the specimen fractured at the
onset of loading, and the ones pointing to the right indicate that the
tests were suspended at that cycle without failure of the specimen.
There was a large scatter, but the fatigue life of the specimens greatly
increased as stress amplitude decreased. At room temperature, fatigue
strength at 10 7 cycles was about 60% of the original strength. On the
other hand, the specimen was not fractured after 10 7 cycles by an
amplitude stress of 300 MPa, i.e., 95% of tensile strength at 1000oe.

At room temperature, fatigue strength was higher under pulsating

stress than under alternating stress. At 800 oe, however, both cyclic
fatigue strengths under alternating and pulsating were equivalent within
the scatter of the data. In addition, the pulsating fatigue strength is
lower than the alternating fatigue strength at 1000°C. The contribution
of mean stress on fatigue strength was significant with increasing
temperature.

700 SSN-A a
<II 600

~500
ui'\OO

.'".
CIl

.... 300
1Il

-
~200 Ten-Camp (R--l) Ten-Ten (R~O)
.~
ORT
~ ... BOO'C ~ BOQ'C
_ 1000'C IOOO'C
100 :--:""'":"::-7"~~"""::-';'""""::,"",:"....L-,;,-,,'""'-~...l...,:",",,,"...L..:-,",,,,oL..,.....,j
10· 10' 10 J 10' 10 ~ 10.) 10' 10' 10' 10 t 10 10

umber of Cycle to Failure, J

700 SSll-B b
_-0
'" 500.
~ 500 t • -=:: -'0
0--"'0_0 ~
-~­

ui '00 f --- e
.-e().t5o-
.".
CIl

~300
1Il
~
() e-
f
Ten-Camp (R=-l) ren-ren (R=O)
o RT
• IOOO'C r:J lO00'C
• 1200'C () 1200'C
100 I, J J J J J ! f.J J I J .J
o· 10 t 10' 10.) 10 ~ 10.) 10' 0' 10' 10' 10 It

Number of Cycle to Failure. N

Fig. 2. S-N diagrams of silicon nitride. (a) SSN-A at room temperature,

800, and 1000oe, (b) SSN-B at room temperature, 1000, and
1200 oe. The symbols on the vertical axis represent the tensile
strength of the used material.

484
 S-N curves for SSN-B with a crystalline grain boundary phase are
shown in Fig.2 (b) for both tension-compression and tension-tension
loading. Similar to SSN-A, the cyclic fatigue strength under alternating
stress at room temperature is about 60%. Cyclic fatigue behavior at room
temperature was not strongly dominated by characteristic of grain
boundary phase. However, the SSN-B appears to show increasing fatigue
strength at 1000°C, compared to that at room temperature. On the other
hand, the fatigue strength represented S-N curve decreased at 1200°C.
The degradation behavior of SSN-B by cyclic fatigue at elevated
temperature is not similar to that of SSN-A.

Static fatigue behavior in silicon nitride

The results of the tensile stress rupture tests are shown in Fig. 3.
The fracture strength of SSN-A under static stress decreased as the
temperature increased, as shown in Fig. 3 (a). It was also noted that the
specimens fractured with lower stress in tensile stress rupture test than
cyclic fatigue test at 1000°C, as compared with results in Fig. 2 (a).
The strength degradation was caused by slow crack growth.

In contrast, the SSN-B specimens showed on-off type behavior; some

specimens either sustained for 1000 to 2000h or ruptured at the onset of
loading under 450 to 600 MPa as shown in Fig. 3 (b). The increasing of
cyclic fatigue strength at 1000°C compared with that at room temperature
was caused by no enhanced slow crack growth. At temperature over 1100°
C, specimens showed delayed fracture, that is, time to failure was
dependent on the applied stress. In addition, the SSN-B specimen showed
creep deformation at temperature over 1100°C. The creep strain at failed
increased with increasing temperature and decreasing applied stress. The
strength degradation of SSN-B at elevated temperature was caused by creep
deformation.

The results of the tensile stress rupture tests for SSN-C are
presented in Fig. 3 (c). Similar to SSN-B, the SSN-C specimen showed
delayed fracture and creep deformation at temperature over 1200°C. The
resistance of SSN-C to static fatigue was high compared to the behavior of
another silicon nitride, as shown in Figs. 3 (a) and (b). The difference
among the silicon nitride ceramic is attributed to the characteristics of
grain boundary phase at elevated temperature.

Predicted life time of silicon nitride

1) Fatigue life time considering slow crack growth

The fatigue life of ceramic materials has been predicted by the power
laws 7 . 8 or exponential laws 9 . 10 for crack propagation. The lives of
different materials or under different environments are predicted by
different procedures. It is necessary to use different procedures to
predict the life of silicon nitride at elevated temperature, because the
strength degradation is caused by different mechanisms, depending on the
temperature, stress and microstructural characteristics. The following
power law crack propagation equation is widely used to predict the life
time for ceramic materials:

da AK ,n (1 )
dt

where A is a constance and a is crack length.

485
 1000
900 a
800 SSN-A
700 A 800'C
.1000·C

..
600 • 1100'C
al
Il. 500

-----A ---11._
:::ll -A
oi 400
Ul
II)

~ 300
en .~. ~

.~
~
.~
'a.
Il.
-<
ZOO
• •
,.~~
100
90
10-'
., ~~

Time to Failure. h

1000
900 b
800

.------..
700

.,
al
Il. 500
600
i: ---==---. ----:=-----~-
:::ll
~
...& -.~
oi .................
.....
400

•
Ul
II)

en 300
,~
~
.~
'a. zoo
•~.
\
Il. SSN-B
-<
.\
A 1000'C
.1100·C
.IZ00·C
$ 1300'C
100 ~
90
10 -. 10-' 10-'> 10-' 10-' 10' 10' 10' 10' 10' 10'

Time to Failure. h

1000
900 C
800
700
600
os
Il. 500
:::ll
iii 400

.....
Ul
II)

en 300
~
.~
'a.
Il.
zoo
SSN-C
-< A lZ00'C
• 1300'C
• 1400'C

Time To Failure. h

Fig. 3. Results of tensile stress rupture test.

(a) is SSN-A, (b) SSN-B, and (c) SSN-C.

486
 The stress intensity factor K I is given by the following equation:

K, = Y q (a)I/2 (2)

where q is the stress and Y the geometric factor. Equations (1) and (2)
give the life time t. in the static tensile stress rupture test as,
C. q -" (3)

Ca =

where q I is inherent strength for the initial crack length. Tensile

strength q t under a constant stress rate q , in which called dynamic
fatigue strength, is given by combining equation (l)and (2),

q ,"+' = (n+l)C. q (4 )

Time to failure t. is given by combining equation (3) and (4), as

equivalent time t •• with respect to static fatigue:

1
t.. = -----,-----'------=-- t. (5 )
(n+l )

Under the assumption that the mechanisms of static and cyclic fatigue
are identical, the lifetime of cyclically loaded specimen can be computed
from data on the life times under constant load and constant stress rate.
In case of a sinusoidal alternating loading, cyclic fatigue life time t,
is given by the following equation l :

to
= J o(q(t))"dt

= q :., g(n) t, (6)

The equivalent time on cyclic fatigue, t •• is given by combining equation

(4) and (6):

t •• g(n) t , (7)

Comparison of life times of SSN-A under dynamic, static, and cyclic

load is shown in Fig. 4 (a). The equivalent time were calculated using n
values of 40 at 800'C and 11 at 1000°C, based on the static fatigue
test results shown in Fig. 3 (a). The equivalent life times of dynamic
fatigue and cyclic fatigue agreed with the static fatigue data at 800°C.

At 1000°C, on the other hand, the equivalent life time of dynamic

fatigue also agreed with the static fatigue data. However, the equivalent
life time of cyclic fatigue at 1000°C tended to shift to the higher-
stress, longer-life side than the static fatigue data. Equation (1) is
not applicable to cyclic fatigue under high frequency (e.g .• 20Hz) cyclic
stress, other mechanism must be considered for cyclic fatigue at elevated
temperature.

487
 The relationships between stress and equivalent time to failure for
SSN-B and SSN-C are shown in Fig. 4(b). The equivalent times of tensile
strength data were calculated using the n value of static fatigue data.
The results of SSN-B and SSN-C are represented by two straight line
divided into two stress region. It is possible to apply the power law
crack growth formulation to the high stress region. However, equation (3)
based on the slow crack growth from preexisting flaw, tends to
overestimate life time in low stress region. It is therefore necessary to
use another procedure for creep rupture region.

2) Predicted static fatigue life considering creep rupture

The following Larson-Miller parameter P is widely used to predicted

life time of creep rupture in metallic materials:

P = f (t7 ) = T ( C + log L ) (8)

SSN-A a
600
I;

"-;:
~~-'"
500
a:l =A ...
Po. 400
:::s ... '" ~~ 40-

b
oi
III
Gl 300 o ': ~~~*;:-
00

a::l . D~ ~-
....a
200 8oo'c 1000'C 0 0
Tensile I> IJ "- IJ
H "-
a:l Static ~ 0 0 IlD 0
:::s
Cyclic (R=-l) ... _II ""

(R=O) '" ""

100 0- 0-
90
10'"
Equivalent Time to Failure, h

1000
900 b
800 Static Fatigue Tensile Strength
700
SSN-B 1200'C 0 •
SSN-C 1200'C 0 •
600 1~0~ 6 ~
oj
Il. 500
:::s
In 400
In
ClI

Ci'"l 300
'I:l
.~
P. 200
0-
-<

Equivalent Time to Failure. h

Fig. 4. Comparison of life time under dynamic, static, and cyclic load.
(a) is SSN-A, (b) is SSN-B and SSN-C.

488
where T is absolute temperature, t, is time to creep rupture, and C is a
constant. The C value of 20 in equation (8) is widely used in case of
metallic materials. The relationship between applied stress and Larson-
Miller parameter depends on the temperature. It is noticed that the C
value of 20 is unsuitable for used silicon nitride. Figures 5 (a) and
(b) show the master Larson-Miller curve, where C= 44 for SSN-B and C=30
for SSN-C are used. The results of both SSN-B and SSN-C are represented
by a line, and no dependence of temperature is shown. The effect of
temperature on the creep rupture strength of SSN-B were significantly more
sever than SSN-C. The C value in equation (8) depends on material, the
higher the C value, the more sensitive the influence of temperature on
creep rupture time.

1000
900
a
800

700

600 l:r+
A
500 I:::-
l:r+
A
..
•
\
400 .~

~
~
" \.
300 .ii
fli
fIl \ • •
"...
'"
CJJ
200 SSN-B
/11000'C
A 1100'C
o 1150'C
•\
\

.1200·C
••
\
o 1250'C
.1300·C
Ell 1350'C

100
90
-til
55 60 65 70 75
P:T(44+1ogtr) XlO·'

1000
900
b
800
700

600

500

\
400 A

•
\
"
•
~ \
~ 300

•\
ui \
fIl

"...
'"
•
CJJ

.,
200 SSN-C
A 1200'C
• 1300'C
• 1400'C \
100
90 L -_ _J -_ _--'-_ _- ' -_ _- ' -_ _ ~

35 40 45 50 55 60

P:T(30+1ogtr)Xl 0·'

Fig. 5. Master Larson-Miller curve for silicon nitride.

(a) is SSN-B using C=44 and (b) is SSN-C using C=30.

489
 600

. ..
500 H1P-SC
(fJ

~400 I ::I
en ::I • ()
en
Q)

en'"
....
300 ()
•
S
;j200
S
.>< • RT (R=-I)
(fJ
;::;t • 1200'C (R=-I)
() 1200 'c (R=O)
100 L....L.~................."--'-~"'---'-~"'-'-~"'-'-~"'-'~""-'...u..u""--'...u..u""--'u..uw<

10' 10 I 10' 10 J 10' 10' 10' 10 7 10' 10' 10 10

Number of Cycles to Failure, N

Fig. 6. The results of cyclic fatigue test for HIP-SC. Cyclic fatigue
test carried out at room temperature and 1200°C.

Cyclic fatigue behavior of silicon carbide

The results of cyclic fatigue test for HIP-SC are presented

graphically in Fig. 6. Cyclic fatigue at room temperature is on-off
type; specimens either sustained up to 2 to 3 X 10 7 cycles at 250 to 350
MPa or failed at the onset of loading with 350 to 400 MPa. Cyclic
fatigue behavior in HIP-SC is not similar to that of silicon nitride. The
microstructure in HIP-SC is monolithic and free of grain boundary phase
between silicon carbide particle. The difference of cyclic fatigue
behavior among non-oxide ceramic at room temperature is caused by
microstructure characteristics.
At 1200°C, however, specimen showed cyclic fatigue fracture under
both alternating and pulsating stresses. No difference between number of
cycles to failure under alternating loading and that at pulsating loading
was observed within scatter of data. It seems that the slow crack growth
contribute to fatigue failure at elevated temperature.

CONCLUSION

Cyclic and static fatigue tests were carried out using tensile
specimen, the fatigue behavior of silicon nitride and silicon carbide were
clarified as following:

(1) With increasing temperature, the cyclic and static fatigue strengths
decrease due to slow crack growth and creep deformation.

(2) The fatigue strength degradation in silicon nitride is strongly

depended on microstructure characteristics at elevated temperature.

(3) In slow crack growth failure without creep deformation, the power law
for crack growth rate controlled the dynamic, static, and cyclic fatigue
strength degradation.

(4) In creep deformation regime, the modified Larson-Miller parameter was

applicable to life prediction under static tensile stress.

(5) The cyclic fatigue phenomenon in silicon carbide is observed at

elevated temperature, but not at room temperature.

490
(6) The difference of fatigue behavior among non-oxide ceramic under
various stress state was caused by microstructure characteristics.

Acknowledgment

A part of this work was performed under the management of the Engineering
Research Association for High Performance Ceramics as a part of the R&D
Project of Basic Technology for Future Industries supported by NEDO (New
Energy and Industrial Technology Development Organization).

References

1. Y. Kobayashi, T. Inagaki, E. Matsuo, and T. Ozawa, SAE Paper 910401

(1991).
2. I. Tsuji, S. Aoki, S. Miyazaki, Y. Hara, Y. Furuse, and S. Hamada,
ASME 91-GT-311, (1991).
3. M. Masuda, N. Yamada, T. Soma, M. Matsui, and I. Oda, Nippon
Seramikkusu Kyokai Gakujutu Ronbunshi, 97(5), 520-4 (1989).
4. M. Masuda, T. Soma, M. Matsui, and I. Oda, Nippon Seramikkusu Kyokai
Gakujutu Ronbunshi, 96(3), 277-83 (1988).
5. M. Masuda, T. Soma, M. Matsui, and I. Oda, Nippon Seramikkusu Kyokai
Gakujutu Ronbunshi, 97(6), 612-18 (1989).
6. M. Masuda and M. Matsui, Nippon Seramikkusu Kyokai Gakujutu
Ronbunshi, 98(1), 83-92 (1990).
7. A. G. Evans, Int. J. Frac. 10, 251-59 (1974).
8. T. Kawakubo and K. Komeya, J. Am. Ceram. Soc., 70[6], 400-405 (1987).
9. G. G. Trantina, J. Am. Ceram. Soc., 62[4], 377-80 (1979).
10. T. Ohji, Y. Yamauchi, W. Kanematsu, and S. Ito, Nippon Seramikkusu
Kyokai Gakujutu Ronbunshi, 98(6), 521-28 (1990).

491
CYCLIC FATIGUE OF ELECTRICALLY POLED PIEZOELECTRIC CERAMICS

T. Nishikawa, J. Takahashi, A. Hattori and M. Takatsu

Dept. of Materials Science and Engineering

Nagoya Institute of Technology
Gokiso-cho, Showa-ku, Nagoya, 466 Japan

INTRODUCTION

Static and cyclic fatigue properties of unpoled lead titanate (PT) and lead
zirconate titanate (PZT), were earlier investigated and classified according to
the fatigue parameter for the crack propagation charateristics [ 1 ] .
However, the polar direction in ceramics must be obtained by applying high
voltage and the orientation may bring about the anisotropic mechanical
properties, using these ceramics for piezoelectric material. Actually, Yamamoto
et al. [2] found that the crack length introduced by Vicker's indentation,
exhibited anisotropy with the polar direction for PT, while, Mehta et al. [3]
obtained the same results for poled PZT under the application of mechanical
stress. Bruce et a1. [4] measured the crack propagation of poled PZT by DT
technique and found the fracture behavior depended sensitively on the state
of poling. Mechanical properties of PZT were distinctly different depending
on whether the material is poled parallel or perpendicular to the direction of
applied stress.

In this paper, the static and cyclic fatigue of poled piezoelectric ceramics,
which were same material used in the previous study [ 1 ] , were investigated,
and the crack propagation properties in poled PT and PZT were discussed
quantitativeb' using the fracture parameter.

EXPERIMENTAL

Preparation of test pieces

The specimens used in this work were commercial lead titanate (PT) and
two kinds of lead zirconate titanate (PZT), which were described in the
previous work [ 1 ]. The PZT(a) and (b) in the present study corresponded
to PZT(b) and (d), respectivel~', in the previous paper. The mechanical
properties of these specimens were listed in Table 1. All specimens belonged
to a tetragonal crystal system. For the polar handling, the PT specimen was
subsequently poled in an insulated oil at 150°C under an electric field of 60
kV fcm for 30 min. The PZT specimen was poled at 150°C under an electric
field of 20 kV fcm for 20 min. Test pieces were cut to 4x3x40 mm, with applying
the load direction in three point bending test is parallel ( II ) or perpendicular
( .L ) to the polar direction. In Table 1, the upper values were obtained under
the former case and the below values did under the latter case. The values in
Fracture Mechanics of Ceramics, Vol. 9
Edited by R.C. Bradt el at., Plenum Press, New York, 1992 493
 Table 1. Mechanical properties of electrically poled PT and PZT ceramics

specimen Density Vicker's Fracture Bending Weibull's Young's

hardness toughness strength modulus modulus
q/cm J GPa MPaJIlO·5 MFa GPa
II 1.7 161 15
PT 7.5 4.36 (1.6) (165) (20) 135
J. 2.1 1.3 177 13
II 1.0 74 19
PZT(a) 7.6 2.94 (1.1 ) (84) (13) 75
J. 1.7 0.6 74 19
II 1.5 108 16
PZT(b) 7.6 3.79 (1. 3) (104) (18) 90
J. 1.8 0.9 103 22

~r
F===~I?
Load

6r
, P

~~4"
3 "(1 E
19'" Ql 1
: i'
30.. I
I I

Fig. 1 Shematic representation of the applied

load and polar direction

parentheses were quoted from the data for the unpoled PT or PZT. Two
different KI C values were calculated for the specimen, which were poled
perpendicular to the direction of indentation. The preparation of test pieses
was shown in Fig. 1 schematically. The test pieces were lapped to a mirror
finish with ground corners.

Fatigue Test

The mean bending strength was previously measured by a three-point

bending test to determine the Weibull parameter. Then, cyclic and static
fatigue tests were performed under maximum applied stress ( (J max), which
was 70 to 100% of mean bending strength, to measure the time to failure (t~).
Cyclic fatigue test was conducted on a high frequency cycling instrument,
which provides a sinusoidal cyclic frequency of approximately 450 Hz with a
stress ratio (R= (J m 1 .. 1 (J ,r. a x) of 1.0, 0.7 or 0.1 and one-side oscillation. The
experiment was conducted at room temperature under 50% R.H. for a maximum
of 10 15 seconds.

RESULTS

Static and cyclic fatigue results of each test piece were shown in Fig. 2, in
terms of the relation between the maximum applied stress (J m ax and the time
to failure t~. Static fatigue test results were indicated by the solid line and
the range of standard deviation by the dashed line, as obtained by the least
squares method. Data on three-point bending strength are shown on the left
side in Fig. 2 as an average value with deviation.

The data for PT at R=O.7 shifted slightly toward the long life side compared
with those at R=1.0. For the PT .L, the load direction was perpendicular to the
polar direction, fatigue data shifted to the short life side at stress ratio

494
 200 r--=--r--..---r-rT-,-,r----rr-"]"'O';:-;;;--,
150
100
1-:-:---';r=+:~=-1
~

J
~ 200~qJ~~;...c4+-+-j---++___r~.L..;__i
150 •

100

150
100

~ 501-:-:--'-,~~'-r-::-l-
~

i 150
100 • .-\~~_a.~2..~k:1Ib~b<I-
50 50

tt (s.c) tt (spc)

Fig. 2 Relations between maximum loading stress ( (J max) and fatigue life (t.. )
for poled PT and PZT ceramics under the different stress ration (R)

R=O.l. This shift means that this test piece at R=O.l easily failed for a short
time at the same maximum stress. This acceleration effect of fatigue appeared
for PZT independent of the polar direction at R=O.l.

DISCUSSION

(~uantitative Method of Fatigue Behavior

In order to express the above fatigue behavior quantitatively, the data

were normalized using the crack propagation rate equation V=AIK,/K,c)n on
the subcritical crack growth, where V is crack growth rate, K I is stress
intensity factor and K I C is its critical value. The detailed discussion is found
in Appendix I. The A, n were constants known as fatigue parameters of
material at a given load condition. The normalized results were shown in Fig.
3. The solid line and the dashed line were similar to those in Fig. 2. If
experimental data under cyclic load were located between the two dashed
lines, the crack propagation rate under cyclic load did not change with that
under static load. No change in crack propagation behavior for PT 1/ was
recognized with decreasing R. However, cyclic fatigue data for PT.l. shifted
toward the short life side. This suggested that the crack propagation rate
was accelerated under cyclic fatigue test. For unpoled PT, however, this
al..:l.:d~ralion was not observed. Such acceleration and unisotropic fatigue
behavior must be caused by polar handling. Conversively, for PT.l. under
R=O.7, the cyclic fatigue data slightly delayed and located in the long life re-
gion.

For PZT, acceleration was observed at R=O.l, independent of polar and load
directions. The data for PZTla) shifted even further to short life side
compared with those for PZT( b). The different fatigue properties in the same
material may involve microstructure. particle size and polarization.
~Ieasuring the cyclic fatigue data at the stress ratio R for PZT(a), the

495
 1.2r---r-r----,r-T-"T""1r---r-r----,,.,--,..,r-1
11

10 10
.!. 0.9

J- 0.8

0.7 "'K,.-.+O:'-r-"
...... o 7 F.:K,.-.-ro:'-T-:():-+~• ..,
0.6 RH 1.0 0.1 0.6 RH 1. 0 0 7 0.1
10·' l(j> 10' 10' 10' 10' 10" lr:P 10' 10' 10' 10'
h·g-leuC) hog,I(MC)

1 2r---r-,----,rT-..,r---r-.-----.--r-..,.......... 1 2,...---r-.--r-r--,-,----r-'----'rT--'-'--'

07 07
•
0.6 K. 0 () 4 •• 0 0.6 ",•• 1 0 () • • •
RH 1.0 0.7 0.5 0.3 0.1 O.HI> RH 1.0 0.7 0.5 0.3 0.1
10" 1(:1' 10' 10' 10' '0" lr:P 10' 10' 10' 10' 10'
tf-g-I(uc) h golcn(.)

I 2r---r-'--rT--.--r---r-'--rT--'-r--. I 2 r---r-.-----,rT-..,r--r,---.-r-,~,..,
11 11

10 10

0.9

J~;; 0.8 e.
o 7I:Ko,..-,;Lo;:'.,.-;()~-:.~
0.6 RH 1.0 0.7 0.1
• o 7F.:Ko--'-'-:O:'-T-;()+~
0.6 RH 1.0 0.7 0.1
• ..,
•
10" lr:P 10' 10' 10' 10' 10' 10·' lr:P 10' 10' 10' 10'
h-g-le Me ) 1'-9-1 (MC)

Fig. 3 Analysis of cyclic fatigue properties on poled PT and PZT ceramics

Ke Somple
o PT II
() P.J..
70 I::> PZT(clll
a PZHcll.
o PZT<blll
60 ..!.. PZT(b).!..
I' <{
"J
c: 50 0>
E
0

PZT(a,
30

20 1.0
0 0.5 1.0
R (-)

Fig. 4 Fig. 5
Relations between applied stress Relations between applied stress
ratio (R) and fatigue parameter (n) ratio (R) and fatigue parameter (A)
The broken lines indicated the data The broken lines indicated the data
for llnpoled samples. for unpoled samples.

496
acceleration under cyclic load clearly became less than 0.5 at R, that is the
increase of amplitude of the vibration. Fig. I showed the change in fatigue
parameter n, which was calculated from the slope of the line at the stress ratio
of R for each test piece. Larger n value means the decrease of crack
propagation rate. The n value of each specimen was constant independent of
R with few exceptions. Therefore, it IS difficult to discuss the effect of R.

The fatigue behavior was discussed using parameter A, which is found in

Appendix II. The log ~ A was taken with R and shown in Fig. 5. The log ~ A
indicated the distance in the horizontal shift from the static fatigue data at (1
o, .. x/S~=l.o. Its positive value means the acceleration to short life time and
negative means the delaytion. These treatments clarified the degree of accel-
eration under cyclic load quantitatively with decreasing R. Especially, the
data for PZT 1. tended to shift toward short life compared with those for PZT

Fractography of Ceramics Revealed Fatigue Acceleration

Fatigue parameter n value of PT or PZT poled electrically is similar to that

of each unpolar specimen. Thus, the n value of PT was approximately 30 and
that of PZT was 40 to 60, respectively. These higher values than those for
other oxide ceramics indicates the remarkable resistance to mechanical fatigue
at low applied stress. Bruce et al. [4] and Freiman et al. [5] investigated
the crack propagation of PZT and BT by DT or DeB technique. Caldwell et al.
[ 6] also studied PZT using cyclic fatigue test. The n values in these papers
were 60 to 60, which corresponded to those obtained in this work. The accel-
eration mechanism was actually recognized under cyclic fatigue in the present
study.

The acceleration mechanism of crack propagation is still under discussion

in relation to the microstructure. Kishimoto et al. [7] proposed a model of
incomplete crack-closure and the formation of tensile stress at crack tip in
the unloaded condition. Tanaka et al. [8] explained the fracture model
based on the wedging of debris, which consisted of fallen particles in the
crack plane. Kawakubo [ 9] also carried out cyclic fatigue tests on some
ceramics and found acceleration mainly in ceramics which exibited a
inter-granular fracture. These acceleration models based on the fracture
mode were confirmed for silicon nitride and alumina ceramics [ 10,11 ] .

The microstructure of the fracture surface for PT and PZT was shown in
Fig. 6. The particle size of PT and PZT was 1 J.l m and 4 to 5 J.l m in diameter,
respectively. The origin of fracture was almostly large pores ( ..... 50 J.l m) in
or on the surface of test pieces. The semicircular fracture mirror, on
subcritical crack growth, was observed below the origin of the fracture. The
crack plane of PT was relatively smooth, in which the trans-granular fracture
was predominant and small particles existed. The crack plane of PZTla), in
which inter-granular fracture was predominant and large particles and pores

Fig. 6 Hicroscopic SEM fractographs of poled PT and PZT ceramics

497
"ere observed. was remarkably rough. For PZTlbl, trans-granular fracture
"as mainly observed. However. as the trans-granular fracture was
predominant for PT and PZTlbl, these fracture models did not sufficiently
apply for the piezoelectrical ceramics.

Yamamoto et al. [12] reported that the fracture mode change with polar
handling, that is from trans-granular to inter-granular fracture. Kim et al.
(13] also reported that inter-granular fracture was mainly observed in test
pieces after polar handling. However, the change in fracture mode and its
ratio was not observed sufficiently in this work, compared with those for po-
lar and unpoled test pieces. Kishimoto et al. [7] and Tanaka et al. [8]
used pre-cracked CT or SEPB test pieces in their experiments, in which the
crack length was long and there was obvious interaction of the adjacent crack
plane.

On the other hand, short crack length and semi-elliptical mirror, due to the
narrow displacement even under maximum applied stress, was confirmed in
this work. The crack length just before unstable fracture was estimated by
the following equation in CSF method,

1C /2
¢l = i [ sin 2 tP +la/cl 2 cos 2 t/J] I. '2 d t/J,
o

where. a was the length of short axis and b was that of long axis in elliptical
shape. e indicated the eccentricitic angle. The maximum radius was up to
250 /01. m with a semi-circle shape. This value corresponded to that observed
by SEM and suggested that the critical crack length in non pre-cracked
testpieces was small. These results indicated that acceleration effect under
cyclic load did not explain only by interaction of the adjacent crack plane.

Acceleration by the Formation of Domain

Residual internal stress occurs in piezoelectrical ceramics by thermal

expansion anisotropy or phase transition at Curie point after polar handling.
This kind of stress is known to cause microcracks along the grain boundary.
However, the formation of domain in particles, which exhibited the same c-axis
direction, abolished such stress. Kim et al. [ 13] studied the bending
strength of PZT of various particle sizes. They found that formation of domain
was difficult in small PZT particle and therefore residual stress was consumed
the formation of microcracks along the grain boundan'. Okada et al. [ 14 ]
l'eported fatigue fracture was caused by the connection of these microcracks,
testing alumina ceramics under static fatigue test. Grathwohl [ 15 ] also
proposed the accelaration model due to microcracks under cyclic fatigue. Ac-
l~eleration of crack propagation due to residual stress was repol'ted by Lewis
~t al. [ 16,17 ]. These results suggested that higher residual ,stress and
lower mechanical bonding along the grain boundary brought about formation
of microcracks and internal stress. which in turn accelerated the crack
propagation under cyclic load.

In the present study, the residual internal stress and the formation of
domain must be considered. For the specimen to which indentation was made
perpendicular to the polar direction, cracks parallel to the c-axis in domain
hardly extended. The acceleration was recognized for PT .L' PZT -'- under
cyclic load. These results showed that microcracks required to extend crack
might exist perpendicular to the c-axis in domain. The formation and
interaction of cl'ack and domain was discussed by Pohanka et 301. [ 18] and

498
t-1ehta et al. [::J). Pisarenko et al. [ 19) explained the anisotropy of
fracture toughness by the switching model in domain at crack tip. This
switching of the domain may also affect crack propagation properties.

Briefly, the acceleration and anisotropy of crack propagation under cyclic

load and were explained as follows. The residual stress occurred by the re-
arrangement of domain, accompanying the formation of microcracks. The
interaction between domain and crack also was contributing factor.

Appendix I Calculation of Parameter n

The velocity of the crack propagation at below the critical stress intensity
factor (K, c) is represented by the empirical formula:
V=(dc/dt)=A(K,/K,c)n (1)
where, V=crack propagation velocity, K=stress intensity factor and
A,n=constans.

Assuming a randomly picked sample possessing an initial crack length C

which requires a time to failure t~ until it grows to length C~ and begins to "
have an unstable growth, the following equation is obtained by integrating
Eq.(l):
t r
Sn-2=[(n-2)/2](A/K,c 2 )y2 ~ [cr (t)]ndt (2)
o
In this equation, S denotes the strength when a dynamic load has been exerted
on a sample possessing an initial crack length C and has a relation:
S=K I c/(YC, '/2). The relationship of S with the "bending strength Sr at a
loading stress velocity 15 is obtained as follows, by solving Eq. (1) under the
condition of cr (t)= d' t:

(31

By substituting Eq.(3) in Eq.(2) and rearranging, the following is obtained:

tr
[ 0- -, /(n+ll]Sr n +,= ~ {cr (t)}ndt (4)
o
By carrying out the integration on the right side of Eq.(41 with the time
range of (t 2 >t>t, ) that satisfies the stress (cr (t) > cr "m) corresponding to
the range (K,>K'"m) where Eq.(ll is applicable, and by making the stress term
of Eq.(41 non-dimensional using the applied stress cr mex and then rearranging,
Eq. (5) is obtained

log( cr mex/S~)=[-l/(n+lll1og(tr' g-I I-log B (51

where g- I is the term relative to the applied stress wave-form given by Eq.(6).

t2
g-l=l {cr (tl/cr me,,}n/Adt (61
t,

According to Eq. (5) and from all the fatigue test data obtained, S~ and g -,
could be calculated; then by plotting logarithmic graphs of two expressions cr
mex/S, and t r · g - I , the fatigue parameter n could be calculated.

Appendix II Calculation of Parameter A

To introduce parameter A, the ratio LI A = Ac / As was used where the A

value representing static fatigue was denoted as As. and the A value rep-
resenting the cyclic fatigue as Ac • Eq. (2) was solved with the value A,
resulting in Eq.(7):

499
 A= [2/(n-Zl] (K,c"'/Y"" (j ,,,o,,2·t,'g-')(S/(j me><)r.-2 (7)
With As and A c denoting static fatigue for A and cyclic fatigue for A,
respectively, to obtain .1 A. Its logarithmic expression is found in Eq. (8).
log.1 A=log{t,Js-log{t,' g I }(;+A'
where,

In the case of static fatigue, g=1. If it is assumed that approximately S=S"

Eq.(8) represents the distance, in the direction of the horizontal axis, between
the approximated linear cyclic fatigue and the approximated linear static
fatigue at (j n. ,,/S ,=1.0, plotted on a graph of log( (j '" C ,,/S rl and log! t,' g- I ).
f

REFERENCES

1) M. Takatsu, J. Takahashi, T.Nishikawa, K.Ohya and A.Hattori,J.Ceram.Soc.Jpn.,

98,1343-48(1990)
2) T. Yamamoto, H.Igarashi and K.Okazaki, Ferroelectrics,50, 273-78 (1983)
3) K.Mehta and A.V.Virkal', J. Am. Ceram. Soc., 73,567-74(1990)
4) J.G.Bruce, W.W.Gerberi,ch and B.G.Koepke, in "Fracture Mechanics of
CeramIcs, \'01.4, Ed. by R.C. Bradt, D.P.Ii. Hasselman and F.F. Lange,
p.687-709, Plenum Press, New York, (1978)
5) S. W.Freiman, K.R.t-1cKinney and H.L.Smith, "Fracture Mechanics of Ceramics,
yoI.4, Ed. by R.C. Bradt, D.P.H. Hasselman and F.F. Lange, p.659-76, Plenum
Press, Ne'" York, (1978)
6) R.F.Caldwell and R.C.Bradt, J.Am.Ceram.Soc.,60, 168-70(1977)
7) H.Kishimoto, A.Veno and H.Kawamoto,J.Soc.Mat.Jpn.,36, 1122-1127(1987)
8) S.Tanaka, N.Okabe and Y.Ishimaru, ibid., 38, 137-43(1989)
9) T.KaKakubo, Dr. Theme, Tokyo Institute of Technology,(1988)
10) t-I.Takatsu, K.Ohya and M.Ando, J.Ceram.Soc.Jpn.,98, ·190-98(1990)
11) H.Kamiya, !'1.takatsu, K.Ohya, !'1.Ando and A.Hattori,ibid" 98, 456-63(1990)
12) T.Yamamoto, H.Igarashi and K.Okazaki,CERAmCS International,11,75-79
(1985)
13) S.-B.Kim, D.-Y.Kim, J.-J.Kim and S.-H.Cho,J.Am.Ceram.Soc., 73,161-63(1990)
14) T.Okada and <:i.Sines, ibid., 66, 719-25(1983)
15) G.Grathwohl, Mat.-wiss.u.Werkstofftech., 19, 113! 1988)
16) D.Lewis and R.W.Rice, Ceram.Eng.Sci.Proc., 3, 714(1982)
17) D.Lewis, Ceram.Eng.Sci.Proc., 4, 874(1983)
18) R.C.Pohanka, S.W.Freiman, K.Okazaki and S.Tashiro in "Fracture Mechanics
of Ceramics, vol.5" Ed. by R.C.Bradt, A.G.Evans, D.P.H.Hasselman
and F.F.Lange, p.353-364 Plenum Press, New York, (1983)
19) G.G.Pisarenko, V.M.Chushko and S.P.Kovalev, J.Am.Ceram. Soc., 68,
259-65(1985)

500
CRACK GROWTH BEHAVIOR OF SINTERED SILICON NITRIDE

SUBJECTED TO CYCLIC LOADING

L.X.Zeng and Z.D.Guan

Department of Materials Science and Engineering
Tsinghua University, Beijing 100084, P. R. China

ABSTRACT

Cyclic fatigue behavior of pressureless sintered Si JN 4 was investigated at room

temperature and 1050t . Three-point bending specimens with Knoop
indentation-induced flaws, at the center of tension side, were tested under cyclic load.
Specimens were subjected to sinusoidal cyclic stress with a stress ratio of R = 0.1 and
frequencies of 15Hz for room temperature and 10Hz for 1050t. It demonstratrs at
room temperature, specimens behaved brittle fracture, no SCG was observed. While at
1050t , the results are quite different. The crack growth rate showed three
characterisic regions having a plateau at 70% to 90% of the fracture toughness, which
suggest a possible intergranular stress corrosion cracking mechanism resembling that
in glass or alumina. Paris exponents for each region are 32.5, 11.1, and 35.4,
respectively. The threshold value of stress intensity factor range, AK..1h' for fracture
initiation in cyclic loading is found about 60% of fracture toughness. ratigue lifetime
10gN r is found to be associated with the initial crack driving force 10gAK I by linear
relation, resembling that in static fatigue.

INTRODUCTION
With the consideration of reliability of ceramic materials in engineering design,
researchers have given more attention to lifetime prediction. Evaluation of fatigue
behavior is essential to lifetime prediction of materials. Generally, it has widely been
accepted that ceramics are simply immune to cyclic fatigue. However, recent studies on
A1 20 J, Zr02-AI20J' TZP, and Si JN 4 indicate (1-4) that lifetime under cyclic fatigue
are much more shorter compared to that under static loading. In one of. his researches,
A.G.Evans (J) concluded that for WC cutting tool material, the crack growth rate
da / dN was determined by average and maximum values of K 1; in researches on
ceramics and there c9mpounds, include Mf.0~ Y20 J-PSZ, AI 20 J, HPSN, and SiC
reinforced Si~N4' Suresh and his coworkers (-12 found type I fatigue crack growth
behavior similar to that found in metallic materials.

More recently, Dauskardt et. at. ( J3) conducted cyclic fatigue tests under
tension-tension loads to MgO-PSZ to find that, as in metals, crack growth rate
da / dN can be fitted to a conventional Paris law relationships (4) :

da = A(AK )m (1)
dN I

Fracture Mechanics of Ceramics, Vol. 9

Edited by R.C. Bradt et ai., Plenum Press, New York, 1992 501
 However, the Paris exponent m in the range of 21 to 42 is significantly larger than
that for metals, which is reported in the range 2 to 4.

So far, only Ritcher, Dauskardt et. al. provided a series of comprehensive data
showing relationship between da / dN and AK for Mgo-PSZ ceramics. No data has
been reported for cyclic crack growth behavior under elevated temperature, on the
other hand, most of the studies were conducted with large cracks, while the situation is
that cracks existing in ceramics are small, usually smaller than lOOLlm in practice.
Recently comparisons of small and large cracks for Al-Li alloy (IS. 16 and
Mgo-PSZ ceramics (17) shows that small cracks extend more rapidly, say, about 2 to
3 orders faster than large ones. Therefore, it is better to evaluate cyclic crack growth
behavior with small cracks.

With the further development of materials science, researchers recognized that it

is essential to evaluate properties of ceramics under cyclic fatigue condition, especially
at high temperature, with small cracks in order to realize reliable application of high
performance ceramics.

Sintered Si 3N. exhibits excellent mechanical properties and, thus is a promising

candidate material for heat engine application, where materials are required to sustain
at about lOOOt and subject to cyclic loading. In the present study, cyclic fatigue
behavior of sintered Si3N. was evaluated at room temperature and l050t with the
introduction of artificial small cracks.

EXPERIMENTAL PROCEDURE

Materials
The material studies was a pressureless sintered Si 3N., with additives of Al 20 3
and Y 203' Some of the properties are listed in Table I . Specimens were rectangular
bars with dimensions approximately 5 by 5 by 50mm, tension sides were polishing to
grit 0.5jlm. All specimens is then subjected to air annealing at lOOOt for Ihr.

Table 1. Some Characteristic Parameters for Presented Material

Ur (MPa) KJ(' (MPa'-' m) Parameters for Indentation

R.T. I 1200t R.T. I 1200t ale I Y. I Ir
770 I 309 I 6.45 0.85 I 1.258 I 0.0533

Knoop indentation induced flaw was introduced at the center of specimen tension
side, Knoop indenter sustained at 31N to 45N for 30 minutes. Cracks thus created
range between 84jlm to 120jlm, which is comparable to those exist in ceramics.

Cyclic Fatigue Tests

Cyclic fatigue tests were conducted in 3-point bending with a span of 40mm at
room temperature and 1050t in ambient air atmosphere using Instron 1343
electro-serve-hydraulic testing machine. Specimens were subjected to sinusodial cyclic
stress with a stress ratio of R =0.1 and frequencies of 15Hz for room temperature and
10Hz for l050t . For tests at high temperature, an electric-resistance furnace was
used. Metallic fixtures contact with specimen directly were replaced by that made from
SiC ceramics.

Stress intensity factor were calculated using the following equations (IB, 19) :

(2)

502
 (3)

where a and c are crack depth and half-length, respectively; P is indentation load;
O'mu and O'min are maximum and minimum value of cyclic stress; Y a is geometric
factor of semi-elliptical surface flaw; and Xr is a dimensionless constant which
characterizes the magnitude of residual stress about indentation.

For semi-elliptical surface flaws (Knoop indentation flaws), some ~B:ers gave
constant values of a / c ratio of 0.85 and Y a value of 1.258 for Si 3N.' 2 ) , crack
lengths were measured as the projected lengths normal to the bending tensile stress
using optical microscopy. In this process, detection of crack increment of 2pm was
possible.

RESULTS AND DISCUSSIONS

Cyclic Loading Tests at Room Temperature

Crack extension behavior results of sintered Si 3N 4 under cyclic loading condition

at room temperature are listed in Table n . Tests were conducted with frequency of
15Hz and a stress ratio of 0.1, maximum stresses were in the range of 280MPa to
350Mpa. In this area of stress, all the specimens tested show brittle fracture behavior.
No crack extension was observed before and after fracture, which means no fatigue
behavior for this sintered Si 3N 4 ceramics under cyclic loading at room temperature.

Table n. Results of Cyclic Loading Tests at Room Temperature

O'max Crack Length 2c(pm) No. of Experimental

~
(MPa) Initial Final Cycles Phenomena
1 300 205 Fracture 15340 No Crack Extension
2 300 212 Fracture 35950 No Crack Extension
3 280 220 222 30000 Unfailure
205 23000
4 280 203 No Crack Extension
Fracture 26580
172 50000
5 350 172 No Crack Extension
Fracture 62000
202 38000
200 No Crack Extension
Fracture 44780
6 280
201 38000
210 No Crack Crack Extension
203 44780
205 10000
205 207 15000 No Crack Extension
7 300 207 17810
212 15000
210 No Crack Extension
Fracture 17810

Cyclic Loading Tests at 1050t

Cyclic loading tests at 1050t were performed with a frequency of 10Hz and a
stress ratio Of 0.1. Crack extension data and the results obtained from formula (2) were
listed in Table ill, which was also shown schematically in Figure 1. It is obvious that
this plot of crack gowth rate da / dN vs ilK) is similar to that of ceramic materials

503
under static loading and that of metallic materials under cyclic loading. The plot
shows three characteristic re.ijions with a plateau portion at from 70% to 90% of the
fracture toughness. Glass (2 and oxide ceramics OS) were reported to also have
plateaus at this area, and these crack growth rates were proven to be associated with
stress corrosion cracking. The sintered Si JN 4 ceramics currently studied has a glassy
phase in its grain boundaries. The cyclic fatigue mechanism at t050t is considered,
then, to be due to stress corrosion cracking. In three regions, crack growth rates can
each be fitted to Paris law relationship. Numerical analysis gives the following
relationship for each region:

:~ = 7.08 x 10 -J\~K/2.5

:~ = 1.08 x 10 -4 (~K/I.I
:~ = 6.92 x 10 -39(~K/s.4

Paris exponents for regions I and ill of 32.5 and 35.4 indicate more susceptible
to cyclic fatigue of crack growth rate in ceramics comparing with metallic materials.

Tableill. Results of Cyclic Loading Tests at 1200t

a mu ao a N ~K da/dN
.N9 (MPa) (}lm) (}lm) (cycles) (MPa~) (m/ cycle)
1 480 88.8 126.0 430 5.632 8.65x to-8
2 460 95.2 114.0 2030 5.327 9.26x 10-9
3 400 93.9 100.3 2030 4.450 3.15x 10-9
4 400 92.2 104.1 2030 4.472 5.86 x 10-9
5 440 93.9 139.0 880 5.376 5.13 x 10 8
6 364 96.5 127.0 11920 4.337 2.73 x 10-9
7 347 84.2 111,4 248990 3.885 1.09 x 10 10
8 347 86.7 101.2 248990 3.800 5.82 x 10 II
9 373 89.7 153.0 31080 4.615 2.04x 10-9
10 373 88.8 98.2 31080 4.084 3.02 x 10- 10
II 351 90.1 99.9 240930 3.873 4.07 x 10- 11
12 351 85.0 93.5 240930 3.750 3.53 x 10-11
13 351 90.5 97.3 240930 3.850 2.82 x 10-11
14 420 95.2 160.7 , 4450 5.379 1.47 x 10 8
15 364 98.6 106.3 4450 4.171 1.73 x 10-9
16 364 93.5 105.8 4450 4.113 2.76 x 10-9
17 445 87.1 166.0 170 5.668 4.64x 10 7
18 435 95.6 132.0 1910 5.254 1.91 x to-8
19 393 93.1 142.0 10180 4.831 4.80 x 10-9
20 427 118.2 175.0 80 5.854 7.10x to-7
21 427 108.4 163.0 340 5.632 1.61 x 10-7
22 400 112.2 148.0 5400 5.166 6.63 x 10-9
23 347 110.5 115.6 5400 4.174 9.44 x 10-10
24 390 105.0 126.0 5940 4.745 3.54 x 10-9
25 338 103.3 106.3 5940 3.917 5.01 x 10- 10

504
 10-6

-~
U
>.
t)
10-1

"S
'-' 10-8
0
0

Z 0
0

"0 0 o 0

"~
"0
10-9

10-1<
.:
0

456
AK, (Mpa.Jol)
da
Fig. 1 dN - AK.curves for SSN at 1050t

L;-
0
00

0
0

~
~
::E 5 n= 15.9
'-' A = 4.32 X 10 14
~ r=0.878
<I 0
0

4
10 1 10 2 103 104 lOS
N r (Cycles)
Fig. 2 AK,- N r Relationship for SSN at 1050t

An apparent threshold AK 1h is found to be approximately 60% of K,c, below

which crack growth is presumed dormant, i.e., slower than 10-lom / cycle.

Relationship between initial stress intensity range AK I and cyclic fatigue lifetime
N r is shown in Figure 2. It can be well fitted to equation (4):

(4)

Which is comparable to the relationship of ceramics under static fatigue

condition. Hence, the same conclusion can be drawn that linear relation exists between
logAK, and logN r.

505
CONCLUSIONS

Cyclic loading tests were performed for pressureless sintered Si3N 4 at room
temperature and 1050t. Crack growth behavior was studied with the introduction of
Knoop indentation-induced flaws. Frequencies were 15Hz for room temperature and
10Hz for 1050t, stress ratio was R =0.1. The following conclusions can be made:
(1) No cyclic loading effect was observed for sintered Si3N4 ceramics at room
temperature, only brittle fracture behavior was found.

(2) Curve of da/ dN vs AK, at 1050t resembles that of ceramics under static
loading and that of metallic materials under cyclic loading. The plot shows three
characteristic regions with a plateau portion at from 70% to 90% of the fracture
toughness. Indicates the cyclic fatigue mechanism at 1050t to be due to stress
corrosion cracking.
(3) An apparent threshold AK lh is found to be approximately 60% of K)c, below
which, crack growth is presumed dormant.

(4) Paris exponents for each stage of da / dN vs AK) curve were calculated. The
values for regions I and ill of 32.5 and 35.4 indicate more susceptible of crack growth
for sintered Si 3N 4 to AK).

(5) Plot of AK) vs cyclic fatigue lifetime N r shows linear relation between
10gAK) and 10gNr. It can be fitted to formula (4).

REFERENCES
(I) A.G.Evans and M.Linzer, Int. J. Fract., 12 (1976) 217
(2) T.Kawakubo and K.Komeya, J. Am. Ceram. Soc., 70 (1987) 400
(3) S.Horibe, J. Mater. Sci. Lett., 7 (1988) 725
(4) T.Hoshide, T.Ohara, and T.Yamada, Int. J. Fract., 37 (1988) 47
(5) R.H.Dauskardt, et. at, J. Am. Ceram. Soc., 70 (1987) 248
(6) L.Ewart and S.Suresh, 1. Mater. Sci. Lett., 5 (1986) 774
(7) L.Ewart and S.Suresh, J. Mater. Sci., 22 (1987) 1173
(8) S,Suresh, Engi. Fract. Mech., 21 (1985) 453
(9) S.Suresh and L.A.Sylva, Mater. Sci. Engi., 83 (1986) L7
(10) J.R.Brockenbrough and S.Suresh, J. Mech, Phys. Solids, 35 (1987) 721
(11) S.Suresh and lR.Brockenbrough, Acta Metall., 36 (1988)
(12) S.Suresh, L.X.Han, et.a1., J. Am. Ceram. Soc., 71 (1988) C-185-C-161
(13) S.Suresh, L.Ewart, et.al., J. Mater. Sci., 22 (1987) 1271
(14) P.Paris and F.Erdogan, J. Bas. Engi., 85 (1963) 527
(15) K.T.Venkateswara Rao and R.O.Ritchie, "Fatigue-Crack Propagation in
Advanced Aerospace Materials: Aluminum-Lithium Alloys·, Paper Collection
(16) K.T.Venkateswara Rao, et.al, Engi. Fract. Mech., 31 (1988) 623-35
(17) A.A.Steffen, R.H.Dauskardt, and R.O.Ritchie, to be published
(18) J.J.Petrovic,1. Am. Ceram. Soc., 66 (1983) 277
(19) D.B.Marshall, B.R.Lawn, et.al., J. Am. Ceram. Soc., 64 (1981) 539
(20) G.D.Quinn and J.B.Quinn; pp.603-36 in "Fracture Mechanics of Ceramics·
Vo1.6. R.C.Bradt, A.G.Evans, et.al., eds.
(21) J.H.Gong and Z.D.Guan, J. Chinese Ceram. Soc., 19(1991) 234
(22) J.H.Gong and Z.D.Guan, "Effect of Residual Stress due to Knoop Indentation
on Subcritical Crack Growth Behavior in Ceramics·; this volume
(23) Y.Y.Zhao, Diplomatic Thesis, Tsinghua University (1990)
(24) S.M.Wiederhom, J. Am. Ceram. Soc., 50 (1967) 407
(25) A.G.Evans, J. Mater. ScL, 7 (1972) 1137

506
CRACK GROWTH IN ZIRCONIA BEARING CERAMICS UNDER CYCLIC
LOADING

Kai Duan, Brian Cotterell, and Yiu-Wing Mai

Centre for Advanced Materials Technology

University of Sydney
N.S.W.2006
Australia

INTRODUCTION

Fatigue of ceramics due to cyclic loading as distinct from static fatigue due to
environmental effects was until recently thought impossible because of the absence of
appreciable crack tip plasticity (Evans, 1980). A substantial and growing body of
evidence now indicates that true cyclic fatigue may be possible in a wide range of
ceramics, for example, Guiu (1976), Ko (1986), Dauskardt et al (1987, 1989, 1990),
Hoshide et al (1988), Sylva and Suresh (1989), and Davidson et al (1991). Evidence for
true cyclic fatigue has also come from tests performed under cyclic compression (Ewart
and Suresh, 1986, 1987). However, a significant portion of crack growth under cyclic
loading in air or other reactive atmospheres is due to environmentally-assisted slow
crack growth. For true cyclic fatigue there must be some form of hysteresis whereby
energy must be dissipated during cycling. Hysteresis effects have been demonstrated
for several transformation-toughened ceramics (Bowman et aI, 1986). Such behaviour
is not confined to transformation-toughened ceramics, but is likely to be more marked
in the tougher ceramics.

The crack growth rates of partially stabilized zirconia (PSZ) are greatly affected
by the formation of a dilatant transformed zone that shields the crack tip. Since both
true cyclic fatigue and environmentally-assisted subcritical crack growth depend on
the state of stress at the crack tip, shielding in these ceramics decreases the rate of
crack growth (Li and Pabst, 1980; Lenz and Heuer, 1982; Jensen et al, 1989; Sylva
and Suresh, 1989; Dauskardt et al, 1990). However, there have been few quantitative
analyses of the effect of crack shielding. Dauskardt et al (1990), assuming that crack
growth is entirely due to true cyclic fatigue, have considered the effect of abrupt
changes in the stress intensity factor range on the crack growth rates using a simplified

Froclure Mechanics of Ceramics. Vol. 9

Edited by R.C. Bradt el al.• Plenum Press. New York, 1992 507
analysis whereby the transformed zone is represented by a series of flats and circles
estimated from the applied stress intensity factor. They also assume that following a
sudden increase in applied stress intensity factor that there is no immediate change in
the shielding of the crack tip, we do not follow the logic of this assumption. The exact
transformed zone, assuming that the transformation is triggered by a critical
hydrostatic stress value, can only be obtained by iteration (Amazigo and Budiansky,
1988; Stump and Budiansky, 1989), and the size of the zone is overestimated if only
the stress due to the applied stress intensity factor is considered. However, at the
lower stresses used in cyclic fatigue the overestimation of the transformed zone is not
very significant. We have shown that the effect of crack tip shielding on the static
fatigue of transformation-toughened ceramics can be predicted from an estimation of
the transformed zone obtained from the applied stress intensity factor (Duan et aI,
1991). In this method the non-dimensional parameter w given by

w = (1 + v)EOT / a~(1-v) (1)

that defines the transformation toughening process is obtained from the ratio of the
fracture toughness at crack initiation K~c (obtained from the fracture toughness of the

non-toughened ceramic) to the plateau value of the fracture toughness Kic.

In this present paper we explore the significance of environmental slow crack

growth on the cyclic fatigue of transformation-toughened ceramics. We assume that
true cyclic fatigue is not very significant in non-transforming ceramics and use the
data from overaged PSZ ceramics to estimate the crack growth rate as a function of
the crack tip stress intensity factor K tip . With this crack growth law the rate of crack
growth is predicted, for the same ceramic heat treated to obtain transformation
toughening, on the assumption that there is no crack growth due to true cyclic fatigue
using similar analysis to our earlier paper (Duan et al, 1991) to indicate the
significance of true cyclic fatigue.

AN APPROXIMATE R-CURVE FOR TRANSFORMATION-TOUGHENED

CERAMICS

The crack tip of a transformation-toughened ceramic is shielded by the

transformed region which undergoes a dilatant transformation OT. The effect of the
dilation can be obtained by integrating the expression obtained by Hutchinson (1974)
and the expression for the actual stress intensity factor at a crack tip K " is given by
t lp

508
 K. = K
tIp a
+ EO
T
3{i 11'(1 - II)
f A f r-3/2 cos ~ ¢dA , (2)

where K is the applied or far field stress intensity factor and the integral is taken over
a
the transformed region. It is usually assumed that the martensitic transformation
occurs when the hydrostatic stress reaches a critical value (McMeeking and Evans,
1982; Budiansky et aI, 1983), though the maximum principal stress has also been used
as a criterion (Lambropoulos, 1986). The hydrostatic stress, assuming the crack tip is
in a state of plane strain, is given by

O'~ =
Ka (1 3+ II) [21iR]! cos ¢/2 + f f A F(z,zo)dxodyo (3)

where z = (x + iy) and

F( z z ) =U [1 + II] Re { 1 + 1 }
, 0 1811' 1 - II V(zzo)[v'Z + ~)12 V(zzo)[v'Z + ~12 '

Rand ¢ are defined in Fig. 1, and the integral is taken over the transformed region.

Because Eqn. (3) does not give the transformed zone explicitly, Budiansky et al
(1983) have assumed that the hydrostatic stress can be approximated by the first term.
This assumption leads to an overestimate of the transformed region as has been shown
by their later work which includes the second term (Amazigo and Budiansky, 1988;
Stump and Budiansky, 1989). However, it is necessary to solve a nonlinear integral
equation to determine the "exact" shape of the transformed zone. For application to
fatigue it is desirable to have a simpler algorithm. Here we assume that the
hydrostatic stress can be approximated simply by the first term in Eqn. (3). For
steady state crack growth the crack tip stress intensity factor K is equal to the
tip
fracture toughness K~c of the equivalent non-toughened ceramic and the ratio of K~c

to the plateau value of the stress intensity factor K can be written as (Budiansky et
rc
al, 1983)

K~c/KIc =1- w/4.;3 11' (4)

where w is the nondimensional parameter that defines the transformation toughening

process. The approximate R-<:urves for K~c/KIc = 0.62 is compared with the "exact"
curve in Fig. 2. The R-<:urves are modelled reasonably well by the approximate
method for

509
 y

a - - -__ ~I--- t13. ---I~

Fig. 1. The development of the transformed region at a crack tip.

2r------------------------------,
1.8

1.6 ..... - .. .----------------------------------------------------

1.2

- - - Exact
Approximate
0.8 l- -'- ---''-- -'- ---' ......L..... --'

o 10 20 30 40 50 60
L:alL
Fig. 2. Comparison of an approximate R-eurve with the "exact" one
(K~c/Kic = 0.62).

510
 (5)

SLOW CRACK GROWTH UNDER CYCLIC LOADING

To a first approximation the crack growth rate in a transformation-toughened
ceramic can be separated into two independent parts: one a time dependent crack
growth due to environmentally-assisted crack growth which depends only on the
shielded crack tip stress intensity factor K tip and the other a cycle-dependent crack

growth that depends mainly on the effective crack tip stress intensity factor range
LiK · which allows for crack closure (Dauskardt et al, 1990; Davidson et al, 1991).
t Ip,e
Thus

(6)

where A,n,m are constants, B depends on Ktip,max' and f is the frequency of loading,

Our analysis concentrates on the first term which is assumed to be dominant in

non-transforming overaged PSZ ceramics. It is assumed, in common with Dauskardt
et al (1990), that the maximum applied stress intensity factor determines the size of
the transformed region at the crack tip. Since the crack tip stress intensity factor
depends on both the applied stress intensity factor and the amount of crack growth,
the rate of crack growth is not a unique function of the applied stress intensity factor
but, apart from a transition region after a sudden change in load (which we consider
later), the dependence of crack growth on the initial starting conditions is slight. It is
observed that there is a threshold value for the crack tip stress intensity factor Ktip,th

below which there is no crack growth. Since the exponents in the crack growth
expressions are large, the precise value of the threshold has little effect providing the
stress intensity factor is significantly greater than the threshold value.

For equilibrium crack growth at a constant applied stress intensity factor range,
the frontal portion of the boundary to the transformed zone can be approximated by
the critical hydrostatic stress due to the applied stress intensity factor. In the wake of
the crack tip the width of the transformed zone is determined by the maximum width
of the frontal zone. From Budiansky et al (1983) we obtain the approximate
expression for the equilibrium crack tip stress intensity factor in terms of the applied
stress intensity factor K

K Ip
, =K a -(w/8{J7r)K max. (7)
t

511
Crack closure is neglected in our analysis. This neglect should not cause significant
errors for the same reason that the precise value of the threshold stress intensity factor
is comparatively unimportant. The equilibrium crack growth per cycle can be found
by integration (neglecting the second term in Eqn. 6) and can be expressed in terms of
the applied stress intensity range. Thus

da/dN = A¢[~K/(l- R)]n/f (8)

where ¢ is a function of w,R and K t Ip,

· th/Kt·Ip,max .
We have also considered the case where there is a sudden increase or decrease in
applied stress intensity factor, which causes a transition in the crack growth rates. In
this case the shielding of the crack tip is determined numerically.

COMPARISON OF PREDICTIONS WITH EXPERIMENTAL DATA

Dauskardt et al (1987, 1990) have performed a series of cyclic fatigue

experiments on 9% mol Mg stabilized PSZ ceramics. We have used their results for
the overaged specimens, where there is negligible shielding of the crack tip to calculate
the values of the constant A and the exponent n in Eqn. 6 that give the best fit to the
results (see Fig. 3; A = 10-10A, n = 16.1), assuming that none of the crack growth is
due to true cyclic fatigue, and that the threshold value of the crack tip stress intensity
factor is 1.8 MPa m t as stated by Dauskardt et al (1990). The crack growth rate
deduced from the cyclic fatigue data of Dauskardt et al (1990) is compared with static
fatigue data for similar overaged Mg-PSZ in Fig. 4. There is a large difference in the
crack growth rates measured by Becher (1986) for a 7.2% mol fraction of Mg and
Swain (1986) for a 12% mol fraction, but it can be concluded that the crack growth
rate obtained from Dauskardt's et al (1990) cyclic fatigue data on the assumption that
none of the crack growth is due to true cyclic fatigue is reasonable. The results from
the overaged Mg-PSZ have been used to predict the crack growth rates shown in Fig.
3 for as-fired and two commercial grade Mg-PSZ heat treated to obtain
mid-toughness (MS) and peak toughness (TS) using the initiation and plateau
toughnesses given by Dauskardt et al (1990). The predicted results agree well with the
results for the as-fired ceramic, but underestimate the crack growth rates for the two
tougher MS and TS grades. Hence it appears that true cyclic fatigue becomes more
important as the r-eurve behaviour becomes more pronounced.

The predicted crack growth rate changes due to abrupt changes in the applied
stress intensity factor range are given for the experiments of Dauskardt et at (1990) in
Fig. 5. Since the steady state crack propagation rates are underestimated by
predictions based on the neglect of true cyclic fatigue, the crack growth rates

512
 lE·OS

U lE·06
Predicted

averaged As-Fired MS 6 - TS

:-/
>. 6
~
E t2'

--
~ lE·07 6

y.
•
"'0
co
"'0 1E.08

ro
Q)

a:
.t=
lE.09

~ 0 0
0
<5 lE-lO 0 9J
.:t:
()

o IE-11
ell

K~h=1.8 MPa .ffff

lE·12
1 2 3 S 10 20
Stress Intensity Range, DK (MPa Ei)

Fig. 3. Predicted steady crack growth rates for three Mg-PSZ ceramics.

0.01
a Swain·s data
0.001
U
Q)
6 Becher's data
.!!? 0.0001
E
-0 lE·OS
a
co
"'0
lE-06
o
ro $
Q)

a: lE-07
.t=
~
e lE·08 ~
<.9
.:t: lE-09
()

~
0 lE·l0

lE·l1
2 3 S
Stress Intensity Factor, K (MPa ftf)

Fig. 4. Comparison of crack growth rate deduced from cyclic fatigue data with
static fatigue data.

513
 (a)

o
>,
~
E
- 0,001
Z
"0
""ill
"0

m
Q) lE·07 \~_._-_.",
"'- ....0-9~€T.-D·--€T'
a:
.c. .".----+~e::.....---,r---
~ IE·l1
e
o
.::£.
g IE·1S T5 Mg·P5Z Data
.• - -G'_.
(j Predicted

1E.19 L.... -'-- --'- "'- -'

o 2 4 6 8
Crack EXlension.6a ( mm )

(b)
0.0001

lE·OS
0
>,
~ 1E·06
E
Z lE·07 l:lK= 5,48 L'.K=5.30 L'.K=5.60
"0
""ill
"0

m
Q)
1E·08

0-----0-- &--0-~,o--- 0> -- --

~'&-O
'L
a: 1E·Q9
.c.
~ lE·10
0
'-
(9

r
.::£. IE·l1 MS Mg·PSZ data
0
(1J ··-G-_·
(j lE·12 Predicted

lE·13
0 234 S 6 7
Crack EXlension,t.a ( mm)

Fig. 5. Transient cyclic fatigue growth in peak toughness (TS) Mg-PSZ

showing (a) Transient crack growth following a load reduction and a
single cycle overload, (b) Transient crack growth subsequent to a load
reduction followed by a load increase.

514
predicted for these tests are similarly under--estimated. Qualitatively the changes
observed are predicted by the model, but the predictions show a much smaller
transition region with a much faster return to steady state crack propagation being
predicted than observed.

CONCLUSIONS

It is shown that the crack growth due to cyclic fatigue of weakly-toughened

Mg-PSZ ceramics can be predicted if it is assumed that all the crack growth is due to
environmental slow crack growth and that no crack growth is due to the cyclic nature
of the applied stress intensity factor. However, for tougher Mg-PSZ, a significant
portion of the crack growth is due to true cyclic fatigue.

The transitions in crack growth rates in tough Mg-PSZ ceramics due to abrupt
changes in the applied stress intensity factor range are predicted qualitatively if it is
assumed that no crack growth is due to true fatigue, but the predictions are not
quantitatively accurate.

ACKNOWLEDGEMENTS

The authors wish to thank the Australian Research Council for the continuing
support of this work. One of us (D.K.) is supported by a CSIROjSydney University
Research Scholarship and a Junior Research Fellowship.

REFERENCES

Amazigo, J.C. and Budiansky, B., 1988, Small flaw static fatigue crack growth in
Mg-PSZ, J. Mater. Sci. Lett., 8:1154.
Bowman, K.J., Reyes-Morel, P.E. and Chen, I.-W., 1986, Reversible transformation
plasticity in uniaxial tension-eompression cycling of Mg-PSZ, in "Materials
Research Society Symposium Proceedings on Advanced Ceramics", P.F. Becher,
M.V. Swain, and S. Somiya, eds, Materials Research Society, Pittsburgh.
Budiansky, B., Hutchinson, J.W. and Lambropoulos, J.C., 1983, Continuum theory of
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propagation in magnesia-partially-stabilized zirconia ceramics, J. Am. Ceram.
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515
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516
FATIGUE BEHAVIOR OF SINTERED Si3N4 UNDER
ROTARY BENDING AND STATIC FATIGUE

H.N. Ko
Nakanihon Automotive College
Sakahogi-cho, Kamo-gun, Gifu-ken, Japan 505

ABSTRACT
Rotary bending and static fatigue tests were carried out at room
temperature on sintered Si3N4 whose diameters were 8 and 6 mm. An Ooo's
rotary bending fatigue testing machine was used on the operating condition
of 3420 cycles per minute. The rotary bending test was performed within
the range 104 to 109 stress-cycles. Besides. the static fatigue test was
performed for less than 107 seconds using the non-rotating fatigue machine.
The fatigue behavior under rotary bending was different from that under
static fatigue. The value of n under rotary bending was much smaller than
that under static fatigue, in the expressions of an N = constant and
an t = constant, and the assumed fatigue limit for the former was lower
than that for the latter. However, both assumed fatigue limits showed the
similar relationships between the strengths and the specimen sizes. The
characteristic appearance of mirror-like regions on the fractured surfaces
after both fatigue tests were almost the same as those after the static
test. The size of each mirror-like region was found to have stronger
correlation with the applied stress than with the loading condition.
Stress intensity factor at the deepest point in the mirror-like region
was also nearly constant. No remarkable difference between fatigue
fractured morphology and static fractured one could be found even under
microscopic observation. The existence of the fatigue limit, the basic
character of rotary bending strength, the size effect on the assumed
fatigue limit and the fatigue fracture features are discussed on the basis
of the results.

INTRODUCTION
It is important to know the fatigue behavior of ceramics when using
them as structural components, since the fatigue strength is generally
lower than the static strength. Their behavior has already been examined
in the various types of loading, and it is known that for some ceramics
the fatigue strength depends on the loading condition such as the applied
stress state. However. basic data are not sufficient. More information
on factors affecting fatigue strength seems to be necessary to clarify the
fatigue fracture mechanism of ceramics and their reliability as structural
materials.

Fracture Mechanics of Ceramics, Vol. 9

Edited by R.C. Bradt et al., Plenum Press, New York, 1992 517
 Rotary bending and static fatigue tests were carried out on sintered
Si3N4 at room temperature to study the effect of loading conditions on the
fatigue behavior. The fatigue behavior of sintered Si3N4 under rotary
bending was examined in the previous studies [1-3]. In the present study.
sintered Si3N4 whose strength was much higher than the previous sintered
Si3N4 was tested. and the basic character of rotary bending fatigue
strength was studied. The rotary bending test was performed within the
range 104 to 109 stress-cycles. and the existence of a knee was examined.
The test results were compared with the static fatigue strength measured
for a fairly long period by the non-rotating fatigue machine.
The size effect on the fatigue strength of ceramics has not been
studied much and even elementary data are few. Thus, the specimens with
small diameter were tested and the size effect on the assumed fatigue
limits was studied.
The fractured surfaces after both fatigue tests had mirror-like
regions which were similar to mirrors [4] observed on the fractured
surfaces after a static test. Mirror-like region of fractured surfaces
after the fatigue test has not been so clarified well as mirror in the
static test. Therefore. the basic character of mirror-like region was
examined to clarify the fatigue fracture features.
Based on the results. the difference and the similarity of the fatigue
behavior under rotary bending and static fatigue were discussed.

Figure 1. Specimen geometry (dimensions in mm).

EXPERIMENTAL PROCEDURE
The material used was sintered Si3N4 obtained from Kyocera(Japan).
It was fabricated with Y203 and Al203 as additives [5]. The material had
rod-shaped grains with various aspect ratios; average grain size was 1-2,um.
The geometry of specimens is shown in Fig.1. The middle part of the
specimen had a straight cylindrical shape with a constant diameter; the
diameters were 8 and 6 mm. and the straight length was 15.4 mm. Each end
of the specimen had a larger diameter of 12 mm for chucking, and the two
parts of different diameters were connected by a smooth curved surface
without generating stress concentration. The specimen was ground
perpendicularly to its axis so as to make the finished surface smooth; the
maximum roughness of the middle part of the specimen was about 1,u m.

518
 The machine used was an Dno's rotary bending fatigue testing machine
operating 3420 cycles per minute. The loading tYpe of the machine was
four-point bending. The stress state of the specimen under rotary bending
was reversed bending. The static and static fatigue tests were performed
using the non-rotating fatigue machine. The static test was performed by
increasing the appied stress gradually until the specimen was fractured.
The static fatigue test was performed by holding a constant load, and the
holding time was measured with a hand made apparatus capable of digital
display for time.
Fractured surfaces of specimens were observed by both the optical
microscope and the scanning electron microscope(SEM). The size of mirror-
like region was determined by the optical microscope with a magnification
of 25, in the same manner as the previous study [1].

RESULTS AND DISCUSSION

Rotary Bending Fatigue Strength
Fatigue testing was carried out generally for two specimens at each
stress level and within the range 104 to 108 stress-cycles. Some
specimens were tested at cyclic numbers more than 108 to examine the
existence of a knee; 108 stress-cycles is equivalent to about 20 days
under the present test condition. Test points for different diameters,
denoted by the symbols () and ~ , are plotted together on a semilogari-
thmic graph. The S-N curves obtained are shown in Fig.2; the arrowed
points indicate those for which testing was stopped. It is known that the
fatigue strength for small diameter is higher than that for large diameter.
The material has the character that its life increases remarkably as the
stress amplitude decreases. In addition, the material does not show a
distinct knee at cyclic numbers less than 107 in any case. Three speci-
mens with 8 rom diameter are fractured at 1.02x107 , 3.75x10 7 and 1.23x108
stress-cycles which are equivalent to about 2, 8 and 25 days, respectively,

540
520
.....--r--r--rrr
1--+-++++.........
II
I::>~ r-....... I::>
,1+
----;r-++
I --+-++--H-++It--+-I-+t~

500 I-+-H-I+ --++;-t+t-ltf-=::::";"q-j-tt1+1t---fl'J. I::> -H++

t! ..'80 I--++++I~
~ u~1
K-o·
--...
I::>
ex)
1::>"-+++tittF"~'l-t+iifl:
-. l'J.
11111'l--1+-+++
rll::> t:v
~ 460 f- 0 ~""'If-+++l+f~A».~ t:v - l'J.
o 440 _+---1f-H+ttIfl-r-_O--t°-+~"I.lol::l:----t-IO g~~ ~I-: ~
0
420 1----ii-H-!+l+H-+-4--H+H*-+-+-t+ j"-.....N-. ° ~ Wt:v~:m
° N~,C»I~ 1 U
400 fo-- 0 fo--~C» ~ ~
OC» 0 ~.
380 ~
OJ> <» t»
360 f-- '"
o 8 mm II~
340 I--- OJ>
I::> 6 mm
320 f-- 111t
300 I 11111111 I --'-.1....l....U..
103 10'- lOS 1d7 loB
N

Figure 2. S-N curve.

519
while three specimens with 6 rom diameter are fractured at 1.35xl07 ,
1.56xl08 and 1.94xl0 8 stress-cycles which are equivalent to about 3, 32
and 39 days, respectively. However, from the figure, each knee seems to
exist at cyclic numbers more than 108 ; the fatigue limits seem to be about
380 and 430 MPa, respectively. A similar S-N curve, indicating the exist-
ence of a knee, was obtained in the previous studies [2,3] on sintered Si3N4
whose assumed fatigue limit was about half that of the present material.
These rotary bending test results suggest that fatigue testing should
be carried out at least for more than several tens of days for confirming
the basic fatigue strength of sintered Si3N4. Although it was reported [6]
that sintered Si3N4 was fractured at cylic numbers even more than 109 ,
this test was performed at very high frequency, 3 kHz; it took only about
4 days to obtain the data at 109 stress-cycles. As it can be considered
that frequency affects the number of cycles to failure, the specimens in
the present test, which are not fractured under a near assumed fatigue
limit, is expected not to be always fractured at cyclic numbers more than
109 . A specimen with 8 rom diameter was tested at 392 MPa up to 1.56xl09
stress-cycles using a high speed rotary bending testing machine operating
6400 cycles per minute.
S-N Curve, Including Static Bending Strength
The static bending test was performed using an Ooo's rotary bending
testing machine. The mean static bending strengths obtained were 627 MPa
for 8 rom diameter and 682 MPa for 6 rom diameter; the values were obtained
from 7 and 2 specimens, respectively. By comparison of the fatigue limit
with the static bending strength, the ratio of the former to the latter
was about 5/8 for the two. This ratio seems to be different because of the
strength of the material, in comparison with the results in the previous
studies [3,8].
As it appeared possible to correlate static bending strength with
fatigue strength, their test results were plotted together on a logarithmic
graph; the S-N curve, including static strength, is shown in Fig.3. Each
straight line in the figure was obtained by the least squares method from
the data except the arrowed points. As seen in the figure, the S-N curve
can be approximately represented by a straight line up to about 108 stress-
cycles and can be expressed by the formula:

an N = const. (1)

800 I I I I
~ 0 8 mm -
700
~-r- t: . 6 mm

-- - - --- - -- T
I
/f.
~ 600

- I
~
o 500 = ~&t::.~"" ;;;;: :::.6 6

-=
0

-.g.. i-~~~
o 00_ 'il;.6
~
400
- f; ::: ~ ~-
--
~~i
300
-
- If,08 109
,CP ,OJ 10" 105 161
N

Figure 3. S-N curve, including static bending strength.

520
where a is the stress amplitude and N is number of cycles to failure.
The exponent n for 8 rom diameter was 39.9. which was obtained from the
slope of the straight line. and the stress at N = 1 was 623 MPa. It seemed
that datum point of the straight line could be taken as the mean static
strength although the straight line for fatigue data was a little different
from that shown in the figure; the value of n for fatigue data was 49.7.
The straight line obtained for 6 rom diameter showed that the value of n was
44.8 and the stress at N=1 was 663 MPa. The similar correlation between
rotary bending strength and static strength was obtained in the previous
studies on sintered Si3N4 [2.3] and sintered A1203 [3.7,8]. It is consi-
dered that the S-N curve, including static strength, is useful for estima-
ting the fatigue strength under rotary bending.

=
700

=
If.
~
650 -
--
- 0
6
-- 6_
r-
-- 6
-r- ts>
ts>
ts>
o 600 0 o>ts>- ts>
-
=
I 0
I 0
0
o ~
- 0 8 mm r - 00'-6

I
550 I---
f- 6 6 mm
o -r- C» - i - -

II
l-
I- go>o
500
f-
0>/
10° 101 10 2 10 3 10' lOS

sec

Figure 4. S-t curve.

Static Fatigue Strength

The static fatigue test was performed mainly on the specimens with
8 rom diameter using the non-rotating fatigue machine. The test was carried
out generally for less than 10 6 seconds, and some specimens were tested for
more than 106 seconds to examine the existence of a knee. Test points
were plotted on a logarithmic graph shown in Fig.4; the arrowed points
indicate those for which testing was stopped. The size effect on static
fatigue strength was also examined as a preparatory experiment. The data
obtained for 6 rom diameter are also shown in the figure. Although the
number of data is low, it is known that the static strength for small
diameter is higher than that for large diameter. The solid straight line
for 8 rom diameter was obtained by the least squares method from the data
except the arrowed points; the interrupted line is simply drawn, assuming
that 6 rom data have nearly the same slope as 8 rom data. As seen in the
figure. the S-t curve can be approximately represented by a straight line
up to about 10 6 seconds and can be expressed by the formula:

an t = canst. (2)

where a is the applied stress and t is the time to failure. The exponent
n was 179.1. and was much larger than that under rotary bending.

521
 Fig.4 shows that the static fatigue limit. defined as the stress level
below which prolonged service life expected. seems to exist at the time
more than 106 seconds; the assumed static fatigue limits are about 540 MPa
for 8 rom diameter and 610 MPa for 6 rom diameter. A similar S-t curve.
indicating the existence of a knee, was obtained in the previous study [9]
on sintered Si3N4; the test was performed on rectangular rods. using a
four-point apparatus and a servo-hydraulic fatigue testing machine.
Comparison of Fatigue Behavior under Rotary Bending
with That under Static Fatigue
It was confirmed that the fatigue strength under rotary bending
decreased remarkably than that under static fatigue. and that the value of
n for the former was small in comparison with that for the latter; this was
expected from the previous results obtained under rotary bending [2] and
four-point bending static fatigue [9] on sintered Si3N4. The exponent n
indicates fatigue resistance of materials and also seems to indicate the
exponent in the subcritical crack velocity V against stress intensity
factor KI relation, V = A KIn. where A is a material constant. Values
for present and previous materials and literature values for each same
material are listed in Table 1. It is seen from the table that the value
obtained under rotary bending whose stress state is reversed bending is
small in comparison with that obtained by other test methods such as static
fatigue test. The similar tendency is understood. comparing the value of n
for sintered Si3N4 under tension-compression [10] with that under dynamic
fatigue [11]. It can be said that the value of n in reversed bending is
smaller than that in repeated unidirectional bending, in comparison with the
data [12] reported on sintered Si3N4 in a four-point bending fatigue test.

It seems that the fatigue behavior of precracked specimens, as well

as smooth specimens. is affected by loading conditions. in comparison with
the fatigue data reported on sintered Si3N4 with precracks due to Knoop or
Vickers indentation under reversed bending and repeated unidirectional
bending [13] or repeated unidirectional bending and static fatigue [14] in
a four-point bending fatigue test. The crack growth data [15] of compact
tension specimens, whose material is similar to sintered Si3N4 used in the
previous studies [1.2.3], show that the crack velocity under repeated
unidirectional stress is higher than that under static fatigue at the same
maximum stress intensity factor. and that the value of n for the former is
smaller than that for the latter. The similar tendency is seen in the
crack growth data [16] on sintered Si3N4 measured by constant moment
method under repeated unidirectional stress and static fatigue. It is
considered that the initiation stress for the crack growth from the initial
flaw in smooth specimens is lower under rotary bending than under static
fatigue.
It can be concluded that n for sintered Si3N4 is different because of
the applied stress state. Although the mechanism is not clear. the
applied stress state seems to have big effect upon the crack growth
behavior, and the compressive stress under cyclic loading seems to playa
certain role in the behavior; the crack growth data [17] of compact tension
sintered Si3N4 specimens show that the crack velocity under reversed stress
is higher than that under repeated unidirectional stress at the same
maximum stress intensity factor.
From Table 1. the value of n for the present material can be concluded
to be larger than that for the previous material. It is considered [18]
that in the same applied stress state the value of n is different because
of the material microstructure such as grain size, grain morphology and the
character of grain boundary.

522
 TABLE 1. n for sintered Si3N4 at room temperature.

n Experimental method Material Reference

50 cyclic fatigue(reversed) present material
179 static fatigue present material
30 cyclic fatigue(reversed) previous material 1
75 static fatigue,four-point bending previous material 9
58 D.T. previous material 5
41 Cyclic fatigue, tension-compression material A *
76 dynamic fatigue, three-point bending material A 11

23-28 C.T. cyclic fatigue(unidirectional) material B 15

56-65 C.T. static fatigue material B 15
30 C.T. cyclic fatigue(reversed) material C 17
25-37 C.T. cyclic fatigue(unidirectional) material C 17
147-171 C.T. static fatigue material C 17
19 C.M. cyclic fatigue(unidirectional) material D 16
112 C.M. static fatigue material D 16

* Based on the data in [10].

Material B is similar to the previous material.

TABLE 2. Assumed fatigue limit and static strength.

Test conditions Ratios

Rotary Bending Static Fatigue Static Test R.B/S.F R.B/S.T S.F/S.T
MPa MPa MPa
d=8 380 540 627 <623> 0.70 0.61 0.86
(0.88) (0.89) (0.92)<0.94>
d=6 430 610 682 <663> 0.71 0.63 0.89
( ): 0"8 / 0"6 • the ratio of strength for 8 rom diameter to that for 6 rom.
< >: based on the stresses at N=1 in Fig.3.

523
Size Effect on Fatigue Strength
The test results obtained are summarized in Table 2. It seems that
the increase of assumed fatigue limits with the decrease of specimen size
is almost the same for the two, and that the ratio of the fatigue limit
under rotary bending to the static fatigue limit is the same for each
diameter. The weakest link hypothesis predicts that large specimens should
have lower failure stresses than small specimens, and the mean failure
stresses, a 1 and a 2, are related to effective volumes VE, 1 and VE, 2 as
the following formula [19] :
al / a2 (VE,2 / VE,1 )1/m
= (3)
where m is the Weibull modulus. The applicability of this equation to
fatigue strength was examined.
To know the value of m for the present material, a static test was
carried out at a crosshead speed of 0.5 rom/min using four-point bending
apparatus with an inner span 10 rom and an outer span 30 rom. The test
specimens used were rectangular rods with 3 rom thick and 4 rom wide, cutting
the bar specimens made for the present study; they were ground perpendicu-
larly to the longitudinal axis according to bar specimens. The distribution
of static strengths for 40 specimens is shown in Fig.5. The value of m
obtained by the least squares method was 11.9, and the mean static strength
was 674 MPa. The effective volumes VE,R.B under rotary bending and VE,S.F

99.9
{;'
d
99
95
90
~
- o§

f
-
Q. 50
,-
I)/J
1:&
~
~
~ ~

20 ~

/p

/0
0
10 / 0

5 ~

3 ~ /0
2

0
-
I I I I I I

500 600 700 800 850

Static Strength MPa

Figure 5. Distribution of static strengths for rectangular

specimens under four-point bending.

524
under static fatigue are obtained as follows:

VE,R.B = 2V / (m +2) (4)

VE,S.F = (2V/.,r;) S ~/2sinm ecos 2 ed e (5)

where V is the volrnne of the straight middle part of the specimen in which
the fracture occurred; the effective volrnne under a static test is expressed
by Eq.(5). The effective volrnne of a rectangular specimen under four-point
bending is obtained:

VE,4P = V / 2(m +2) (6)

where V is the volrnne of the specimen in the inner span of bending apparatus.
By comparison of the static strength for 8 rom diameter with that for
rectangular specimens, the ratio, a 8, S. T / a 4P' was 627 MPa/674 MPa=O. 93.
which was about equal to 0.92 predicted from Eq.(3). taking m=11.9 and
applying Eqs. (5) and (6). The ratios. a8.S.T / a6,S.T and a6.S.T / a 4P'
were 627 MPa/682 MPa=0.92 and 682 MPa/674 MPa=1.01. and did not agree well
with predicted values. Taking the static strengths as the stresses at N=1
in Fig.3, the ratios, a8.S.T / a6,S.T and a6,S.T / a 4P' were
623 MPa/663 MPa= 0.94 and 663 MPa/674 MPa=0.98, which were about equal to
0.95 and 0.97 predicted from Eq.(3), respectively. Then the increase of
the static strength with the decrease of specimen size could be explained
by Eq. (3).
By comparison of the rotary bending and static fatigue strengths for
8 rom diameter with those for 6 rom diameter, the ratios. a 8. R. B / a 6. R. B
and a 8, S. F / a 6. S. F ' were 380 MPa/430 MPa=O. 88 and 540 MPa/610 MPa=O. 89,
and were almost the same. Eq. (3) shows a8,R.B / a6.R.B = a8.S.F / a6.S.F
=0.95 on the assrnnption that the value of m is constant regardless of the
loading condition. It is considered that rotary bending strength and static
fatigue strength show the similar relationships between the strengths and
the sizes.
The size effect on the fatigue strength. as well as the static strength.
could be estimated roughly using Eq.(3). and the fatigue strength seemed to
be influenced more significantly than the static strength. Estimating the
value of m lower. 5. the ratios predicted from Eq.(3) agree with fatigue
data obtained. However, the estimated value of m is much lower than the
measured value, 11.9, even considering experimental errors. There may be
the possibility of the change in the value of m depending on the loading
condition. The measured value of m was obtained from the distribution of
static strengths. In this case the specimen was subjected to the stress
slightly lower than the critical stress for catastrophic failure of the
material. On the other hand, assrnned fatigue limits were obtained under
the stress much less than the critical stress. The distribution of fatigue
strengths may be different from that of static strengths. The accrnnulation
of fatigue data on size effect is needed hereafter for further explanation.
By comparison of the rotary bending strength with the static fatigue
strength. the ratio. aR.B / as.F ' was about 0.7 for each diameter.
Taking into account of the size effect, and taking m=11.9, the ratio
predicted from Eq.(3) was 0.83. As the predicted value is larger than
the experimental value, the fatigue limit under rotary bending is lower
than that under static fatigue, even taking into account of the size effect.

525
The similar tendency is seen in the data [20] reported on sintered Si3N4
under rotary bending and static fatigue.
Fracture Features of Fractured Surface
"The appearance of the fractured specimen after rotary bending test is
shown in Fig.5. In most cases, the fractured surface was not perpendicular
to the specimen axis. The inclined failure seemed to occur due to crack
branching; the typical example is shown in Fig.7. The previous sintered
Si3N4, whose fatigue strength was about half that of the present material,
had the fractured surface which was perpendicular to the specimen axis [9];
the fractured shape was similar to an upside down "T". The fractured shape
seems to be different because of the strength of the material relative to
its branching tendency.

Figure 5. Fractured specimen after rotary bending test

(a= 451 MPa, N= 1.54x10 5 ).

Figure 7. Fractured specimen after static bending test

( a = 588 MPa ).

Macroscopic observations showed that each fractured surface after both

fatigue tests and the static test had a flat region and a rough region; the
flat region was referred to as mirror-like region [1,9]. The macrophoto-
graph indicating the feature is shown in F~g.8. Mirror-like region is
located in the highest part of the figure. The overall fractured surface
after rotary bending test was relatively smooth compared with that after
static fatigue test. However, it seemed that this difference was simply
due to the magnitude of applied stress, since the fractured surface seemed
to be rougher as the fracture stress was high; the rotary bending fractured
surface of the present material was much rougher than that of the previous
material.

526
 Typical microphotographs of the fractured surface after rotary bending
test are shown in Figs.9a and b. Fig.9a shows the microphotograph in
mirror-like region and Fig,9b shows the area surrounding the region. The
fracture occurred mainly as an intergranular process and the fracture
features were not so different in the two regions. Moreover, no distinct
boundary line separating both regions was recognized under microscopic
observation. The macroscopically apparent difference between the mirror-
like region and the rough region seems to be simply due to the irregulari-
ties in the fractured surface. Microscopic observations on the fractured
surface after rotary bending test were similar to those after static fatigue
test and to those after static test. No characteristic indication of cyclic
fatigue fracture could be found.

Figure 8. Overall fractured surfaces after rotary bending test

(0= 412 MPa, N= 2.94x10 6 ),

In some cases, the mirror-like region had the fracture orlglns such as
a void, a porous region and an inclusion(Fe, Cr), The fracture origin could
not be detected, in other cases. An example of fracture origins is shown
in Fig.10. If the fracture initiation took place near the specimen surface,
the mirror-like region was roughly semicircular and fracture propagated
radially from this area, as shown in Fig.11. In the case where the mirror-
like region existed in the inside of the specimen, the fracture origin was
near the center of the mirror-like region, as shown in Fig.12. The inside
fracture origins would need to take the effective volume as fracture cont-
rolling factor in the weakest link hypothesis rather than the effective
surface.

527
Figure 9. Typical microphotographs of fractured surface after rotary
bending test (a = 431 MFa. N= 6.96 X105 ). (a) of mirror-like
region. (b) of the area surrounding mirror-like region.

528
Character of Mirror-like Region
If the fracture initiation part takes place near the specimen surface,
the mirror-like region is roughly semicircular. This kind of mirror-like
region was examined for specimens with 8 mm diameter; mirror-like region in
the inside of the specimen was left out of consideration. The size of
mirror-like region made under various applied stresses of rotary bending,
static fatigue and further static test was examined by the optical micros-
cope; the mirror-like region was detected more clearly by the optical
microscope than by SEM [1]. The relation between the depth of mirror-like
region d and the applied stress a is shown in Fig .13. The straight line
in the figure was obtained by the least squares method, considering three
kinds of data as the same thing. As seen in the figure. the relation can
be represented by the same straight line regardless of the loading condition.
and can be expressed by the formula:
ads = const. (7)

Figure 10. Void as fracture origin.

The exponent s was 0.59, and the value was about the same as the literature
value [4] which was obtained from the relation between mirror radius and
the applied stress under static test.
The stress intensity factor KI at the deepest point in the mirror-like
region was calculated, assuming mirror-like region as the semicircular
surface crack. In the calculation. the expression [21] reported on a
surface crack in a shaft was used. The formula is as follows:
K
I
= F a .f7ib (8)

where a is the bending stress. b is the crack depth, and F is the dimen-
sionless quantity dependent on the shape of the crack and the ratio of the
crack depth to the specimen size. The relation between the depth of mirror-
like region d and stress intensity factor KI is shown in Fig.14. KI
obtained under each loading condition is almost constant. independent of

529
 Figure 11. Typical mirror-like region of fractured surface
(a= 412 MPa. N= 2.94Xl0 6 ).

Figure 12. Mirror-like region in the inside of fractured surface

(a= 421 MPa. N= l.02xl07 ).

530
 800

r:. 700
~
~
O~
o 0

o 600 D6~~D 6 6 l>IS>

ll>
6~
500 "'-
f--
o Rotary Bending
0a§'o 0
0,
l:> Static Fat igue 0, 0
0 0 ...
400 t - - Static
,
0
I'
380
100 150 200 250 300 350 400 450
d J.lm

Figure 13. Relation between depth of mirror-like region

and applied stress.

12
I- 0 Rotary Bending

-
N
'M
E 11 I:> Static Fatigue -
z I- 00 0 Static
~ 0 0 ~
10

f
l- 10 l!1> I:>
~
I:> ~ I:> l!J I:>
00 0
l- 0
[ll.1:> 6 00
0
9
ugg 0 1--0
I- 0
8 I-

100 150 200 250 300 350 400 450

d )..1m

Figure 14. Relation between depth of mirror-like region

and stress intensity factor.

531
the depth of mirror-like region. The mean and standard deviation are shown
in the right side of the figure. The mean value was KI = 9.5 MN/ m3/ 2 .
It was considered that the failure occurred when the size of mirror-like
region reached a critical value dependent on the applied stress regardless
of the loading condition. The critical value seemed to be related to
fracture toughness KIC of the material. but the value obtained was higher
than KIC; KIC of the present material was 6.7 MN/ m3/ 2 which was measured
by the Vickers indentation method [22]. The discrepancy between the value
of KIC and that calculated by using the size of mirror-like region seems to
suggest that KIC depends on the crack size and/or crack shape. on the
assumption that the Vickers indentation method does not give lower value
for KIC compared with the true value.
The life of ceramics seems to be controlled by the subcritical crack
growth from the initial flaw. The subcritical crack growth behavior seems
to be different because of the applied stress state. as already discussed.
The size of mirror-like region was correlated with the applied stress
regardless of the loading condition. and the failure occurred when its size
reached a critical value dependent on the applied stress. It is considered
that the difference of the fatigue behavior under rotary bending and static
fatigue can be related to the difference of the subcritical crack growth
behavior in the mirror-like region. The KI-V diagrams assumed in mirror-
like regions seem to be similar to those [15.17] measured on compact tension
sintered Si3N4 specimens under reversed stress and constant stress.

CONCLUSIONS
The fatigue behavior of sintered Si3N4 under rotary bending and static
fatigue was studied. The results obtained are summarized as follows:
1. The life of the material increased as the stress amplitude or the
applied stress decreased. The S-N curve and the S-t curve could be repre-
sented by the straight line up to about 108 stress-cycles and 106 ceconds.
and could be expressed by the formulas. an N = constant and an t =
constant. respectively. The exponent n under rotary bending was much
smaller than that under static fatigue.
2. The knees seemed to exist at cyclic numbers more than 108 and at
the time more than 10 6 seconds. respectively. The assumed fatigue limit
under rotary bending was lower than that under static fatigue.
3. Both assumed fatigue limits showed the similar relationships between
the strengths and specimen sizes. The size effect could be estimated
roughly by the weakest link hypothesis. and the size effect on the fatigue
strength seemed to be stronger than that on the static strength.
4. The fracture features of fractured surfaces after both fatigue
tests could not be distinguished. and the features were similar to those
after the static test.
5. The size of mirror-like region was correlated with the magnitude
of applied stress regardless of the loading condition. and stress intensity
factor at the deepest point in the region was almost constant.
6. It was considered that the difference of fatigue behavior under
rotary bending and static fatigue was due to the subcritical crack growth
behavior in the mirror-like region.

532
ACKNOWLEDGEMENT
Sincere thanks should be presented to Dr. O. Kamigaito of Toyota Central
Research and Development Laboratories for valuable advice and suggestions.
Thanks should be also presented to Kyocera Kagoshima Factory for their
support.

REFERENCES
1. H. N. Ko, J. Ceram. Soc. Japan, 94, 534 (1986); ibid., 95, 472 (1987).
2. H. N. Ko, J. Mat. Sci. Lett., 6, 175 (1987).
3. H. N. Ko, Proc. of the MRS International Meeting on Advanced Materials,
5, Materials Research Society, Pittsburgh (1989)P.43.
4. H. P. Kirchner and R. M. Gruver, Fracture Mechanics of Ceramics, 1,
Plenum Press, New York (1974)P.309.
5. Kyocera, Private communication.
6. M. Masuda, N. Yamada, T. Soma. M. Matsui and I. Oda. J. Ceram. Soc.
Japan, 97. 520 (1989).
7. H. N. Ko, J. Mat. Sci. Lett., 5. 464 (1986); ibid .. 6. 801 (1987).
8. H. N. Ko. J. Mat. Sci. Lett., 8, 1438 (1989).
9. H. N. Ko. J. Ceram. Soc. Japan, 97. 599 (1989).
10. M. Masuda. T. Soma, M. Matsui and I. Oda. J. Ceram. Soc. Japan. 96.
277 (1988).
11. Y. Yamauchi, S. Sakai, M. Ito. T. Ohji, W. Kanematsu and S. Ito.
J. Ceram. Soc. Japan, 96. 885 (1988).
12. T. Kawakubo and K. Amano, Proc. of the 32th Japan National Symposium
on Strength, Fracture and Fatigue, Anzen-Kyodo-Kenkyu-Kyokai. Sendai
(987)P .1.
13. Y. Yamauchi, S. Sakai. M. Ito, T. Ohji, W. Kanematsu and S. Ito,
J. Ceram. Soc. Japan. 94. 631 (1986).
14. T. Kawakubo and A. Goto. J. Soc. Mat. Sci. Japan, 37, 939 (1988).
15. H. Kishimoto. A. Deno. H. Kawamoto. J. Soc. Mat. Sci. Japan. 36.
1122 (1987).
16. H. Sugawara. A. Otsuka and T. Amano. Paper presented at the 20th
Symposium on Fatigue, J. Soc. Mat. Sci. Japan (1990)P.158.
17. H. Kishimoto, A. Deno, H. Kawamoto and Y. Fujii. J. Soc. Mat. Sci.
Japan, 38. 1212 (1989).
18. H. N. Ko. J. Mat. Sci. Lett., 10. 545 (1991).
19. D. G. S. Davies, Proc. Brit. Ceram. Soc., 22, 429 (1973).
20. K. Saruki. K. Ogawa and T. Asano. Trans. Japan Soc. Mech. Engrs ..
54-A, 2082 (1988).
21. Y. Murakami and H. Tsuru, Stress Intensity Factors Handbook.
Pergamon Press, Tokyo (1987)P.657.
22. K. Niihara. R. Morena and D. P. H. Hasselman. J. Mat. Sci. Lett .. 1.
13 (986).

533
AN APPROACH ON LIFETIME PREDICfION FOR CERAMICS UNDER

ELEVATED TEMPERATURE WITH STATIC FATIGUE *

L.X. Zeng, Z.D. Guan, and X.F.Zhao

Department of Materials Science and Engineering
Tsinghua University, Beijing 100084, P. R. China

ABSTRACf

Stress-Time-Probability (STP) diagrams for sintered Si 3N.. at 1200t were

studied with static fatigue experiment in three-point bending specimen. Microcracks
were introduced before the tests by Knoop indentation at the center of the specimen
tension side in order to reduce the scatter in fatigue data.

Three-point bending tests and static fatigue experiments were performed on

sintered Si 3N.. specimens to give Weibull's parameters and SCG exponent seperately.
It can be deduced from the curve of Pc verse (uc-u u), in which u u is threshold value of
Weibull distribution, that the average strength meets the following equation:

By using different Uu to carry on linear regression of Inln[1 / (I-Pc)] verses

1n(uf-uu)' we can get different values of ilf. Comparing them with the measured value
enable us to make out Uu value.
STP diagrams were established for sintered Si 3N.. ceramics at 1200t at different
fracture probabilities.

INTRODUCfION
Studies on lifetime prediction for ceramic materials began in the recent twenty
years. The brittleness and time-dependence of strength especially at high temperatures
of these materials - - the former results from the variation of pre-existing flaw size,
as well as the variation of fracture locations (J) ; while the latter is caused by slow
crack growth (SCG) of pre-existing flaws - - make it difficult to accomplish lifetime
prediction, which is indepensable in practice.

Usually, in engineering design, when security of material needs to be considered,

proof test has been employed, after this experiment, the maximum initial size of the
survival samples is considered to be smaller than a certain limit, hence the possible
least lifetime is determined. But that is far from enough. In recent years, many
researchers turned their attentions to the study of STP diagram (2,3.") .
* This paper is done under the cooperative research contract with Hitachi Chemical
Co., Ltd.
FrQl:/ure Mechanics of Ceramics, Vol. 9
Edited by R.C. Bradt e/ al.• Plenum Press, New York, 1992 535
 More information of great avail in engineering design and lifetime prediction can
be shown clearly on STP diagram. It can be used to determine the maximum possible
applying stress when the fracture probability and the demanded lifetime are given; and
to estimate for how long a structure can serve safely under a certain applying stress
and fracture probability.

Silicon Nitride ceramics, with its high hardness, high strength, better resistance to
corrosion, oxidation and thermal shock, as well as its excellent high temperature
mechanical properties, is becoming one of the most promising condidate for heat
engines, cutting tools and other high temperature applications. To keep pace with the
present development on this material, we established its STP diagram by means of
static fatigue method.
STRESS-TIME PROBABILITY RELATIONSHIP
Weibull Distribution Function
In brittle materials, fracture is usually caused by the propagation of a weakest
crack, therefore, strength data distribution of a sample depends on the distribution of
weakest cracks existing in the sample. In 1951(: W.Weibull derived that fracture
strength distribution could be expressed as follow S):

(I)

where Pc refers to the fracture probability of a sample; V is effective volume; tTc is

fracture stess; tT u is called threshold stress; V o is a unit volume; tTo refers to
normalized strength. By the introduction of the characteristic modulus of rupture (6) :

Equation (1) can be simplified to give:

P f = 1-exp [ - (~~:: fJ (2)

where m is refered to as Weibull's modulus, it is a yardstick for strength uniformity of

materials. Big value of m means more concentration of strength data.
Stress-Time Relationship
Slow crack growth (SCG) in ceramics is a predominant reason for time-
dependent gegradation of strength. SCG rate varies with K I value on the crack tip as
shown in Figure 1 (7) • In region I, cracks remain arrested, while in regions ill and IV ,
cracks grow rapidly to reach critical dimension, soon catastrophic fracture follows.
Hence, SCG can simply be described by the steady propagation stage, i.e. region n. In
this region, v and K I are related by the empirical formula (B) :
N
v=AK I (3)

where N is refered to as SCG exponent. Replaceing K I by tTY.r;; to give lifetime

under static loading condition:
N
t fs = B/ tT c• (4)
where B is a constant, tTcs is static loading stress.

536
 K1
Fig.I. A typical Kl-v Curve for Ceramic Materials

Stress-Time-Probability Relationship
Assuming failure stresses under both static loading and dynamic loading
conditions equal to each other, i.e., O'C'=O'Cd' Knowing that failure time under static
loading tCI and that under dynamic loading tCd meet Eq.(S) (2) :

(5)

From Eq.(4), we get:

(6)

Taking into consideration that O'cs=o"t N and that O'CI=O'fd=O'N' the following is
facile to work out:

)N
1
0' Cd
(7)
O'N = ( (N + l)o"t O'Cd
N
Combining formula (7) with (2) we derived:
Aim
MORoe + 0' )
NInO' N + In tN = (N + 1)ln ( C u (8)

l
where A=lnln _ p ,C=[(N+])q]I/(N+l), q is loading rate while performing
l eN
strength experiment. Upon determination of parameter m, MOR o, O'u' and N by
experiments, STP diagram can be set up.

DETERMINAnON OF WEIBULL'S PARAMETER AND SCG EXPONENT

Calculate Weibull's Parameter by Strength Experiment

By taking logrithum on both side of formula (2), rearranging it, we derived:
I
Inln] _ P = mln(O' C - 0' u) - mlnMOR o (9)

537
 When a group of strength data is obtained by experiment, which is 0'\ ; 0'2 ; •••
;0'1 ; ••• ; 0'11 in increasing order, the failure probability of this sample corresponding
to a stress of 0'1 is given by the evalutor (9) :

P. = i -0.5 (10)
I n

Assuming
1
~ P ,X = In(O'( - 0' J, equation (9) shows a linear
Y = lnln
association between Y and X, thus m and MORo values could be carried out by linear
regression (S) •
Determination of O'u
For Weibull's distributio~, there exists lohe following relation (\0) :

(II)

Giving several O'u values, using equation (9), carrying on linear regression results
a set of different values of m and MORo' Substitute each set of data into equation (I 1)
to give corresponding average strength qf. Compare them with the measured average
strength, to make a decision on which set of data is the exact one we were seeking for.

Carrying out of SCG Exponent with Static Fatigue Method

Usually, we have direct and indirect methods for carrying out of SCG exponent.
The more popular one is indirect method which includes static fatigue and dynamic
fatigue methods. Here, we use static fatigue method.
In static fatigue experiment, there exists:

t( = BO' -N (I 2)

N can be obtained by the linear regression of InO' and the corresponding failure
time Inte•

EXPERIMENT
A sintered silicon nitride ceramics was used. It is composed of 81.6wt% Si}N4 ,
13.9wt% Y 203 and 4.5wt% A1 20 3. Specimens were rectangular bars with dimensIons
3mm high, 4mm wide and more than 36mm long. The tensile surface were polished
with diamond paste (grit size 0.5jlm). After polishing, the specimens were chamfered
along the edges. Artificial cracks were made by Knoop indenter with load of 3200g
hold for 30 seconds. Three-point bending strength tests were performed with a span of
30 mm, and a loading rate of 4.97MPa / s.
Static fatigue tests were performed on high temperature creep machine. Before
subject to a stress, specimen stayed in the furance for 10 minutes to ensure its internal
temperature meeting the required condition.

RESULTS AND DISCUSSIONS

Experimental Results
Static fatigue tests were performed with different level of load stress. Table I
shows the results.
Taking logrithum of both sides of equation (12), we obtained:

538
 104

103 0
0 0

--...,.... 10
til
2

.
00

10 1

100
260 280 300 .320
(la (MPa)
Fig.2. Results of Stress Rupture Testing

Table 1. Static Fatigue Results of SSN at 1200t

Specimen Specimen Applied Time to

M Width Thickness Stress Failure 19(1 19 tr
B(mm) H(mm) (I. (MPa) t r (s)
1 3.74 3.06 300 339 2.477 2.530
2 3.92 3.08 295 247 2.470 2.393
3 3.78 3.06 290 119 2.462 2.076
4 3.84 3.08 290 113 2.462 2.053
5 3.82 3.00 295 227 2.470 2.356
6 3.82 3.06 275 1175 2.439 3.070
7 3.80 3.08 275 516 2.439 2.713
8 3.84 3.10 270 755 2.431 2.878
9 3.82 3.06 270 519 2.431 2.715
10 3.76 3.04 285 262 2.455 2.418
11 3.82 3.08 310 6 2.491 0.778
12 3.80 3.08 305 21 2.484 1.322
13 3.84 3.08 303 21 2.481 1.322
14 3.76 3.06 300 441 2.477 2.644
15 3.84 3.02 303 5 2.481 0.699
16 3.82 3.08 305 70 2.484 1.845
17 4.02 3.04 285 660 2.455 2.820
18 3.82 3.08 280 800 2.447 2.903
19 3.82 3.02 304 20 2.483 1.301
20 3.78 3.00 276 5440 2.441 3.736
21 3.84 3.08 303 30 2.481 1.477
22 3.82 3.04 303 63 2.481 1.799
23 3.84 3.08 290 174 2.462 2.241
24 3.82 3.08 300 13 2.477 1.114

,
Int r = - Nln(l + B (13)

which demonstrates a linear association between lOCI and lntr shown schematically in
Figure 2, gives N = 33.16, B = 8.13 X 1083 • Thus far, the value ofN is determined.
A number of specimen were subjected to a fixed loading rate of 4.97MPa / s at
1200t to obtain Weibull's parameters. Experimental results are listed in Table II
(shown in Figure 3). By carrying on linear regression analysis and using equation (13),
we obtained Weibull's parameters at 1200t is m= 16.27, (lu=~OMPa. and
MOR o=356.1MPa.

539
 2.0

..··
~
1.0 f- m= 16.27
uu =40MPa
MOR o= 356.1MPa
..',
I

0.0 f-
.'
··.I'
.....
-,
--l lo

.......
......
-1.0

..·
.....l:l: -2.0
.....
-3.0

-4.0
300 340 380 420
UJUu (MPa)

Fig. 3. Weibull Plot for SSN at 1200t

300 po..~f"'o<;;::--+--+-....---H

250 r---:--~~

'0" 200 1;----+--1-

150 '--_.........._-'--...L.-..l-.---'_-.l.........1
J min 1 hr 1 dayl mon 1 year
Duration tN

FigA. STP Diagram for SSN at 1200t

Tablell. Experimental Results ofWeibull's Parameters

No. of Specimens ar (MPa) <Tc (MPa) an_I(MPa) an-I/ <Tc (%)

40 378.7-418.0 385.21 ±22.7 ± 5.89

Establishment of STP Diagram

Equation (8) shows that, knowing the values of au' m, N, and MOR o, STP
diagram can easily be worked out as shown in Figure 4. For this kind of ceramics at
1200t,

Int H + 33.161na H = 183.8 (P=0.001)

540
 Int N + 33.161DO' N = 187.9 (P = 0.01)

In general.1 A discount factor (or loading factor) L is used to modify the loading
mode effect (IIJ :

For uniaxial tension: L= 1

1
For 3 - point bending: L=
2(M + 1)2
2+m
For 4 - point bending: L=
4(M + 1)2
1
For pure bending: L=2(M + 1)

Using subscribes N and A represent experiment condition and applying condition

respectively, and taking the dimension effect and the loading mode effect into
consideration, leads to the following relation:

q
~ __ (L V)~
&_&-
(I4)
qA - L N VN

Now, it is obvious that the normalized stress actually refers to a stress under the
experiment condition.

Until now, the establishment ofSTP diagram and its application is completed.

CONCLUSIONS
Three-point bending tests and static fatigue experimnets were performed on SSN
sample to give Weibull's parameters and exponent seperately. It can be deduced from
the curve of P r verses qr that the average strength meets equation (11). By using
different qu to carry on linear regression, we can get different values of <1(. Comparing
them with the measured value enable us to make out qu value.

STP diagrams were established for a kind of SSN ceramics at 1200t.

REFERENCES

(D Y.Matsuo and K.Kitakami, in "Fracture Mechanics of Ceramics", Vo1.7.

R.C.Bradt, A.G.Evans, D.P.H.Hasselman, and F.F.Lange, ed., Plenum Press,
New York, 1986
(2) R.W.Davidge, J.R.Mclaren, and G.Tappin, J. Mater. ScL, 8 (1973) 1699
(3) K.K.Smyth and M.B.Magida, J. Am. Ceram. Soc., 66 (1983) 500
(4) B.Gurumoorthy, K.Kromp, F.B.Prinz, and A.G.Bornhauser, J. Mater. ScL, 22
(1987) 2051
(5) W.Weibull, J. Appl. Mech., 18 (1951) 293
(6) D.F.Dailly, et. aI., in "Special Ceramics", Vol.7, ed. by T.Taylor (1981) 191
(7) A.G.Evans, J. Mater. ScL, 7 (1972) 1137
(8) B.Bergman, J. Mater. Sci. Lett., 5 (1986) 611
(9) J.D.Sullivan and P.H.Lauzon, J. Mater. ScL Lett., 5 (1986) 1245
(to) Ayal de S.Tayatilaka, et.al., in "Fracture of Engineering Brittle Materials"
(t 1) F.F.Lange, unpublished. 1985

541
LIFETIME OF HIPed SILICON NITRIDES AT ELEVATED TEMPERATURES

Isao Tanaka, Giuseppe Pezzotti, and Koichi Niihara

The Institute of Scientific and Industrial Research

Osaka University, Ibaraki, Osaka 567 JAPAN

ABSTRACT

Lifetime of brittle ceramic materials at elevated temperatures are

determined by their resistance to time dependent failure processes. In
this paper, special attention is paid to describe slow (subcritical) crack
growth (SCG) behavior, and a method to evaluate the SCG resistance of
materials is proposed. HIPed high-purity Si 3N4 sintered without additives
and pressureless sintered SiC with Band C additions were found suitable
for the examination of SCG behavior at 1400·C because of their low creep
ductility. Based on the experimental data, lifetime of the "as machined"
Si 3N4 specimen was estimated to be about 400 h under 300 MPa of static
load at 1400· C: It showed fairly good agreement with the real-time static
loading data. The SCG resistance in the HIPed Si 3N4 was found much better
than in the SiC. In stoichiometric high-purity beta-sialon series, creep
ductility increased with solute concentration (z-value) and transi tion
from elastic SCG regime to more creep ductile failure was found.

1. INTRODUCTION

Brittle ceramic materials suffer considerable time-dependent strength

degradation especially at high temperatures, and understandings of time-
dependent mechanical properties are strongly required I.hen structural
components are expected t.o be loaded for long-term operative cycles. It
is, therefore, inappropriate and dangerous to design such components only
using data obtained from short-term tests, for example by standard bending
strength measurement. Procedure taking into account t.he long-term
processes is, however, not established, and even their phenomenology have
not been sufficiently clarified yet. Unless the phenomena as well as their
elementary processes are revealed, we could not safely apply such
materials for real high temperature components.
Si 3 N4 is a prime calldidate for high t.emperature structural
application, and understanding of the time-dependent. mechanical properties
at high temperatures is strongly required. Many works have treated the
phenomenology of the time-dependent failure processes[1-5]. However, the
Si 3N4 materials examined in these studies were fabricated with 5 to 20

FrQl:ture Mechanics of Ceramics, Vol. 9

Edited by R.C. Bradt et al., Plenum Press. New York:, 1992 543
vol% of various kinds of oxide additives, and the time-dependent processes
have been found greatly influenced by the type and the amount of
additives. Moreover, there has been no standard tests for the evaluation
of such behaviors. As a consequence, what and how material parameters
affect the time-dependent properties are still not clear.
By using glass-encapsulation technique of hot isostatic pressing
(HIP), high-purity Si 3N4 powders can be fully densified without additives.
Our previous studiesL6,7] found that the intergranular phase of the
material started from high-purity powder and sintered without addi ti ves
consists only of high-purity glassy silica. They localize as small glass-
pools at the triple points and thin-film of about 1 nm between grains.
These systems with "simple grain boundary" can be cons idered as a
reference material of Si 3N4 sintered bodies.
In this paper, the slow (subcritical) crack growth (SCG) resistance of
this high-purity Si 3N4 has been examined based on a method proposed in the
present study. The time-dependent failure processes at high temperatures
are classified and the methodology for the evaluation of SCG is described
before the experimental results. HIPed Si 3 N4 without additives and
pressureless sintered SiC are found appropriate to apply the present SCG
test up to 1400'C because of their low creep ductility. Increase of creep
ductility with solute concentration was found in high-purity beta-sialons,
and the transition from elastic SCG regime to more creep ductile failure
has been pointed out.

2. TIME DEPENDENT FAILURE AT HIGH TEMPERATURES

2.1 Classification of the degradation processes

Time-dependent failure of cerami cs under loadi ng at elevated

temperatures can be classified at least into two categories depending upon
the creep ductility of the material. They are SCG and creep failure. When
creep deformation rate is negligibly small and time-dependent phenomena
are only originated at the tip of pre-existing flaw, SCG from single flaw
determines the failure time or stress. Thus the lifetime or strength is
strongly dependent on the size of the initial flaw. When the plasticity
even at the crack tip is negligible, SCG behavior can be described in
terms of elastic stress intensity factor, KI and the SCG rate may have the
power-law relationship analogous to the stress corrosion cracking behavior
of glasses as follows[I]:

da/dt = A KI n (1)
where A and n are constants. When local creep deformation at the crack tip
gives rise to crack blunting, elastic stress intensity becomes
inappropriate to describe the crack growth bihavior. It may be well
describe9[8] in terms of the creep J-integral, J (the modified J-integral
or the C parameter), as

(2)

With the increase of creep rate of the material, the pre-existing

flaws tend to be blunted and the fail ure becomes controlled by creep
damage accumulation processes. In this regime, failure occurs after large
creep deformation and the lifetime of the material shows little dependence
on the initial flaw size. Between the SCG regime and the creep failure
regime, Wilkinson et 11.1[9] have recently proposed further classification
into "microcrack" regime based on their experiments in alumina. In this

544
regime several microcracks are formed perpendicular to the stressing
direction in flexure bars and they grow until one of them becomes a
critical size. Such microcracks are formed as a result of local creep
damage accumulation and they are not necessarily originated from the pre-
existing flaws. Dalgleish et a1[10] have foulld this behavior earlier in
alumina and called it, the damage by formation of "shear band". Zeng et
a1[l1] also recently found such damage profile in HIPed Si 3 N4 -10wt%Si0 2
specimen.

2.2 Description of SCG behavior and lifetime

In elastic SCG regime, integration of eq(l) until the failure gives

the time to failur'e as

(3)

in which <0"1) shows the average of an that is

tf
<0"1) = l/ t f I" a(t,)n dt' (4)
-0
Here, a geometric factor for the crack is assumed to be invariable
throughout the test. When n-value is larger than 10 as often observed for
SCG behavior of engineering ceramics at high temperatures,
(2-n)/2 (2-n)/2
aO » af (5 )

Therefore, eq (3) becomes

t
f
= 2/(n-2) A-I y-n aO(2-n)/2 / < an) (6 )

In this regime, lifetime prediction can be made by simple

extrapolation of experimental data. Lifetime t x under static loading of ~
for a specimen whose illitial flaw size is ax is given by eq(6) as

= (7 )

where aO' to and < a n)O aee the experimental data.

Before applying the above equations, the following points should be
experimentally checked. (l)The amount of creep deformation prior to
failure should be negligible small. (2)No creep damage can be observed in
fractographs or on the tensile surfaces by microscopy: Failure should
originate from a single flaw. (3)Flaw size sensitivity of failure stress
indicate the elastic SCG: In constant-strain rate t.est with st.ressing rate
of & , eq(6) can be modified to give the flaw-size sensit.ivity of fracture
stress af as follows,

a nt1 = 2 a(ntl)/(n-2) A-- l y-n aO(2-n)/2 (8)

f

Figure 1 shows the hypothetical flaw size sensitivity of failure stress by

const.ant st.rain rate test. The dependence of failure stress becomes
smaller with the increase of creep ductility because of crack blunting,
which may give rise to the increase of Weibull modulus. But, the crack-
blunting process is often accompanied by the time-dependent damage
process, and it is very dangerous to design the real struct.ural components
to use under such "damaging" condition even if the apparent advantage of
crack blunting can be expected. From the engineering point of view, the
elastic SCG regime of the mat.erials should be clarified, and service

545
 INITIAL FLAW SIZE

Schematic flaw size dependence of failure stress in three re~imes.

temperature and stress should be chosen sufficiently below these levels

especially for component expected to be loaded for long-term. Under these
conditions, creep damage process is negligible, and the material may not
suffer any time-dependent failure processes.

2.3 Effective lifetime under static loading

When one wants to compare the high temperature "time-dependent" data

(strength, lifetime etc.) measured by different loading schedule, concept
of effective lifetime under static loading may be useful. For any loading
schedule, the lifetime under static loading at failure stress, uf of the
same material can be given as
Un (9)
f
The ratio t s to t f is defined as g(n)n in which g(n) is given by

g(n) = < un)/n / uf (10)

and it is only a function of n-value. Analytical forms of g(n) for three

typical loading conditions are shown in Fig. 2.
We define the value t s as effective lifetime under static loading.
Concept of the effective lifetime is schematically shown in Fig. 3. In
elastic SCG regime, when initial flaw size and the effective lifetime is
fixed, the flaw severity for SCG of materials can be compared in terms of
failure stress. This will be described in the-next section.

2.4 SCG resistance

For the evaluation of fast fracture resistance (fracture toughness),

measurement of flexural strength on pre-cracked specimens are generally
recommended because the reliability of the initial flaw size and geometry
makes the testing procedure convenient. Here, a similar procedure is
proposed for the evaluation of the SCG resistance from bending test of
pre-cracked specimens.
Consider a flexure experiment at elevated temperature for a precracked
specimen in which failure takes place by elastic SCG at the stress of uf
after total testing time of t f . A stress intensity can be directly
obtained from experiment using initial flaw size aO'

KI * = y aO
1/2 (11 )

546
 (a) STATIC (b) DYNAMIC

Of (fJ Of ,
(fJ
(fJ (fJ
W W
0::: 0:::
I- I-
(fJ (fJ

If
TIME TIME
(c) 2-RATES

°Fo,
° ..........................
(fJ
(fJ
W
0:::
I-
til

t~ tFI,+12
TIME

Aoalyti cal forms of 9(0) = <0">1/" / Of

STATIC
DYNAMIC
2 RATES

Fig.Z Typical loading conditions: (a) Static-loading, (b) dynamic-

loading, and (c) 2-rates dynamic-loading. Analytical forms of gIn)
(see text) are shown in a table.

547
Only initial flaw size is considered because the initial flaw size is
mainly responsible for the SCG lifetime as shown in eq(6). When a specimen
of this material is statically loaded under uf and the initial stress
intensity is as large as KI *, the static-load lifetime of the specimen
becomes t f g(n)n which is the effective static-load lifetime of this test
given in eq(9). Since this stress intensity is directly obtainable by
experiments, it is very useful to represent the SCG behavior. When tests
are performed by fixing the effective lifetime, direct comparilon between
these materials in terms of KI value becomes possible. The KI parameter
will be hereafter called SCG resistance.
The advantage of material with high SCG resistance can be demonstrated
clearly by the estimated static-load-lifetime. Assuming that the initial
flaw size of two materials are the same, eq(7) shows that a lifetime
increase for one order of m¥ni tude under the same constant stress
requires a 26 % increase in KI when n=10, and 12 % when n=20.

2.5 Stepwise loading test

SCG resistance for a fixed effective static-load lifetime can be

experimentally obtained most easily by stepwise loading tests. The
stepwise loading may be also useful in highly refractory materials in
which the range of external strain rate required for the examination of
time-rlependent failure process is very low and reliable constant strain
rate can be hardly applied. A typical schedule of a stepwise loading is
shown in Fig. 4. In order to save the experimental time, a stepwise load
is started from u 1 at which the SCG rate is considered to be negligible
small ( ufn» ul n). In the elastic SCG regime, a factor g( n) can be
obtained as shown in Fig. 4.
The stepwise loading is a kind of pseudo-static loading, and when n-
value is sufficiently large and stress-step is well chosen, the final step
becomes dominant within the total loading time, and the effective
lifetime becomes asymptotic to the holding time of each step (see Fig. 8).
Therefore, testing by a fixing effective lifetime can be made, which is
the important advantage of this loading method.

3. EXPERIMENTAL PROCEDURES

Materials used in this work are 1) Si 3N4 sintered without additives

and 2) stoichiometric beta-sialons, both fabricated by the present
authors. Both materials were started from high-purity powders and HIP-
sintered up to >99.5% of theoretical densi ty. Sintering temperatures of
sialon materials were chosen so as to get the similar microstructure.
Details of the fabrication processes and properties have been described
elsewhere[6, 12]. For comparison, 3) pressureless sintered a - and J3-SiC
sintered with concurrent addi tion of Band C ( a: Hexolloy SA by
Carborundum and 13: Ibiceram SC850 by Ibiden) were purchased and used.
The specimens were cut into 3 mm x 4 mm x 20 mm bars, and a controlled
surface flaw was introduced into the center of the tensile surface by
Vickers indentation at 49 N . The specimens were then annealed for 1 h at
> 1200·C to release the residual stress introduced by indentation.
Bending tests were performed at around 140~C. For Si 3N4 specimens,
tests were performed in both air and in nitrogen gas atmosphere, and no
notable difference could be found. Stepwise loading was performed in three
point bending geometry with a 15-mm span. The loading rate up to the
initial step was 0.02 mm/min (outer fiber strain rate of 2.7xlO- 5 s- ),
and the stress was then maintained by the load-cycling unit of a testing
machine (Instron Model 1185) with stress scattering of <2 %.

548
 (/J
(/J
w
~
I-
(/J

TIME
Fig.3 Schematic representation of the meaning of "effective static-load
lifetime, t S '

V>
V>
UJ
~
l-
V>

TIME

g(n) = (liN t. oj")1/

n
ION

when n»1
ts-..6.t

Procedure and gIn) for stepwise loading test.

549
4. RESULTS AND DISCUSSION

4.1 High-purity Si aN4 without additives

Time-dependent degradation behavior at around 1400· C of Si 3N1 started

from high-purity powder and sintered without additives is examined.
Comparison will be made with the data obtained in Si 3 N4 -1.0wt%AIN material
and pressureless sintered a and ~-SiC with Band C addition.
By constant strain-rate tests for 49 N-Vickers precracked specimens at
1400· C, clear intergt'anular SCG p[oP~fation can only be found when the
strain rate was lower than 1.5xl0 s . Typical fractographs showing the
intergranular SCG are shown in Fig. 5. No plastic strain was detected in
all three materials prior to failure even when cleat' SCG was found. This
suggests that the time-dependent degradation mechanism of these materials
under these conditions is elastic SCG: The phenomena may be described in
terms of elastic stress intensity factor. Flaw size dependence of the
fracture stress by SCG provides an evidence for this assertion. Figure 6
shows the fract~re stress determined by SCG measured at constant strain
rate of 1.5xl0- s-1 as a function of initial flaw size introduced by
Vickers indentations. Assuming the flaw size dependence in elastic SCG
regime given as eq(8), n is calculated to be 17 from this data, which may
be typical for the elastic SCG.
Further evidence of elastic SCG can be obtained by flexural creep rate
measurements. At 1400·C, stead!, state strain rate under 200-360 MPa was
found to be about 3-10xl0- 9 s- in Si 3N4 without additives[13]. In a-SiC
used in this study, flexural steady _1bate:... {ree p strain rate at 1400· C
under 414 MPa was reported to be 4x10 s [14]. These strain rates are
about 3 to 4 orders of magni tude smaller than the extemal strain rate
necessary to give rise to the intergranular SCG in these materials. Thus
creep relaxaJion process may be neglected under the external strain rate
of about 10- s-l.
The stepwise loading tests for precracked specimens are made from
140 MPa with 10 MPa/600 s at 1200-1400·C. Initial flaw was introduced by
*
Vickers indentation of 49 N. The SCG resistances, KI obtained by this
test are summarized in Fig. 7. The failure stress at 1400·C for Si 3N4 , two
SiC and Si 3 N4 -1.0wt%AIN specimens were 250, 180, and 150 MPa,
respecti vely. As can be seen, the highest SCG resistance was found in
Si 3 N4 without additives. a-SiC and ~-SiC are found no different from the
viewpoint of SCG resistance. The effective lifetime of these results are
shown as a function of n-value in Fig. 8. As already m ntioned in section
3
2.5, the effective lifetime of these data are about 10 s and not so much
dependent on failure stress and n-value: It is asymptotic to 600 s which
is the holding time of each step. Thus the SCG resistances of different
materials in the present tests are comparable.
From the SCG resistance data, lifetime of these materials under static
loading condi tion can be estimated with eq (7). Figure 9 shows the
calculated results assuming the initial flaw size is 40 ~m and n is 20. As
already mentioned, small difference in SCG resistance is significantly
amplified in lifetime: It is about 3 to 4 orders of magnitude longer in
Si 3 N4 without additive$ than in a- and ~-SiC. Addition of lwt% of AIN
shorten lifetime for 5 to 6 orders of magnitude! The validity of the
lifetime prediction can be checked by real time experiments. Figure 10
shows the results for as machined Si 3 N4 and 1.0wt% AIN added specimens
statically loaded in bending geometry. They show good agreement with the
predicted values.

4.2 High-purity beta-sialon series

In HIPed high-purity Si3N4'_6ti~rdependent failure at 1400·C under

external strain rate of about 10 s was found well described by elastic

550
Fig.5 Optical micrographs of fractured surfaces after the stepwise
loading tests (10 MPaj600 s from 140 MPa) for 49 N Vickers-indented
la) high-purity Si 3N4 and (b) ~-SiC specimens.
Tests were performed at 1400·C .

.......
o

! 1400·C
~ 400
<.:>
z
UJ
~
tn 200
~
5i! 100
~
u...
100 200 400
INITIAL FLAW SIZE 0mJ)
Ei,&Ji Flaw size dependence of failure stress in high-purity Si N .
3 4
Tested at 1400·C by 3-point bending of Vickers iniented specimens with
49 N, 98 Nand 196 N-loads. Strain rate was 1.5xl0- s-1

551
 ,-..
~
4
-E

-
SiJN4
•
C
a.. e 0
::;;
3
...,Vl
0 a,p-SiC.··.
II
j!}
2

.
"--
~

':Z 1
1000 1200 1400
TEMPERATURE (oe)
j
~I SCG resistance for the effective lifetime of about 10 s as a
function of temperature. o :Si 3N4 , ... : a-SiC, . : /3-SiC, and
• : Si 3N4-1wt%AlN .

...-.
...!l- 4
w 10 r---r---,-----,---,--.,...---.-----,
~

~
u..

~
:J Si3N4-1wt%.~IN
a,p-SIC
~ I 103
_ Si 3 N4
u
-==,;;;;;;;;;===
~
Ul
W
>
i=
~ 102 '-----''------'-----'_----'-_----'-_-L_-l
l±: 0 20 40 60
w
n
~ Effective static-load lifetime, t s ' for the present stepwise
loading tests as a function of n-value for three materials.

552
 800 Initial Flaw; 4O;un n=20
700
600
"0 500
Fast Fracture Level
a..
.......
:::::!:
400

V)
V)
300
w
c::::
t-
V) 200

100 L....I.--l....l.i.L-L..-L.U.L....I.--.LJL.I..L...l.......JL.LJJL...J.......L..I..LI.....J.......J....uJ-L......L.J..I.L.....J
10--3 10-1 101 103
ESTIMATED LIFETIME (h)

E~ Estimated lifetime to failure as a function of stat.ic stress level.

Initial flaw size is t.aken to be 40 pm, and n-value is assumed to be 20.

800 1400·C n=20

700
........ 600
0 Fast Fracture Level
a.. 500
.......
:::::!:
400
V)
V)
300
w
~
V) 200

100 L....I.--l....L.I..L--'---L.l..LL....I......L..I..LI.......l.......J....uJL...J.......L..I..LI.....J.......J....uJ---L....L.J..1L.J
10--3 10-1 101
LIFETIME (h)

fig.lQ Experiment.al lifetime under static load at 1400' C. Lines indicate

the estimated values shown in Fig. 9.

553
 ,.... .300,....-~-..-~---,-~---,-..----,
c
~
i' 200b
~
~ 100 0
0 0 o o o
VI

f:~: ::'::
0
0 1 2
Z-VALUE
.3
j
4

Fig.ll (Top) Initial surface flaw length introduced by Vickers

indentation at room temperature, (Middle) fallure strength 3[ p~Icracked
specimens at 1400' C measured with strain rate of 1. 5xl0 s, and
(Bottom) Final flaw length measured on fracture surface after the
fracture at 1400'C for stoichiometric high-purity beta-sialons.

554
Fig.12 F:~ct~fraphs after the bending tests at 1400· C with strain rate of
1.5x10 s for precracked (Vickers 49 N) beta-sialon materials.
{a)z=O, (h)z=0.05, (c)z=0.25, and (d)z=l.O.

, 400·C. 750 MPo

COMPRESSION 0

o
o

Fig.13 Compression creep steady state strain rate of beta-sialons (mean

grain size of about 1-2 ~m ) as a function of z-value.

SCG. In this section, transition from elastic SCG to more creep ductile
fracture only by changing the solute concentration, clearly found in high-
purity beta-sialon series, is described.
All the eight specimens were precracked at I'oom temperature by Vickers
indentation of 49 N. Z-values represent the solute concentration of the
sialons in their general formula of Si 6_ Z AI Z 02jN 8 _ . Initial surface flaw
length (from the center of the indentation untIl Jle crack tip) was found
not significantly different between materials as shown in Fig. 11. All the

555
specim~rs !lere subjected to 4-point bending test with strain rate of
1.5x10 s at 1400·C in nitrogen gas, and their strength are plotted in
Fig. 11. Fracture stress was found drastically decreased between z=O and
0.50, and it kept almost constant between z=0.5 and 3.8. For convenience,
these ranges will be called low-z regime and high-z regime, respectively.
As can be seen in Fig. 12, considerable SCG propagation was found in
fractographs of materials in the low-z regime. The SCG area became
drastically larger with the increase of z-value in the low-z regime, and
it became indistinguishable from the fast-fracture area in the high-z
regime. No plastic strain prior to the fracture was detected in the low-z
materials. In the high-z materials, however, some specimens showed small
plastic deformation prior to the fracture.
These results clearly indicate the transition from elastic SCG regime
to a more creep ductile regime with the increase of z-value. Analytical
treatments assuming the elastic SCG may be useful only in the low-z
regime. With the increase of z-value, SCG resistance may decrease
monotonously, but at the same time creep ductility increases which gives
rise to the crack blunting. As a consequence, strength decreases
monotonously only in the low-z regime which can be considered as elastic
SCG regime, but it does not decrease in the high-z regime. Steady state
creep data measured by compression tests as a function of z-value at
1400·C shown in Fig. 13 well demonstrates the increase in creep ductility
with z-value. Details of the solution effects and their electronic
mechanisms are described elsewhere[15].
As shown in the previous section, Si3NCl.Owt%AIN material exhibits
SCG resistance lower than in Si 3N4 without additives at above 1300·C. In
this material, AIN was found dissolved into Si 3N4 matrix to form dilute
sialons (z=0.07) [16]. The degradation by the AIN addition may be ascribed
to the solution effect.

ACKNOWLEDGEMENTS

Special thanks to Dr. Y. Ikuhara of Japan Fine Ceramics Center for his
helps for a part of flexural tests performed in the Center, and also to
Mr. K. Igashira and Mr. K. Oda of ISIR, Osaka University for their
experimental assistances.

References

1. A.G. Evans and S.M. Wiederhorn, J. Mater. Sci., 9 270-8 (1974).

2. R.K. Govila, Ceramics for High-Performance Applications III
Reliability, Ed. by E.M. Lenoe, R.N. Katz and J.J. Burke ,Plenum Press,
NY ,pp.535-67 (1983).
3. G. D. Quinn and J. B. Quinn, Fracture Mechanics of Ceramics 6 Ed. by
R. Bradt, A. Evans, D. Hasselman and F. Lange, Plenum Press pp.603-36,
(1983) .
4. G.D. Quinn, J. Mater. Sci., 25 4361-76 (1990).
5. M.R. Foley and R.E. Tressler, Proc. Int'l COllf. on Ceramic Components
for Engines, Ed. by V.J. Tennery, The Am. Ceram. Soc., pp.457-71, 1989.
6. I. Tanaka, G. Pezzotti, T. Okamoto, Y. Miyamoto and M. Koizumi,
J. Am. Ceram. Soc., 72 1656-60 (1989).
7. 1. Tanaka, G. Pezzotti, K. Matsushita, Y. Miyamoto and T. Okamoto,
J. Am. Ceram. Soc., 74, 752-59 (1991).
8. D.S. Wilkinson and V. Vitek, Acta Metall., 30 In3-32 (1982).

556
9. D.S. Wilkinson, C.H." Caceres, and A.G. Robertson, J. Am. Ceram. Soc.,
74 922-33 (1991).
10. B.J. Dalgleish and A.G. Evans, J. Am. Ceram. Soc.,6B 44-48 (1985).
11. J. Zeng, I. Tanaka, O. Yamada, and Y. Miyamoto, J. Am. Ceram. Soc., 74
in press.
12. 1. Tanaka, K. Igashira, and T. Okamoto, unpublished.
13. I. Tanaka and G. Pezzotti, J. Am. Ceram. Soc., 74 in pr"ess.
14. J.E. Lane, C.H. Carter, Jr, and R. F. Davis, J. Am. Ceram. Soc., 71
281-95 (l988).
15. 1. Tanaka, S. Nasu, H. Adachi, Y. Miyamoto and K. Niihara, Acta
Metall. Mater., submitted.
16. I. Tanaka, G. Pezzotti, Y. Miyamoto and K. Niihara, J. Mater. Sci.,
submitted.

557
AN INDIRECT METHOD FOR THE DETERMINATION OF da/dN-~K-CURVES

FOR CERAMIC MATERIALS

T. Fett and D. Munz

UniversiUit Karlsruhe, Institut fUr Zuverlassigkeit und Schadenskunde im

Maschinenbau, and
Kernforschungszentrum Karlsruhe, Institut fUr Materialforschung II
Postfach 3640, 7500 Karlsruhe, FRG

ABSTRACT

Crack growth under static and cyclic loads is an important failure mode and responsible
for delayed failure. Knowledge of the crack growth law da/dN =f(dK,) is necessary to make
lifetime predictions in connection with the failure of relevant cracks, Le. small natural cracks.
In this investigation a method is described that allows the crack growth law of natural cracks
to be determined indirectly by measurements of inert strength and lifetimes in cyclic tests. In
order to demonstrate the procedure in detail, measurements are reported for Al20 3-ceramics in
cyclic bending tests with an R-ratio of R=-1.

1. INTRODUCTION

In recent years many efforts have been spent on investigating the cyclic fatigue behaviour
of ceramic materials. For large cracks the fatigue data have been obtained in the same way as
usual for metals. Crack propagation can be measured directly with a microscope combined with
a stroboscope or indirectly by recording the increase in compliance with increasing crack
length. Also electrically conductive layers have been provided on the specimen surfaces to be
able to measure the actual crack length by the potential drop method 1.2. Such macro-crack tests
resulted in da/dN-dK relations.

The behaviour of small cracks is much more important to the lifetime of ceramic compo-
nents with a natural flaw population than the behaviour of macro-cracks is. The fatigue crack-
growth data for such failure-relevant small cracks cannot be derived from results which are
valid for macro-cracks. At least for subcritical crack extension under constant load it is a well-
known fact that the crack growth behaviour of natural cracks differs significantly from that of
macroscopic cracks, especially for such materials with a pronounced R-curve behaviour 3-6.

2. BASIC RELATIONS

The crack growth in one load cycle da/dN is a function of the range of the stress intensity
factor

.!!E....=f(M) (1)
dN
where ~K is dependent on the stress range ~(1 and the crack depth a by
M=~(1j8Y (2a)

Instead of the stress range the maximum stress can be used

Fracture Mechanics a/Ceramics, Vol. 9

Edited by R.C. Bradt et aI., Plenum Press, New York, 1992 559
 ilK = u max (1 - R)ja Y , R = umin/umax (2b)

Especially for a power law relation

(3)

the number of cycles until failure can be easily obtained by integration of eq.(1) from the initial
crack depth a; up to the critical crack depth ac • The initial and the critical naw sizes can be
expressed by:

a.= [ K/ c
'uCY
]2 (4a) - - ]2
a - [ - K/c (4b)
c- umaxY

Equation (4a) can be applied if the inert fracture strength and cyclic fatigue are caused by
the same naw population. Then the number of cycles until failure is given by

BU c n-2
Uc
B n-2
N,=---= n n with (5)
(ilut u max (1 - R)

In a plot of Ig ilu or Ig U max versus Ig N, a straight line with a slope of -1/n must result.

3. EVALUATION OF FATIGUE DATA WITH SPECIMENS CONTAINING SMALL CRACKS

The evaluation of tests with constant amplitude leads to a relation between the stress
amplitude (or u m•.) , lifetime (expressed as N, or t,c) , and failure probability or to a relation
between daldN and ilK.

3.1 Statistical procedure

A statistical procedure to determine the da/dN-ilK-relation is described here. It is analogous

to the method developed for static tests by the authors 7 . It does not assume a power-law
relation between da/dN and ilK. In the evaluation procedure the general relation

(6)

is used with

(7)

(8)

The integral equation (6) can be solved by differentiation and one obtains
2 2
d (N,ilu y ) ilK;
----'---- = -2 -----'-- (9)
d(ilK;) s!E... (ilK)
dN I

Assuming that the same naws are responsible for fatigue failure and for strength, the initial
crack size can be replaced by the inert fracture strength - eq.(4a) - and ilK; by

(10)

After introducing logarithmic derivatives, eq.(9) leads to the crack growth rate daldN at the
beginning of the cyclic test (ilK = ilK;):

560
 (11)

The idea underlying the evaluation of eq.(11) is to use the natural scatter of the strength
and the lifetime and to correlate the corresponding values for the same failure probability. A
number of N specimens are used for strength and lifetime measurements. The results are
ranked and corresponding values ( j th strength and j th lifetime) are used in a 10g(~G/Gej) ver-
sus log(Nfj~G2) plot. From this plot the slope is determined and da/dN is calculated for the cor-
responding Nfj , Gej according to eq.(11). The corresponding ~Kij is given by

(12)

If different numbers of specimens are used for lifetime and strength measurements, the
corresponding values have to be obtained for the same failure probability according to

F= j - 0.5
I N (13)

In principle, this method requires tests to be performed at only one stress level.

3.2 A least-squares procedure

If the lifetime tests are performed at several stress levels and the number of results
obtained at each level is too small, it is recommended to apply a least-squares routine to find
the mean dependency between ~G/Gc and ~G2Nf. If the fitting curve - not necessarily a straight
line - is analytically expressed by

this relation can be introduced in eq.(11) which can be rewritten in a more convenient form
containing only the quantities ~GIGe and ~G2Nf

da 2K/~ ( ~G)2 1 de log ~GIGcJ

dN = -7 --u; ~G2Nf d[ log ~a2NrJ (14)

Thus, the v-K-curve is obtained directly as a mean curve. This variant seems to be best
appropriate for artificial surface cracks with their strongly reduced scatter.

4. TESTING DEVICE

Figure 1 shows a simple testing device 8,9 for cyclic bending tests with R=-1. The specimen
(1) is fixed at its ends in brass tubes (2) by an epoxy resin (3). Due to the low Young's modulus
of the epoxy resin compared with the Young's modulus of the ceramic specimen, the load can
be applied without any notch effect. The second type of specimen fixing may be recommended
for materials with a relatively low Young's modulus (i.e. glass). The cyclic load is generated by
the magnet system of a loudspeaker (4) and transferred to the specimen by a cantilever (5). The
bending moment is measured by strain gauges (6) provided on the fiXing bracket as well as
directly on special specimens used for calibration. By additional application of a spring (7) the
mean stress can be changed in a wide range. At the moment of failure, a silver strip (8) on the
specimen is interrupted, the loudspeaker stops working and a time counter is stopped.

The simple testing device - illustrated in fig.1a - is best suited for resonance applications
resulting in an excellent sinoidal wave shape. In order to study frequency effects it is necessary
to operate far away from resonance. In this case, non-linearities of the load-displacement
behaviour of ordinary loudspeakers have to be expected which may generate disturbing har-
monics. Unfortunately, also the mechanical forces obtainable decrease.

In fig.1b a further development of the apparatus is shown 10. The cooperation of two loud-
speakers results in a correction of non-linear distortions as well as in doubling of the load.

561
 Fig. 1a Testing device and specimen fixing for alternating bending tests.

amplifier

time
counter

Fig. 1b Modified testing device for alternating bending tests.

562
5. MATERIALS AND SPECIMEN PREPARATION

Measurements were carried out on 3.5x4.5x50mm specimens made of two A/z0 3-ceramics:

Material I: A 99.6%-A/z0 3 (AI23, FrialiUDegussit, Friedrichsfeld AG, Mannheim, FRG) with a mean
grain size of 20/-Lm and a density of 3.75g/cm 3 was roughly ground which only resulted in a rel-
atively low strength. Such a surface state will ensure that all specimens will fail on account of
surface cracks. The specimens were annealed in vacuum for 5 hours at 1200°C. Then the sam-
ples were divided into two series. One of them was damaged by Knoop-indentation tests. Due
to the low strength of the 99.6%-A/z0 3 specimens with "natural" crack population larger
Knoop-cracks had to be introduced to ensure fracture at these artificial cracks. This was fulfilled
for Knoop-cracks obtained with an indentation load of 294N. After indentation the Knoop-dam-
aged specimens were annealed once more under the same annealing conditions in order to
remove the residual stresses due to the indentations.

Material II: The second material was an Al z0 3 containing 2.7%SiO z (V38, FeldmOhle AG, Plo-
chingen, FRG). The specimens were diamond machined and then annealed at 900 c C.

2r-----------------,

• A

l fO
O
,.....
D
o
•• '
I. /
L:' 0
I

::;-1
c:
~-2
o

o
. :

... ...
...
t • 10)

o Ib)
• ... ... II)
-3
•
-2~;"20~---'---;;-l;-;:;-----'---~C-=-----L-.J
2.40 2.60
Ig (strength), (strength in MPa)

Fig. 2 Inert bending strength for material I (natural cracks la, Knoop-cracks Ib)
and material II (natural cracks).

6. EXPERIMENTAL RESULTS

Figure 2 shows inert bending strength data obtained in 4-point bending tests, loading rate
dF/dt = 3000N/s, using a transient recorder. The median strength for the Knoop-cracked speci-
mens of material I is Gc = 192MPa and for the natural cracks it results: Gc = 225MPa (material I),
Gc = 360MPa (material II). The fracture toughness was determined with straight edge notched
bending specimens with a saw-cut of 50/-Lm width. The result is: KfC =3.3MPaJffi for material I
and KfC =3.4MPaJffi for material II.

Figure 3 shows the result of cyclic lifetime measurements performed with the two Al z0 3
materials at room temperature in cantilever beam tests (fig.1) carried out exclusively under
alternating' load at 50Hz frequency for specimens with natural cracks as well as Knoop-cracks.

563
 • II)
220 •• •• o

• ..
Ib)
0- 200 A
a..
•• A • 10)

.•
180
---
~

III
III
...
CD

iii 140
160
•
0 cP
~ _.
• rJf----
oa§b
E 00 0
:3120
E 0
·x 00 ITIIIlDD
c ODOlJ 0
E 100
~

80
0.01 1 100
lifetime (h)

Fig. 3 Lifetimes in cyclic tests (R = -1) for material I

(natural cracks la, Knoop-cracks Ib)
and material II (natural cracks).

....
.. •
0
maximum stress
0

• 20 MPo
0
0

0 o 0
---.....
143 MPo
•
0
0
I 0
• •
---
0
:::--1 0
•
•
~ 0
E 0
E
-2 0
•
0 •
-3
-4 -2 0 2
Ig (lifetime) (lifetime in h)

Fig. 4 Weibull representation of the cyclic lifetimes

for material I (natural cracks).

564
7. DETERMINATION OF THE da/dN-MrRELATION

7.1 Statistical procedure

The statistical procedure of evaluation of da/dN is relatively simple and will be outlined
below for the 99.6%-A/20 3 with natural cracks for the special load case of alternating bending
(R =-1). The cyclic lifetimes obtained with the natural cracks (fig.3) are plotted once more in fig.4
as Wei bull distributions. First, the cyclic fatigue data (N t,) have to be related to the corre-
sponding inert strength data G e . In case of Knoop-cracks "with predetermined location of failure
the fatigue and strength data are directly correlated and the cumulative failure probabilities are
identical
(15)

In case of natural cracks the correlation between strength and lifetime data is different.
Since in alternating bending tests with natural cracks the effective surface (volume) is twice the
effective surface (volume) of dynamic bending strength tests, the failure probability of fatigue
data has to be related to the failure probability of inert strength by

(16)

a b c
0.0
° nat. croc ks c Knoop-crocks • not. crocks

-0.1
0""

0" ,0:,
N
"0
<J -0.2
Ol
•
E
° •
-0.3 °

6 8 10 12 146 8 10 12 146 8 10 12 14

Fig. 5 Auxiliary diagrams: a) Material I, natural cracks

b) Material I, Knoop-cracks,
c) Material II, natural cracks.

In the auxiliary diagram, fig.5a, the lifetime quantity t!G 2N, is plotted versus the normalized
stress range t!G/2G e . This diagram provides the derivative necessary in eq.(11).

For application of the statistical procedure it is very important that lifetimes as well as
strength measurements have to be performed using the same loading configuration. This is
indispensable since the scatters in lifetime and strength must not be influenced by use of dif-
ferent testing devices. Furthermore, it has to be ensured that the same crack population is
responsible for strength as well as for lifetimes. This will at least be fulfilled for the Knoop-
cracks when a sufficiently high value is chosen for the indentation load.

565
 -6,r------------, r------------,
a • b

-8

•..
...
.... •
.. •
..
-l41-----L-I----lI_ _.L.J I I I
0.4 0.6 0.8 1. 0.4 0.6 0.8 1.

K,/K 1c

Fig. 6 a) da/dN-6K,-data for material I

(solid circles: natural cracks; dashed lines 80%-scatter band for Knoop-cracks)
b) da/dN-6K,-data for material II (natural cracks).

From the data of fig.5a and application of eq.(11) the da/dN-6K data of fig.6a result. The
relation can be described by

da
-=3·10
-S( -tiK- )28.2 in (m/cycle) (17)
dN 2K ,e

7.2 Least-squares procedure

The least-squares procedure is applied to the Knoop-data of the 99.6%-Alz0 3-ceramic and
the natural cracks of the Alz0 3-ceramic with SiOz shown in fig.3. In figs.5b and 5c the quantity
log 6(1/2(1c is plotted versus log 6(1zN, . A least-squares fit yields

for the 99.6%-Alz0 3 and

for the Alz0 3 containing 3% SiOz. The dashed lines in fig.5b represent the scatter band
describing 80% of the individual results. From these results the da/dN-6K data were obtained
from eq.(14) as represented in fig.6. The crack growth laws resulting from the least-squares
procedures are power laws

~ _ . 10-6( 2KtiK )23.2

dN - 3.8 in (m/cycle) (18)
Ie

for the 99.6%-Alz0 3 and

~ _ . 10-S( 2K6K )26.4

dN - 3.1 in (m/cycle) (19)
Ie

566
 -6r----------

-14·L---__..I...-' 'L-_...J.....J
0.4 0.6 0.8 1.

Fig. 7 Common representation of crack growth data for both materials

for the Alz0 3 containing 3% SiOz. The crack growth data for the Knoop-cracks obtained from the
scatter-band in fig.5b are additionally plotted in fig.6a. A good agreement with the result of the
natural cracks is obvious.

It should be mentioned once more that the lines plotted in fig.7 characterize the range of
scatter where 80% of the measurements are included.

7.3 Direct determination of the power law exponent

Under the assumption that a power law description by eq.(3) is possible - that is the case
for a linear dependency in fig.3 - the parameters of the crack growth law can be determined
directly by a least-squares fit of the lifetime relation 8 .
N f = ft f DC (t.a)2

with the frequency f. Linear regression of the data shown in fig.3 yields for

• Alz0 3 containing 3% Si0 2 : --+ n = 26.4, A=2.5 . 10-27 (in MPa,m,s)

• and for the Knoop-data of the 99.6%-A/20 3:
n =21.5 if all data points are used in the fitting procedure
n = 22.7 if the two outliers at the stress level a max ~ 110 MPa are excluded.

These values are in good agreement with the data represented by eqs.(18,19), as has been
expected.

8. SUMMARY

Measurements of cyclic fatigue were carried out on two A/20 3-ceramics (99.6%A/ 20 3 and
A/20 3 + 3%SiOz) in bending with an R-ratio R =-1. Two types of relatively small cracks have been
considered, namely natural cracks and artificial cracks (Knoop-cracks).

In order to determine da/dN-t.K-curves for small cracks from lifetimes achieved with cyclic
loading a procedure has been derived which is based on a method usually applied to subcritical
crack growth 7 .

567
 The main results are:

• Within the scatter of data both crack types (natural and Knoop-cracks) exhibit the same
da/dN-t.K-relation.

• The exponent of the Paris law (n~23 for material I, n~26 for material II) is significantly
different from the exponent of the power law for subcritical crack growth (n~38 for both
materials8•11 ).

9. REFERENCES

1. R.H. Dauskardt, W. Yu, R.O. Ritchie, Fatigue, J. Amer. Ceram. Soc. 70:C248(1987).
2. N. Brugger, Thesis, Univ. Karlsruhe, 1987.
3. T.E. Adams, D.J. Landini, C.A. Schumacher, B.C. Bradt, Ceramic Bulletin 60:713 (1981).
4. B.J. Pletka, S.M. Wiederhorn, J. Mater. Sci. 17:1247 (1982).
5. K. Chen, Y. Ko, Amer. Ceram. Soc. Bull. 67:1228 (1988).
6. T. Fett, D. Munz, J. of the European Ceram. Soc. 6:67 (1990).
7. T. Fett, D. Munz, Comm. of the Amer. Ceram. Soc. 68:C213(1985).
8. T. Fett, G. Martin, D. Munz, G. Thun. J. Mater. Sci. 26:3320(1991).
9. T. Felt, G. Thun, German Design Patent G 8911720.4.
10. T. Fett, G. Thun, German Design Patent G 9107645.5.
11. T. Fett, D. Munz, Static and cyclic fatigue of ceramic materials, Proc. of the 7th CIMTEC,
24/30 June 1990.

568
EFFECT OF RESIDUAL STRESS DUE TO KNOOP INDENTAnON ON
SUBCRITICAL CRACK QROWTH BEHAVIOR IN CERAMICS *

J.H. Gong and Z.D. Guan

Department of Materials Science and Engineering

Tsinghua University, Beijing 100084, P. R. China

ABSTRACT
The application of indentation technique to the evaluation of elevated
temperature subcritical crack growth (SCQ) behavior of ceramics is examined in
detail, with particular emphasis on the effect of residual stress. A bending strength test
is made to characterize the residual stress field around indentation. Then, the SCQ
velocity, v , is measured as a function of stress intensity, K. , with the extension of
indentation flaws placed on the tensile surface of specimens in 3-point bending. An
obvious deviation exists between the K.- v curves obtained by considering or
neglecting the residual stress effects due to indentation. So a residual stress term is
suggested to be incorporated into the calculation of stress intensity for indentation
flaw in order to establish a precise K.- v curve. With a further discussion on the
earlier period of extension of indentation flaws, it is shown that the stress intensity at
crack tip exhibits a decreasing tendency and a characteristic stress is proposed to
differentiate the mechanisms for the delayed failure of ceramics at elevated
temperatures.

INTRODUCTION
The subcritical crack growth (SCQ) of preexisting flaws, such as machining
damage or inclusions, is recognized as a primary source of high temperature failure of
ceramics. A general way to study SCQ behavior of ceramics is to measure the SCQ
velocity, v, as a function of the applied stress intensity, K.. then establish so-called K.
- v curve. The purpose of such measurement is to gain an understanding of the nature
of crack extension at K1values well below the critical value, K 1C'
Since the end of 1970s, several authors (\-)) have explored the efficacy of using
indentation flaws in conjunction with bend loading to measure K 1- v relationship.
The advantages of such a method is confirmed as: (1) The dimensions of indentation
flaws are of the same order of magnitude as those of natural flaws (J) ; (2) a very low
crack velocity, which plays an important role in the lifetime prediction of ceramics, can
be measured with this technique (2) • The main obstacle for using this method is the
effect of residual stress around indentation, as the another applications of indentation
flaw technique (4,5) •

* This paper is done under the cooperative res~arch contract with Hitachi Chemical
Co., Ltd.
Fracture Mechanics a/Ceramics. Vol. 9
Edited by R.C. Bradt et al.• Plenum Press, New York:, 1992 569
 I 2c {
""""""111" I
~
A B
Fig. 1. (A) Schematic of Specimen Showing Traces oflndentation Flaws and
(B) Fracture Profile of Knoop Indentation Flaw in Depth of Specimen

In this paper, the effect of residual stress on subcritical growth of indentation

flaws in a pressureless sintered Si3N. is studied.

EXPERIMENTAL PROCEDURE

A pressureless sintered Si,1N. is selected for this study. Test specimens are of
dimensions 4mm wide x 3mm thick x 36mm long approximately. The tensile surface of
specimen is polished carefully using MO.s# diamond paste and the edges are well
chamfered. Then all specimens are subjected to air annealing at 800t for 30 mins.

Several indentation flaws of same size are introduced into the tensile surface of
specimen by Knoop indentation. These flaws are oriented perpendicular to the
longitudinal axis of specimen and at least 2mm apart; it is reasonable to assume that
this is a sufficient distance to prevent the stress field in the vicinity of the flaws from
interacting on loading (I) • Figure I (A) shows schematically the traces of flaws placed
on the tensile surface of specimen and Figure I (B) shows the flaw profile in fracture
surface of specimen.
After measuring the initial dimension, the indentation flaws are extended by
subjecting the specimen to constant bending stresses at high temperatures for
durations of 180s to 25000s, respectively. Test temperatures of 1lOOt and 1200t are
used. All experiments are conducted in air and the specimens are held at the testing
temperature for about 10 min before load is applied. After specimens are unloaded
and cooled to room temperature, the crack extension on the surface of specimen are
measured by optical microscopy. The thin surface oxide layer formed at high
temperature is removed by slightly polishing the surface before the measurements to
promote the accurate measurement of crack length.
In order to obtain the magnitude parameter of residual stress, 'Ir , some other
specimens with only one indentation flaw placed at the center of span are prepared to
measure 3-point bending strength at same conditions. A span of 30mm and crosshead
speed of O.OSmm / min are used.

RESULTS AND DISCUSSIONS

Determination of Magnitude Parameter of Residual Stress

Accounting of the effect of residual stress around indentation, the total stress
intensity at the tip of indentation flaw in a bending beam can be described as (6) :

K. =K a +K r (l)
where the terms

and
K a =M e q a
Fi
-
a
Q (la)

570
 xr P
Kr = C3/2 (lb)

respectively represent the contributions from the applied loading and the residual
stress around indentation. In these equations, a and c are flaw depth and half-length,
respectively; ua is applied bending stress; P is indentation load; Me is a numerical
factor related to flaw and specimen geometry; Q is a flaw geometry factor; and Xr is a
dimensionless constant which characterizes the magnitude of residual stress.

At critical condition, qa = qr, K I = K lc, rearranging Eq.(l) as:

q
r
+~(.!-)
Y 2.,fa fT
~ =Ky IC .,fa (2)
a C a

where qr is fracture stress of specimen and Y a = M "1t/ Q which has been proved to
be a constant for a given indenter / material system (6) •

Since both a / c and P / c2can be treated approximately as constant for ~ given

material (6) , Eq.(2) shows that a linear relationship exists between qr and 1/ a,
making it possible to use linear regression to calculate the Xrvalue with a series of
bending beam having different indented fla~ depths from Eq.(2), which is included in
the term respresenting the intercept of qr - 1/ a line.

The experimental results of strength testing of indented bending beam is given in

Table I.

Table 1. Knoop Indentation Flaw Depth a Dependence on Fracture Strength qr

Temp. ale Ya Regression Result Xr

1100t 0.855 ± 0.005 1.255 ± 0.005 q r + 104.11 = 4.33Jf (r = 0.9899) 0.0425

1200t 0.853 ± 0.012 1.257 ± 0.009 q r + 75.56 = 3.97 Jf (r=0.9949) 0.0309

(* P / c2 =2855.20± 19.25MPa for the indentation load range used)

The Effect of Residual Stress on KI- v Measurements

The flaw extension measurement with different steady loading duration are
carried out at 1100t and 1200t, respectively. The test data are given in Table n.

Table n. Data for Crack Extension Due to Sustained Loading

Applied Load C;:ondition Crack Length (mm)
NJ Temperature
Load(Kg) Duration(s) Initial Filial
1 1l00t 8.5 25000 0.150 0.202-0.226
2 1100t 16.0 2500 0.176 0.185-0.217
3 1l00t 17.0 1800 0.260 0.264-0.281
4 1200t 12.5 10500 0.176 0.202-0.605
5 1200t 14.0 6010 0.172 0.235-0.948
6 1200t 17.0 950 0.245 0.452-0.752
7 1200t 20.0 400 0.172 0.175-0.235

571
 )0-6.-- ---.
10-7 r - - - - - - - - - - - - ,
o Assume 1',=0
• When 1', Exists

0
0

10-8
0
I- 0

,....., 00
0
0
.-

'"
0:
• 0
.........
e
• 0

0 :.:.
'-'
:>-
0
0
•••
o
• 0

.0

10-9 o

10.... (B)
(A)

10-1
2 3 4
K, (MPaJ~)

Fig.2. KI-v curves for SSN at (A)IIOOt and (B)1200t

The method for calculating the values ofK I and v used are shown as:

- Aa (3a)
v= At
Kia + K n
R, = 2 (3b)

where At is the loading duration; Aa is flaw extension in depth of the specimen

calculated from measured value of 2c, the flaw length in surface of specimen, by
assuming ( I ) the a I c ratio of indentation flaw remains constant during flaw
extension; and K IO and K u are stress intensities correspond to initial and final states
of flaw extension respectively and determined with Eq.(1).
In figure 2, average cracking velocity, v,is plotted as a function of average stress
intensity, K I . Obviously, the KI-v curve can be devided into three regions. The first
is a lower velocity region where the slope is steeper and a distinct SCG threshold exists
at crack velocity nearly 10-9m / s. The second is a medium velocity region where a
power relation exhibits between v and K I , i.e., v = AK~ . The third is a higher
velocity region which is usually neglected in SCG study.
In order to show the effect of residual stress on K I - v measurments, a K.- v
curve is plotted in Figure 2(B) with the K r =0, i.e., neglecting the effect of residual
stress by treating Xc as zero. It is obviously that a deviation appears between the two
curves. This phenomenon can be explained with Eq.(I) and (3b). Denoting AK as this
deviation, we can deduce from the discussion above:

AK=R I -R a

=~[l
312
+ (Co )3/2 ]
C
(4)
2Co I

where Co and c i are crack dimensions before and after crack extension, respectively.
Eq.(4) shows in fact that AK decreases with c l , then with the crack velocity for a

572
certain interval of loading time. This analysis is confirmed by the experimental results
in Figure 2(B).
This deviation may influence the determination of SCG parameters directly.
Table ill gives the calculated values of N and A in the power relation v = AK~ and
SCG threshold K th • The direct comparison of the results listed in Table ill seems to
prove that residual stress plays an important role on the subcritical growth of
indentation flaw. Especially, the threshold do not appear in measured K J- v curve if
the residual stress effect is neglected at 1100t.

Table m. Effect of Residual Stress on SCG Parameters

Test When Xr exists Assume Xr=O
Temperature N A N A
1100t 2.89 3.02 x 10-10 1.88 2.14 x 10-9
1200t 2.68 2.20 x 10-9 1.84 2.52 x 10-9

Residual Stress Effect in Low Velocity Region ofKJ-v curve

Since the low velocity region of K 1- v curve plays an important role in

determining the life of ceramic components under stress, it is necessary to study the
effect of residual stress about indentation on the behavior of cracking in this region in
detail.
Subjecting the indented specimen to a bending stress, the indentation flaw will
extend and the stress intensity about flaw tip will change with the extended flaw
dimension, according to Eq.(1). The variation of K J with flaw dimension, a ,can be
illustrated in Figure 3 for seveal certain applied stresses. These curves pass through a
well-defined minimum. For arbitrary values of applied stress and indentation load,
the dK J/ da = 0 defined the minimum in Figure 3, which we designate by the subscript
m:
(5)

where A' is a constant. Given a / c = 0.85, we can obtain:

A' = 1.71y J/4 (X P) 1/4 (6)
r

The point at which the K J- a curves in Figure 3 intersect the horizontal line
K J= K th , the SCG threshold, correspond to an equilibrium state, Le., the crack will
arrest at this condition, cracking or arresting of indentation flaw according to whether
the value of K m is larger or smaller than K th • A continuous crack extension is
>
expected to occur if K m K th while the crack extension will stop after a certain time if
K m (K th • In the latter, the average value ofvcalculated with Eq.(3a) may be less than
the actural value since an overestimated loading time is used. In other words, a
considerable error may be introduced in the low velocity region of K J- v curve
determined with the present indented bending beam method.

Since K m decreases with applied stress, G'a , a criterion for determining the
mechanisms of delayed fracture of ceramics may be presented by a further discussion
with Eq.(4) and Figure 3.

Two mechanisms have been presented for the delayed fracture of ceramics at
elevated temperatures: subcritical crack growth (SCG) and creep rupture (7) •
Although both have crack growth stages, the main distinctions are that SCG
originates from preexisting flaws and creep rupture has bulk deformation and
microcracking and may not necessarily involve preexisting defects.

573
 a
Fig.3- The Variation ofK J with Extended Flaw Dimension a

It has been shown experimentally by Grathwohl (8) that there is a characteristic

applied stress, ero, above which the failure of ceramics is controlled by SCG and below
which controlled by creep rupture. This experimental result can be confirmed with the
K J- a curves for different era levels in Figure 3: if er.) ero, then K m > K th, a continuous
extension of indentation flaw OCCUrs and the failure of ceramics is controlled by SCG.
If era < ero, on the other hand, the slow growth of indentation flaw will stop
spontaneously after a certain time for the stress intensity about crack tip reduces below
SCG threshold, K th , then the failure of ceramics may be controlled by creep rupture.
This analysis seems to say that the concept of SCG threshold may be applied in the
study of the delayed fracture mechanism of ceramics at elevated temperatures

CONCLUSIONS

The following conclusions may be draw from the present study:

(1) An obvious deviation exists between the KJ-v curves obtained by considering
or neglecting the residual stress effects due to indentation. So a residual stress term is
suggested to be incorporated into the calculation of stress intensity for indentation
flaw in order to establish a precise KI-v curve.
(2) In the earlier period of extension, the stress intensity about crack tip of
indentation flaw exhibits a decreasing tendency, then affecting the accuracy of K J- v
measurements.
(3) SCG threshold may be a characteristic parameter for distinguishing between
two mechanisms for delayed fracture, SCG and creep rupture, of ceramics.

REFERENCES

(I) M.G.Mendiratta and 1.1.Petrovic, 1. Am. Ceram. Soc., 61 (1978) 226-30

(2) M.Kawai, H.Abe, and 1.Nakayama; pp.587-601 in "Fracture Mechanics of
Ceramics· , Vo1.6. Edited by R.C.Bradt, A.G.Evans, D.P.H.Hasselman, and
F.F.Lange (plenum, New York, ]983)
0) M.Yoda and Y.Yoshikawa, J. Am. Ceram. Soc., 70 (]987) C-30]-C-302
(4) D.B.Marshall and B.R.Lawn, J. Mater. Sci., 14 (1979) 200]-12
(5) D.B.Marshall, J. Am. Ceram. Soc., 66 (1983) ]27-31
(6) J.H.Gong and Z.D.Guan, J. Chinese Ceram. Soc., 19 (1991) 234-4]
(7) G.D.Quinn, J. Mater. Sci., 22 (1987) 2309-18
(8) G.Grathwohl; pp.573-86 in "Deformation of Ceramics· , Vo1.2. Edited by
R.E.Tressler and R.C.Bradt (Plenum, New York, 1984)

574
EFFECT OF SURFACE CHARGE ON SUBCRITICAL CRACK
GROWTH IN GLASS

Shin-ichi Takeda and Isao Tari

Faculty of Engineering, Okayama University
3-1-1 Tsushima-naka, Okayama, 700 Japan

ABSTRACT

Stress corrosion of glass proceeds with a chemical process which

involves a stress enhanced chemical reaction between the reactant
species and the highly stressed glass surface near the crack tip. In
this paper, effect of surface charge formed at the glass/solution
interface on subcritical crack growth was investigated in order to
elucidate the mechanism of the stress corrosion of glass.
Post-indentation slow crack growth in soda-lime silica glass in various
aqueous RNO,(Ri Li+,Na+,K+,Rb+) solutions was observed by measuring the
crack length with time after indentation. The crack growth was found to
depend on the pH, the concentration, and the nature of electrolytes.
These behaviors suggested that the surface charge density which was
controlled by the chemical composition of the solution affected the
subcritical crack growth. In the pH range above 10 where the
dissolution of the glass markedly occured, crack growth also depended
on the surfece charge.

1. INTRODUCTION
Adsorption-induced reduction in the hardness of nonmetalic solids
were first reported in 1928 by Rebinder [1] and are known as Rebinder
effects. In the period of time since Rebinder's first announcement, many
others have reported that surface-active media (aqueous solutions,
long-chain organic compounds, etc.) affect the plasticity and/or
fracture of a variety of solids, including metals, polymers, amorphous
glasses, etc. [2] [3] . In particular, Westwood and his co-workers
reported that such phenomena - - - adsorpt ion - induced hardening as well as
softening- - -may be understood in a conceptual way in which the space
charge redistribution occurred in the solid surface [4]. In the case of
soda-lime silica glass, the hardness, rate of drilling with diamond
bits, and fracture energy exibit a maximum in heptil alcohol, in which
the zeta-potential of soda-lime silica glass is ~ 0 [5].

Fracture Mechanics a/Ceramics, Vol. 9

Edited by R.C. Bradt et aI., Plenum Press, New York, 1992 575
 Subcritical crack growth in glass should be associated with the
redistribution of the surface charge as was seen in the papers on
Rebinder effect. In 1975, Wiederhorn and Johnson attempted to manifest
the effect of zeta-potential on the fracture of soda-lime-silica glass
in aqueous solutions by fracture mechanics techniques, but resulted that
its effect was not observed [6] . From the results, we thought that the
velocity of crack growth observed in their fracture experiment was
higher than the rate of redistribution of surface charge. In this
paper, we describe the pronouced effects of the surface charge on the
subcritical crack growth obtained from the experiment in the slow range
of crack velocity.

2. EXPERIMENT

2.1 Glass samples

Commercially available soda-lime-silica glass(produced by Matsunami
Glass Ind. ,Ltd. Japan) was used as glass sample. Plate-shaped specimen
with 1.2-1.5mm in thickness was used for measurements of the streaming
potential and for the crack growth experiments. For dissolution
experiment, the glass plate was grounded into powder with particle size
-149 to +280 mesh, classified, and annealed in an electric furnace.

2.2 preparation of aqueous solutions

The aqueous solutions used for measurements of streaming potential,
crack growth experiments and dissolution experiments were prepared as
follows.
(1) The pH of an aqueous solution was adjusted by adding dilute HNO, or
KOH solution to a KNO, solution of 10. 4 -1 mol/dIn" (M). (2) To investigate
a dependence of the concentration of electrolytes on crack growth, RNO,
solutions (R=Li,Na,K,Rb) were diluted to obtain 10.'-10. 4 Mof solutions.
(3) The solutiuons contained zinc, aluminium, cobalt, and nickel ions
were diluted with 1M KNO, solution. (4) The pH of the solution used for
the measurement of streaming potential was adjusted by adding dilute HNO,
or KOH solution to a KNO, solution of 10. 2 M. A pH meter(made by TOA
Electronics Ltd. Japan, Type HM-26S) was used to measure the pH of the
solutions.
2.3 Crack growth experiment
The crack growth experiments were performed in aqueous solutions
with various pH values, and concentrations of electrolytes to obtain
various charged states at the glass/solution interface. Vickers
indentation fracture method was used in order to induce the microcracks
on the glass surface. Specimens with the induced microcracks were
immersed in various test solutions and the length of the crack growth
during immersion was measured. Figure 1 shows the measuring procedure
for crack growth in test solutions. First, Vickers indentations were
made on glass surfaces in air environment using a microhardness
tester (DMH-2, Matsuzawa Seiki Co. ltd. , Japan). When the length of
median/radial cracks attain 95~m after unload, the specimen was put into
the solutions for various periods at 25~. Next, the specimen was taken
out of the solution and the crack length was measured using a

576
 I
I
Indentation in air
P=9.8 N, 1Ssec

Measurement of crack
length in air before immersion

Immersion in aqueous Crack

growth
solutions at 2SoC

It

Measurement of crack length

in air after immersion
1
----------

Figure 1. Measurement of subcritical crack growth in soda-lime

silica glass in aqueous solutions.

microscope. About 35 measurements of the crack length were made under

the identical condition and the mean values were determined.

2.4 Measurement of streaming potential

The streaming potential developed at the glass/solution interface
was measured in the pH range from 2 to 12 by the streaming potential
method.

2.5 Dissolution test

The glass powder weighing 0.2 grams was immersed in 50ml of the
test solution for 24 hours at 25°C. The supernatant was pipet ted off and
the amount of the dissolved silica component was determined by the
molybdenum blue method.

3. RESULTS AND DISCUSSION

3.1 Charged state at oxide-type glass/solution interface
When a solid is immersed in liquid medium, surafce charge developed
through the electrochemical interactions with solution which involves
ion and/or electron transfer [7] [8]. In the case of soda-lime silica
glass which can be ragarded as a metal oxide, proton can act as a
potential determining ion. Therefore, the surface charge density at the
glass/solution interface depends on the amount of protons contained in
the test solutions. Figure 2(a) shows a typical relation between
streaming potential of soda-lime silica glass and solution pH. This
figure shows that the isoelectricpoint of this glass was not obtained,
and the streaming potential has the maximum value at pH 2-3, because the
hydrophobicity may affect the wettability of glass in the acidic
solution[9]. In the pH range from 2-10, streaming potential increased
with increasing pH so as to reflect the negative surface charge
development due to the dissociation of proton from the surface hydroxy

577
 -0.10

Jg
e 0
·0.08 f-
s: 0
00

..,
0
0
:§ oe
•
0
E -0.06
CD
'0 0
C-
Cl -0.04
om' 0
c:
'E oQ.
aI
~ ••
li) -0.02 •
I
0.00
0 2 4 6 8 10 1214
Solution pH I -
Figure 2(a). Streaming potential as a function of solution pH for
soda-lime silica glass in aqueous solutions.
solution; 10·> M KNO,. immersion time; 0 for 5min
• for 24 hours.

2.5

E 2.0
c-
c-
O
0 1.5
en 0
't:l
CD 1.0 00
.2
0 0
'"
0'"
0.5
00
0

.~oO«p
0.0
0 2 4 6 8 10 12 14
Solution pH I •
Figure 2(b). The amounts of dissolved silica as a function of solution
pH for soda-lime silica glass in aqueous solutions.

578
groups. On the contrary, in the pH range above 10 the potential
decreased with increasing pH. Figure 2 (b) shows the results on the
amount of dissolved silica component. Compared the results shown in
Figure 2 (a) with Figure 2 (b), we considered that the decrease of the
streaming potential in the pH range above 10 is partly correlated with
the dissolution of the silica component which acted as a releasing
charge to the solution.
The factors, other than solution pH, dominating the surface charge
at the oxide-type glass/solution interface are (1) the concentration of
electrolytes and (2) the nature of electrolytes. In the field of the
surface chemistry, many data were already reported on the surface charge
density of silica in aqueous solutions [10-12] . The former factor
affects surface charge density in the manner that the charge density
increases with increasing the concentration of ions. The latter factor
also affects the negative surface charge density in the sequence of

The same results on the surface charge can be predicted for the
charged state at soda-lime silica glass/solution interface as was seen
in silica surface from both concentration and nature of electrolytes.
We also examined the effect of surface charge on the subcritical
crack growth us ing the solut ion with zn", Co", Ni", Al J. ions, which have
been well-known to change the surface charge by specific adsorption [13] .

3.2 Change of the crack length with immersion time

Figure 3 shows that the relation between crack length and immersion
time of specimens in aqueous solutions with various pH. Each point of
the data indicates the mean value of about 35 measurements obtained
under the identical condition. The standard deviation of each
measurement was about 2%. For immersion time less than 5 minutes, there
was no significant difference in crack lengths for any solution pH.
After that time, the rate of crack growth gradually decreased in lower
pH values, and finally the crack length depended on the pH values. In
the pH range from 1 to 10, the higher the pH value. the more the crack
grew. After 24 hours, no further crack growth was apparently observed.
This shows that the crack growth in such a solution reached the steady
state in 24 hours. The crack growth rate calculated from this figure
was about 10- 7 m/s at the initial stage of crack growth(l minute after
immersion), and about 10- 11 m/s at the final stage(24 hours after
immersion). These results indicate that when the crack growth rate was
decreased as the effective residual force is considerably relaxed, the
influence of the pH was remarkable, and the crack growth almost
approached a different staedy state, that is, fatigue limit with
different pH. This variation of fatigue limit with pH corresponds to
the variation of the charged state at the glass/solution interface with
pH. As the purpose of this paper was to manifest the pronounced effect
of the surface charge on the subcritical crack growth, the immersion
time of the test specimen was fixed at 24 hours.

579
 125 305 5min 1h
r-::..;:-:=------::.;=~-:..;.:....--~::;:.:...:...-~;=....=~
24h lOd 25d
pH
• 12.0
120 <) 10.5
o 9.0
o 6.9
E () ~.O
::>. 115 • 1.0

110

Immersion time I sec

Figure 3. Crack length as a function of immersion time for soda-lime

silica glass in aqueous ssolutions.

125

-P
Crack-length

0
0
0 0
120
E
::>. ~
.<::
00
0> 0 0
c: 115
~ CO
.>:
t.>
co 0
()
0
110 HNO:J-KOH
0 0
-0 00 0
0

105
0 2 4 6 8 10 12 14
Solution pH I -

Figure 4. Crack length as a function of solution pH for soda-lime silica

glass in aqueous solutions. The solution pH was adjusted using
KOH or HNO, solution.

580
3.3 Effect of solution pH on subcritical crack growth
Figure 4 shows the relation between crack length in a specimen
immersed in aqueous solutions for 24 hours and the solution pH. In this
figure, each point also indicates the mean value of about 35
measurements, and its standard deviation was about 2%. The solution pH
remarkably affected on the subcritical crack growth. The crack length
was a minimum when the pH was about 2-3. In the pH range from 4 to 10,
crack length increased with increasing solution pH. In the pH range
above 10, the crack length decreased with increasing pH. Comparison of
these results with the charged state of glass shown in Fig.2(a) leads to
an important remarks that the dependence of crack growth on pH agreed
with the dependence of the charged state on pH.

125
00
° 0&
0° 0
oce
Q)
Q

°
(9
120 0
E
:::l. °
L: ca 0
en
c 115 0/}9
~ 8
.,;,
<J
0
<1l
0 8
CD
110 Q:o IO·2 M KN03
00
pa:,0q,°

105 L.......L-'-"'--'--'-""'---''-'-...........-'--'---'--'--'
o 2 4 6 8 10 12 14
Solution pH I •
Fig. 5(a). Crack length as a function of solution pH for soda-lime
silica glass in aqueous solutions. The solution was 10-2M
of KN03.

3.4 Effect of the concentration of electrolyte on subcritical

crack growth

We also investigate an effect of the surface charge on crack growth

by changing the concentration of electrolyte. Figures 5 (a), (b) show
that the results of the crack growth in various concentration of the
potassium ion in the whole pH range. These figures shows that in the pH
range from 4 to 10, crack length increased with increasing the

581
 125 I-
o -
o~~oo
o 00
o 0
00 Q)o
o
120 tf g
E
~
§ 00

0 o
.s:: o
'5 o
c 115 ~ 0
2
~
0
<ll
a
0
o
U
110 1M KN~
o~
P<9
0

105
0 2 4 6 8 10 12 14
Solution pH I -

Figure 5(b). Crack length as a function of solution pH for soda-lime silica

glass in aqueous solutions. The solution was 1 M of KNO,.

pH.i.8 0
125 0
0 0
00 • •
0
• pH.5.6
•
120
E
:1.
0 •
.c
0 •
e;, (J

c
-
(J

••
CD 115
~ 0 (J
U pH.4.0

0
<II
• o eJ
I<-
110 0
(J o Q.
0 0 0 0
0 (J
pH.2.0

105
1<r4 10"3 ltr 10-l
Concentration of KNO J I M

Figure 6. Crack length as a function of KNO. concentration for soda-lime

silica glass in aqueous solutions. solution pH ; ( <> )=6.8,
( • )=5.6, ( () ) =4.0, ( 0 )=2.0.

582
concentration of potassiumu ion. A relation between crack length and
concentration of potassiumu ion in the pH range from 2 to 7 is shown in
Figure 6. I t can be seen from this figure that a concentrat ion
dependence of potassiumu ion on crack growth was noticeable with
increasing the negative surface charge. According to the papers
reported on the surface charge in aqueous solutions, the surface charge
density of silica in aqueous solutions was found to increase with
increasing of concentration of alkali metal ions in the pH range 4 to
10(11]. This tendency of surface charge density was found to agree with
the results on the crack growth.

3.5 Effect of the nature of electrolyte on subcritical crack growth

Figure 7 shows that the results on the crack length measured after
immersion for 24 hours in the solution involved various nature of the
alkali-metal ions. In the concentration of alkali-metal ions from 10·' -1
M, crack length increased with increasing concentration of any
alkali-metal ions. In addition, their cencentration dependence was
different in each ions. The Hofmeister series which was well-known in
the field of surface chemistry and colloid chemistry

Rb· > K· > Na· > Li·

was observed in the crack growth in aqueous solut ions. These results
also agreed with the result predicted from the surface charged
state(ll] (12] at the glass/aqueous solutions interface.

125 <>
.
a
5
<>
0

E 120 <>
•
~
J
::I.
• 0
0

e•
<J
.s::.
0>
c: 0
~
.,;, <>
<> 115 ~ 0 0
<II
<J • <> FlbNO,
U
~
• KNo,
0 <J NaNo,
OLiNO,

110
lCr' 10-3 10-2 Hyl
Concentration M

Fig. 7. Crack length as a function of the concentration of alkali metal

ions for soda-lime silica glass in aqueous solutions.

583
3.6 Effect of specific adsorbed ion on the subcritical crack growth

To investigate an effect of the specific adsorbed ion on crack

growth, we chose zinc ion for the test. In Figure 8, remarkable effect
of adsorbed zinc ion on the crack growth was found in the pH at about 7.
This result was also explained by the surface charge which was
compensated by adsorption of positively charged zinc ion on the
negatively charged surface. Figures 9,10, and 11 show the results using
the solution containing aluminium, cobalt, and nickel ion as specific
adsorbed ions. There found to be the same phenomena as was seen in the
case of zinc ion which affected the crack growth. Each figure shows an
inhibiting effect on the crack growth. All these results also suggested
that the redistribution of surface charge induced by adsorption of metal
ions affect the subcritical crack growth. At the present time, the
definitive mechanism for the redistribution of surface charge induced by
adsorption could not be revealed. On this point, much more experiments
at the electronic level were needed to elucidate the mechanism of
subcritical crack growth.

4.CONCLUSION
The effect of surface charge on the subcritical crack growth in
glass was investigated using soda-lime silica glass as the oxide-type
glass sample. The crack growth was found to be affected by the pH, the

~
000
00 0
«5'0
120 1M KNO> <:P 0

- •,
,.
E 0
=. 115 o I

...
0
I·
•• •
o'
110 °i
• •...
l!I"
e· .-
•

105

2 4 6
-•
100 L-.-..................--'-~~~.......................-......J
a 6 10 12 14
o 2 4 6 6 10 12 14
Solution pH I -
Fig. 8. Crack length as a function of solution pH for soda-lime silica
glass in aqueous solutions. The solution was IO-3M of Zn(N03)2-

584
 125 Q)
'8
1 M KNO] 000
00 0
~0

120 & ••
0

E
•
~

.c
0>
•• • .~• 0
•0
c: 115 0
.!!!
-'0" • • •
U
nI
•
~ !.
<t)

110 08•• 1M KNO]

:,~
10; M AI(NO])
<:3

105
o 2 4 6 8 10 12 14
Solution pH I •

Figure 9. Crack length as a function of solution pH for soda-lime silica

glass in aqueous solutions. The solution was 10·'M of Al(NO,),.

125
Q)
g
000
00 ~

...- ••
• ~o
120 1M KNO, c:P 0
E •
•• •• •
~

.c
0>
c:
.!!! 115 0
••
•• , •
.,
! i
-'0"
nI
• ~
U ~
0•

00
•
110
o
-;
0 •
.
1M KNCh
KT'M Co<NO>h
••
lOS
0 2 4 6 8 10 12 14
Solution pH I •

Figure 10. Crack length as a function of solution pH for soda-lime silica

glass in aqueous solutions. The solution was 10·' M of Co (NO,),.

585
 125

..•
CO

..,00":
~

a
~
E
120 1M KM:lJ at • • ••
~ • oe
• •
•a
~

0
c:
oS!
•
.xu 115 a a

~
~
• ••
a
110
•
00· .
1M KNOJ

a a •
a
• 1O"M Ni (NOl),

•
105
0 2 4 6 8 10 12 if.
Solution pH I -

Fig. 11. Crack length as a function of solution pH for soda-lime silica

glass in aqueous solutions. The solution was lO-3M of Ni(N03)2'

concentration, and the nature of the electrolytes which change the

surface charged state of the glass. It was also revealed that the
surface charge induced the redistribution of the charge existing in the
glass surface, and hence the redistribution of surface charge greatly
affected the subcritical crack growth in very slow range of the crack
veloci ty. Further study on the mechanism of the redistribut ion of
surface charge should be done for more precise understanding the
subcritical crack growth.

ACKNOWLEDGMENT

Grateful acknowledgments is made to Messrs. S.Nakada, Y.Sakamoto,

and M.Ohnishi for their assistance in this study.

REFERENCES

l.P.A.Rebinder,"Effect of surface energy changes on cohesion,hardness,

and other properties of crystals", in Proc. Sixth Physics Conf.,
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2.A.R.C.Westwood and R.M.Latanision, "Environment-sensitive machining
behavior of non-metals", in Proc.of the Symposium on the Science of
Ceramic Machinig and Surface Finishing, edited by S.J.Schneider,Jr.,
and R.w.Rice, (Nat.Bur.Stand. (U.S.), Spec.Publ.,1972,No.348), P.141.
3.M.v.Swain, R.M.Latanision, and A.R.C.Westwood, "Further studies on
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J.Am.Ceram.Soc., ~, 372 (1975).

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R.M.Latanision and J.T.Fourie, (Noordhoff,Leyden, 1977), p.3.
5.N.H.Macmillan, "Chemisorption-induced variations in the plasticity
and fracture of non-metals", in Surface Effects in Crystal Plasticity,
edited by R.M.Latanision and J.Y.Fourie, (Noordhoff,Leyden,1977),
p.629.
6.S.M.Wiederhorn and H.Johnson, "Effect of zeta potential on crack
propagation in glass in aqueous solutions:, J.Am.Ceram.Soc.,Disc. and
notes, 2i, 342 (1975).
7.R.O.James and G.A.parks, "Characterization of aqueous colloids by
their electronical double-layer and intrinsic surface chemical
properties", in Surface and Colloid Science, edited by E.Matijevic,
(John Wiley & Sons,1982, vol.12), p.119.
8.Y.Aikawa, A.Takahashi, and M.Sukigara, "Effect of electrical
potential floating of titanium(IV) oxide particles on photocatalytic
reaction", Nihonkagakukaisi, 292 (1984).
9.J.Laskowski and J.A.Kitchener,"The hydrophilic-hydrophobic transition
on silica", J.Colloid and Interface ScL, 29, 670 (1969).
10.G.H.Bolt, "Determination of the charge density of silica sols",
J.Phys.Chem., ~, 1166 (1957).
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at the silica-aqueous electrolyte interface and the role of some
cataions", J.Electroanal.Chem., 12.,267 (1968).
12.R.P.Abendroth, "Behavior of a pyrogenic silica in simple
electrolytes", J.Colloid and Interface ScL, li, 591 (1970).
13.R.O.James and T.W.Healy, "Adsorption of hydrolyzable metal ions at
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587
International Editional Board

R.C. Bradt, Mackay School of Mines, University of Nevada-Reno, Reno, Nevada 89557-0047
USA

D.P.H. Hasselman, Dept. of Materials Engineering, Virginia Polytechnic Institute and

State University, Blacksburg, Virginia 24061, USA

D. Munz, Institut fiir Materialforschung II, Kernforschungszentrum Karlsruhe

75 Karlsruhe 1, GERMANY

M. Sakai, Dept. of Materials Science, Toyohashi University of Technology, Toyohashi 441

JAPAN

V.Ya. Shevchenko, High-Tech Ceramics Research Center, Academy of Science of The USSR
Ozernaya 48, Moscow 119361, USSR

Organizing Committee

N. Soga, Dept. of Industrial Chemistry, Kyoto University, Kyoto 606, JAPAN

O. Kamigaito, Toyota CRDL, Aichi-Gun 480-11, JAPAN

K. Funatani, Japan Fine Ceramics Centre, Nagoya 456, JAPAN

Y. Hamano, Kyocera Corporation, Kyoto 607, JAPAN

Y. Kagawa, Institute of Industrial Science, The University of Tokyo, Minato-ku 106, JAPAN

T. Kishi, Research Centre for Advanced Science and Technology, The University of Tokyo
Megro-ku 153, JAPAN

M. Matsui, Analysis and Properties Research Lab., NGK Insulators, Ltd., Nagoya 467
JAPAN

K. Niihara, The Institute of Scientific and Industrial Research, Osaka University

Ibaraki 567, JAPAN

M. Sakai, Dept. of Materials Science, Toyohashi University of Technology, Toyohashi 441

JAPAN

M. Takatsu, Dept. of Materials Science and Engineering, Nagoya Institute of Technology

Nagoya 466, JAPAN

589
S. Wada, Toyota CRDL, Aichi-Gun 480-11, JAPAN

E. Yasuda, Tokyo Institute of Technology, Yokohama 227, JAPAN

Session Chairs

K. Ahlborn, Central Research and DevelOpment, Carl Freudenberg, 6940 Weinheim

GERMANY

Y. Akimune, Central Engineering Lab., Nissan Motor Co. Ltd., Yokosuka 237, JAPAN

R.C. Bradt, Mackay School of Mines, University of Nevada-Reno, Reno, Nevada 89557-0047
USA

J.T. Dickinson, Dept. of Physics, Washington State University, Pullman, WA 99164-2814

USA

G. Fantozzi, INSA, GEMPPM, U.A. 341, Lyon, FRANCE

K. Funatani, Japan Fine Ceramics Centre, Nagoya 456, JAPAN

D.P.H. Hasselman, Dept. of Materials Engineering, Virginia Polytechnic Institute and

State University, Blacksburg, Virginia 24061, USA

K. Hirao, Dept. of Industrial Chemistry, Kyoto University, Kyoto 606, JAPAN

Y. Inomata, National Institute for Research in Inorganic Materials, Tsukuba 305, JAPAN

M.G. Jenkins, Oak Ridge National Laboratory, Oak Ridge, Tennessee 37831-6064, USA

Y. Kagawa, Institute of Industrial Science, The University of Tokyo, Minato-ku 106, JAPAN

M. Kaji, Central Research Lab., Kyocera Corporation, Kokubu 899-43, JAPAN

T. Kishi, Research Centre for Advanced Science and Technology, The University of Tokyo
Megro-ku 153, JAPAN

Y-W. Mai, Center fo Advanced Materials Technology, University of Sydney

Sydney, N.S.W. 2006, AUSTRALIA

M. Matsui, Analysis and Properties Research Lab., NGK Insulators, Ltd., Nagoya 467
JAPAN

Y. Matsuo, Dept. of Inorganic Materials and Engineering, Tokyo Institute of Technology

Tokyo 152, JAPAN

N. Miyata, Dept. of Industrial Chemistry, Facal. of Engineering, Kyoto University

Sakyo-ku 606, JAPAN

D. Munz, Institut fiir Materialforschung II, Kernforschungszentrum Karlsruhe

75 Karlsruhe 1, GERMANY

K. Niihara, The Institute of Scientific and Industrial Research, Osaka University

Ibaraki 567, JAPAN

590
T. Nishida, Dept. of Chemistry and Materials Technology, Kyoto Institute of Technology
Sakyo-ku 606, JAPAN

J.E. Ritter, Dept. of Mechanical Engineering, University of Masachusetts

Amherst, MA 01003, USA

J.A. Salem, NASA Lewis Research Center, Cleveland, Ohio 44135, USA

V.Ya. Shevchenko, High-Tech Ceramics Research Center, Academy of Science of The USSR
Ozernaya 48, Moscow 119361, USSR

R.W. Steinbrech, Institute for Reactor Materials, Research Center Jiilich

5170 Jiilich, GERMANY

M.V. Swain, Dept. of Mechanical Engineering, University of Sydney

N.S.W., Sydney 2006, AUSTRALIA

Y. Tajima, R&D Center, NGK Spark Plug Co., Ltd., Komaki 485, JAPAN

K.W. White, Dept. of Mechanical Engineering, University of Houston

Houston, TX 77204-4792, USA

D.S. Wilkinson, Dept. of Materials Science and Engineering, McMaster University

Hamilton, Ontario L8S 4L7, CANADA

591
Authors

W.F. Adler, General Research Corporation, Santa Barbara, CA 93111, USA

K. Ahlborn, Central Research and Deveropment, Carl Freudenberg, 6940 Weinheim

GERMANY

S. Akada, Asahi Glass Co., Ltd., JAPAN

T. Akiba, Central Engineering Lab., Nissan Motor Co. Ltd., Yokosuka 237, JAPAN

Y. Akimune, Central Engineering Lab., Nissan Motor Co. Ltd., Yokosuka 237, JAPAN

H. Awaji, Japan Fine Ceramics Centre, Nagoya 456, JAPAN

S. Baik, Dept. of Materials Science and Engineering, Pohang Institute of Science

and Technology Pohang 790-600, KOREA

S.M. Barinov, High-Tech Ceramics Scientific Research Center, Academy of

Science of The USSR, Ozernaya 48, Moscow 119361, USSR

R.C. Bradt, Mackay School of Mines, University of Nevada-Reno, Reno, Nevada

89557-0047, USA

J.H.A. Bressers, Institute for Advanced Materials, Joint Research Center - CEC
1755 ZG Petten, THE NETHERLANDS

C.Y. Cha, Philips Display Components Company, Ann Arbor, MI 48106-0963, USA

D. Chakraborty, Central Glass and Ceramic Research Institute, Calcutta 700032

INDIA

S. Chandrasekar, School of Industrial Engineering, Purdue University

West Lafayette, IN 47907, USA

Y.M. Chen, School of Industrial Engineering, Purdue University, West Lafayette

IN 47907, USA

J-L. Chermant, Laboratoire D'etudes et de Recherches Sur les Materiaux, LERMAT

URA CNRS 1317, ISMRa, 14050 CAEN Cedex, FRANCE

S.R. Choi, Cleveland State University, Cleveland, Ohio 44115, USA

T-J. Chuang, Ceramics Division, National Institute of Standards and Technology

Gaithersburg, MD 20899, USA

593
A. Chulya, Cleveland state University, Cleveland, Ohio 44115, USA

B. Cotterell, Center for Advanced Materials Technology, University of Sydney

Sydney, N.S.W. 2006, AUSTRALIA

S.K. Datta, Central Glass and Ceramic Research Institute, Calcutta 700032, INDIA

J.T. Dickinson, Dept. of Physics, Washington State University, Pullman

WA 99164-2814, USA

K.Y. Donaldson, Dept. of Materials Engineering, Virginia Polytechnic Institute

and State University, Blacksburg, Virginia 24061, USA

K. Duan, Center for Advanced Materials Technology, University of Sydney, Sydney

N.S.W. 2006, AUSTRALIA

S.N. Dub, Institute for Superhard Materials of The Ukrainian Academy of Science
2 Avtozavodskaya St., 254153 Kiev, USSR

M. Elices, Dept. of Materials Science, Polytechnic University of Madrid

28040- Madrid, SPAIN

G. Fantozzi, INSA, GEMPPM, U.A. 341, Lyon, FRANCE

T.N. Farris, School of Aeronautics and Astronautics, Purdue University

West Lafayette, IN 47907, USA

M.K. Ferber, Oak Ridge National Laboratory, Oak Ridge, Tennessee 37831-6064, USA

T. Fett, Institut fiir Materialforschung II, Kernforschungszentrum Karlsruhe

75 Karlsruhe 1, GERMANY

P. Fourvel, SEP, VERNON 2700, FRANCE

S. Fukui, Faculty of Mechanical Engineering, Technical college of Takamatsu

Takamatsu 761 JAPAN

K. Funatani, Japan Fine Ceramics Centre, Nagoya 456, JAPAN

Y. Furuse, Engineering Research Center, Tokyo Electric Power Co., Inc.

Chofu 182, JAPAN

Y-C. Gao, Center fo Advanced Materials Technology, University of Sydney

Sydney, N.S.W. 2006, AUSTRALIA

A. Ghosh, Philips Display Components Company, Ann Arbor, MI 48106-0963, USA

M. Gomina, Laboratoire D'etudes et de Recherches Sur les Materiaux, LERMAT

URA CNRS 1317, ISMRa, 14050 CAEN Cedex, FRANCE
J.H. Gong, Dept. of Materials Science and Engineering, Tsinghua University
Beijing 100084, CHIN A

594
Z.D. Guan, Dept. of Materials Science and Engineering, Tsinghua University
Beijing 100084, CHINA

1. Guazzone, Dept. of Mechanical Engineering, University of Houston

Houston, TX 77204-4792, USA

D.P.H. Hasselman, Dept. of Materials Engineering, Virginia Polytechnic Institute

and State University, Blacksburg, Virginia 24061, USA

H. Hatta, The Institute of Space and Astrnautical Science, Sagamihara 229, JAPAN

A. Hattori, Dept. of Materials Science and Engineering, Nagoya Institute of

Technology, Nagoya 466, JAPAN

J.C. Hay, Dept. of Mechanical Engineering, University of Houston

Houston, TX 77204-4792, USA

S. Hayashi, Structure and Strength Dept., Research Institute, Ishikawajima-Harima

Heavy Industries Co., Ltd., Koto-ku 135, JAPAN

K. Hirao, Dept. of Industrial Chemistry, Kyoto University, Kyoto 606, JAPAN

W.S. Hong, Institute for Defense Analyses, Alexandria, Virginia 22311-1772, USA

X. Hu, Center for Advanced Materials Technology, University of Sydney

Sydney, N.S.W. 2006, AUSTRALIA

Y. Ikuhara, Japan Fine Ceramics Centre, Nagoya 456, JAPAN

S. Ito, Government Industrial Research Institute- Nagoya, Nagoya 462, JAPAN

A.D. Izotov, Kurnakov Institute of General and Inorganic Chemistry, Academy of

Science of The USSR, 117907, GSP-l Moscow B-71, Leninsky Pr.31, USSR

M.G. Jenkins, Oak Ridge National Laboratory, Oak Ridge, Tennessee 37831-6064
USA

L.C. Jensen, Dept. of Physics, W.ashington State University, Pullman

WA 99164-2814, USA

D.C. Jiang, Dept. of Materials Science and Engineering, Tsinghua University

Beijing 100084, CHINA

H. Jinno, Dept. of Chemistry, Sophia University, Tokyo, JAPAN

Y. Kagawa, Institute of Industrial Science, The University of Tokyo

Minato-ku 106, JAPAN

M. Kaji, Central Research Lab., Kyocera Corporation, kokubu 899-43, JAPAN

I. Kameyama, Dept. of Chemistry and Materials Technology, Kyoto Institute of

Technology, Sakyo-ku 606, JAPAN

A. Kamiya, Government Industrial Research Institute- Nagoya, Nagoya 462, JAPAN

595
N. Kamiya, Toyota CRDL, Aichi-Gun 480-11, JAPAN

W. Kanematsu, Government Industrial Research Institute- Nagoya, Nagoya 462, JAPAN

K. Kawaguchi, Research and Development Division, Sumitomo Metal Industries, Ltd.

Amagasaki 660, JAPAN

H. Kawamoto, Higashifuji Technical Center, Toyota Motor Corp., Susono 410-11

JAPAN

D. Kervades, Laboratoire D'etudes et de Recherches Sur les Materiaux

LERMAT, URA CNRS 1317, ISMRa, 14050 CAEN Cedex, FRANCE

S. Kimura, Dept. of Inorganic Materials, Tokyo Institute of Technology

Megro-ku 152, JAPAN

M. Kinoshita, Government Industrial Research Institute- Osaka, Osaka 563, JAPAN

T. Kishi, Research Centre for Advanced Science and Technology, The University of
Tokyo, Megro-ku 153, JAPAN

H. Kishimoto, Dept. of Mechanical System Engineering, Toyota Technological

Institute, Nagoya 468, JAPAN

K. Kitakami, Canon Research Center, Atsugi, JAPAN

H.N. Ko, Nakanihon Automotive College, Kamo-gun, Gifu 505, JAPAN

A.S. Kobayashi, Dept. of Mechanical Engineering, University of Washington

Seattle, Washington 98195, USA

T. Kobayashi, Dept. of Production Systems Engineering, Toyohashi University of

Technology, Toyohashi 441, JAPAN

Y. Kodama, Government Industorial Research Institute- Nagoya, Nagoya 462, JAPAN

Y. Kogo, Materials and Electric device Laboratory, Mitsubishi Electric

Corporation, Sagamihara 229, JAPAN

N. Kohler, Fachhochschule Rhineland-Pfalz, Koblenz, GERMANY

A. Kokaji, Central Research Lab., Kyocera Corporation, kokubu 899-43, JAPAN

K. Kubo, Government Industrial Research Institute- Nagoya, Nagoya 462, JAPAN

S.C. Langford, Dept. of Physics, Washington State University, Pullman

WA 99164-2814, USA

V.B. Lazarev, Kurnakov Institute of General and Inorganic Chemistry, Academy of

Science of The USSR, 117907, GSP-1 Moscow B-71, Leninsky Pr.31, USSR

S.M. Lee, Dept. of Materials Science and Engineering, Pohang Institute of

Science and Technology, Pohang 790-600, KOREA

596
J. Llorca, Dept. of Materials Science, Polytechnic University of Madrid
28040 - Madrid, SPAIN

E.H. Lutz, Kelterbergstr. 15, W-7562 Gems Bach, GERMANY

Y-W. Mai, Center fo Advanced Materials Technology, University of Sydney

Sydney, N.S.W. 2006, AUSTRALIA

A.L. Maistrenko, Institute for Superhard Materials of The Ukrainian, Academy of

Sciencec ,2 Avtozavodskaya St., 254153 Kiev, USSR

H. Makino, Toyota CRDL, Aichi-Gun 480-11, JAPAN

T. Makino, NGK Insulators, Ltd., Nagoya 467, JAPAN

C.S. Martins, Institute for Advanced Materials, Joint Research Center - CEC
1755 ZG Petten, THE NETHERLANDS

M. Masuda, Analysis and Properties Research Lab., NGK Insulators, Ltd.

Nagoya 467, JAPAN

M. Matsui, Analysis and Properties Research Lab., NGK Insulators, Ltd.

Nagoya 467, JAPAN

R.L.K. Matsumoto, Hercules Research Center, Hercules Incorpolated

Wilmington, DE 19894-0001, USA

Y. Matsuo, Dept. of Inorganic Materials and Engineering, Tokyo Institute of

Technology, Tokyo 152, JAPAN

J. Matsuoka, Dept. of Chemistry for Materials, Mie University, Tsu 514, JAPAN

D.J. Mihora, General Research Corporation, Santa Barbara, CA 93111, USA

B.S. Min, Samsung Electrics Suwon, KOREA

N. Miyahara, Dept. of Mechanical Engineering, Nagaoka University of Technology

Nagaoka 940-21, JAPAN

T. Miyajima, Government Industorial Research Institute- Nagoya, Nagoya 462, JAPAN

N. Miyata, Dept. of Industrial Chemistry, Facal. of Engineering, Kyoto University

Sakyo-ku 606, JAPAN

A.K. Mukhopadhyay, Dept. of Mechanical Engineering, University of Sydney

Sydney, N.S.W. 2006, AUSTRALIA

D. Munz, Institut fiir Materialforschung II, Kernforschungszentrum Karlsruhe

75 Karlsruhe 1, GERMANY

N. Murayama, Government Industorial Research Institute- Nagoya, Nagoya 462, JAPAN

Y. Mutoh, Dept. of Mechanical Engineering, Nagaoka University of Technology

Nagaoka 940-21, JAPAN

597
S. Nakahara, Dept. of Mechanical Engineering, Kansai University, Suita 564, JAPAN

A. Nakahira, The Institute of Scientific and Industrial Research, Osaka University

Ibaraki 567, JAPAN

K. Nakano, Government Industrial Research Institute- Nagoya, Nagoya 462, JAPAN

Y. Nakasuji, Analysis and Properties Research Lab., NGK Insulators, Ltd.

Nagoya 467, JAPAN

H. Nakayama, Faculty of Junior College of Automobile Industory

Osaka Sangyo University, Daito 574, JAPAN

K. Niihara, The Institute of Scientific and Industrial Research, Osaka University

Ibaraki 567, JAPAN

T. Nishida, Dept. of Chemistry and Materials Technology, Kyoto Institute of

Technology, Sakyo-ku 606, JAPAN

T. Nishikawa, Dept. of Materials Science and Engineering, Nagoya Institute of

Technology, Nagoya 466, JAPAN

H. Nishimura, Dept. of Mechanical Engineering, Tokyo Metropolitan University

Hachioji 192-03, JAPAN

R. Nowak, Government Industrial Research Institute- Osaka, Osaka 563, JAPAN

T. Ogasawara, Central Engineering Lab., Nissan Motor Co., Ltd., Yokosuka 237
JAPAN

T. Ogawa, Dept. of Mechanical Engineering, Gifu University, Gifu 501-11, JAPAN

T. Ohji, Government Industrial Research Institute- Nagoya, Nagoya 462, JAPAN

T. Oikawa, Advanced Technology Research Center, NKK Corporation, Kawasaki 210

JAPAN

N. Okabe, Heavy Apparatus Engng. Lab., Toshiba Corporation, Kanagawa 230, JAPAN

A. Okada, Central Engineering Lab., Nissan Motor Co., Ltd., Yokosuka 237, JAPAN

T. Okada, ISIR, Osaka University, Ibaraki 567, JAPAN

A. Okura, lIS, The University of Tokyo, Tokyo 108, JAPAN

C. Olagnon, INSA, GEMPPM, U.A. 341, Lyon, FRANCE

H. Omura, Matsushita Electric Industrial Co., Ltd., JAPAN

S. Owaki, ISIR, Osaka University, Ibaraki 567, JAPAN

F. Pernot, Laboratoire de Science des Materiaux Vitreux- CNRS, URA, USTL.

Place E. Bataillon 34095 Montpellier Cedex 05, FRANCE

598
J. Peussa, Federation of Finnish Metal, Engineering and Electro-Technical
Industries, SF00130, Helsinki, FINLAND

G. Pezzotti, The Institute of Scientific and Industrial Research, Osaka University

Ibaraki 567, J APAN

J. Phalippou, Laboratoire de Science des Materiaux Vitreux- CNRS, URA, USTL.

Place E. Bataillon, 34095 Montpellier Cedex 05, FRANCE

J.W. Pier, Hercules Research Center, Wilmington, DE 19894, USA

M.A. Rigdon, Institute for Defense Analyses, Alexandria, Virginia 22311-1772, USA

J.E. Ritter, Dept. of Mechanical Engineering, University of Masachusetts

Amherst, MA 01003, USA

L.G. Rosa, Institute Superior Tecnico, Lisbon, PORTUGAL

M-H. Rouillon, , Laboratoire D'etudes et de Recherches Sur les Materiaux

LERMAT, URA CNRS 1317, ISMRa, 14050 CAEN Cedex, FRANCE

M. Saadaoui, Ecole Mohammadia D'ingenieurs, Rabat, MAROCCO

S. Sakaguchi, Government Industorial Research Institute- Nagoya, Nagoya 462, JAPAN

M. Sakai, Dept. of Materials Science, Toyohashi University of Technology

Toyohashi 441, JAPAN

T. Sakai, Faculty of Science and Engineering, Ritsumeikan University

Kita-ku 603, JAPAN

J.A. Salem, NASA Lewis Research Center, Cleveland, Ohio 44135, USA

J.M. Sater, Institute for Defense Analyses, Alexandria, Virginia 22311-1772, USA

R.A. Schultz, Mackay School of Mines, University of Nevada-Reno

Reno, Nevada 89557-0047, USA

K. Sekine, Institute of Industrial Science, The University of Tokyo

Minato-ku 106, JAPAN

V.Ya. Shevchenko, High-Tech Ceramics Research Center, Academy of Science of The USSR
Ozernaya 48, Moscow 119361, USSR

G. Sines, Dept. of Materials Science and Engineering, University of California

Los Angeles, CA 90024, USA

N. Soga, Dept. of Industrial Chemistry, Kyoto University, Kyoto 606, JAPAN

M. Steen, Institute for Advanced Materials, Joint Research Center - CEC

1755 ZG Petten, THE NETHERLANDS

R.W. Steinbrech, Institute for Reactor Materials, Research Center Jiilich

5170 Jiilich, GERMANY

599
K. Sugihara, Dept. of Mechanical Engineering, Kansai University, Suita 564, JAPAN

A. Suzuki, Structure and Strength Dept., Research Institute, Ishikawajima-Harima Heavy

Industries Co., Ltd., Kotoku 135, JAPAN

K. Suzuki, Faculty of Education, Niigata University, Niigata 950-21, JAPAN

M.V. Swain, Dept. of Mechanical Engineering, University of Sydney

N.S.W., Sydney 2006, AUSTRALIA

Y. Tajima, R&D Center, NGK Spark Plug Co., Ltd., Komaki 485, JAPAN

Y. Takagi, Advanced Technology Research Center, NKK Corporation, Kawasaki 210

JAPAN

J. Takahashi, Dept. of Materials Science and Engineering, Nagoya Institute of Technology

Nagoya 466, JAPAN

M. Takatsu, Dept. of Materials Science and Engineering, Nagoya Institute of Technology

Nagoya 466, JAPAN

N. Takeda, Research Center for Advanced Science and Technology, The University of Tokyo
Meguro-ku 153, JAPAN

S. Takeda, Dept. of Applied Chemistry, Okayama University, Okayama 700, JAPAN

H. Tanaka, Dept. of Mechanical Engineering, Nagoya University, Nagoya 464-01, JAPAN

I. Tanaka, The Institute of Scientific and Industrial Research, Osaka University

Ibaraki 567, JAPAN

K. Tanaka, Dept. of Mechanical Engineering, Nagoya University, Nagoya 464-01, JAPAN

T. Tanaka, Faculty of Science and Engineering, Ritsumeikan University, Kyoto 603, JAPAN

I. Tari, Dept. of Applied Chemistry, Okayama University, Okayama 700, JAPAN

H. Tsuruta, Engineering Research Center, Tokyo Electric Power Company, Chofu 182
JAPAN

H. Tsuruta, Analysis and Properties Research Lab., NGK Insulators, Ltd., Nagoya 467
JAPAN

H. Uchimura, Central Research Lab., Kyocera Corporation, kokubu 899-43, JAPAN

A. Ueno, Dept. of Mechanical System Engineering, Toyota Technological Institute

Nagoya 468, JAPAN

K. Ueno, Government Industrial Research Institute- Osaka, Osaka 563, JAPAN

K. Urashima, R&D Center, NGK Spark Plug Co., Ltd., Komaki 485, JAPAN

S. Vaidyanathan, Philips Display Components Company, Ann Arbor, MI 48106-0963, USA

600
A. Venkateswaran, Dept. of Materials Engineering, Virginia Polytechnic Institute and
State University, Blacksburg, Virginia 24061, USA

S. Wada, Toyota CRDL, Aichi-Gun 480-11, JAPAN

F. Wakai, Government Industorial Research Institute- Nagoya, Nagoya 462, JAPAN

S. Wakayama, Dept. of Mechanical Engineering, Tokyo Metropolitan University

Hachioji 192-03, JAPAN

M. Watanabe, R&D Center, NGK Spark Plug Co., Ltd., Komaki 485, JAPAN

K.W. White, Dept. of Mechanical Engineering, University of Houston

Houston, TX 77204-4792, USA

D.S. Wilkinson, Dept. of Materials Science and Engineering, McMaster University

Hamilton, Ontario L8S 4L7, CAN ADA

T. Woignier, Laboratoire de Science des Materiaux Vitreux- CNRS, URA, USTL. Place E.
Bataillon 34095 Montpellier Cedex OS, FRANCE

N. Yamada, Analysis and Properties Research Lab., NGK Insulators, Ltd., Nagoya 467
JAPAN

Y. Yamade, Research and Development Division, Sumitomo Metal Industries, Ltd.

Amagasaki 660, JAPAN

K. Yamaishi, Dept. of Mechanical Engineering, Nagaoka University of Technology

Nagaoka 940-21, JAPAN

S. Yamamoto, Faculty of Science and Engineering, Ritsumeikan University, Kyoto 603

JAPAN

S. Yamauchi, Dept. of Production Systems Engineering, Toyohashi University of Technology

Toyohashi 441, JAPAN

Y. Yamauchi, Government Industrial Research Institute- Nagoya, Nagoya 462, JAPAN

Y-N. Yan, Tsinghua University, Beijng, CHINA

L.X. Zeng, Dept. of Materials Science and Engineering, Tsinghua University

Beijing 100084, CHINA

X.F. Zhao, Dept. of Materials Science and Engineering, Tsinghua University

Beijing 100084, CHINA

L. Zhou, Center for Advanced Materials Technology, University of Sydney

Sydney, N.S.W., 2006, AUSTRALIA

601
INDEX

Acoustic Emission, 1 da/dN-dK-Curve, 559

Alumina, 189, 219, 277, 357, 559 Domain Switching, 371
Alumina-Silicon Carbide, 165 Double Notch, 277
Ductility, 53
Bending Strength, 289 Duplex Ceramics, 319
Beta-Sialon, 543 Dynamic Finite Element Analysis, 133
Bridging Dynamic Fracture, 133
Condition, 19
Crack, 19, 29, 265 Effect of Crack Size, 423
Fiber, 69 Effective Surface, 559
Grain, 235
Stress, 387 Failure Prediction, 439
Brittle Matrix Composite, 339 Fatigue, 235, 455, 559
Acceleration, 493
Carbon Fiber, 123 Cyclic, 189, 423, 439, 465, 493, 501,
Ceramic, 209,439 507,517
Fracture, 133 Cyclic and Static, 387, 481
Charpy Impact Testing, 123 Dynamic, 465
Compliance, 219 Overload, 507
Composite Parameter, 493
Anisotropic Hybrid, 179 Static, 465, 493, 517, 535
Carbon/Carbon, 69, 83 Fiber
Ceramic, 53, 147,209,251,319 Bridging, 69
Fracture, 133 Debonding, 1
Glass Matrix, 339 Pullout, 1, 83
Nano, 165 Reinforced Ceramics, 19, 29
Silicon Carbide/Glass, 1 First Matrix Cracking, 69
Crack Fractography, 455
Bridging, 19, 29, 265 Fracture, 251, 339
Bridging Stress, 387 Energy, 83
Growth, 455, 501 Features, 517
Opening Displacement, 423 Mechanics, 209, 289
Propagation Resistance, 209 Mechanism, 147
Resistance, 357 Resistance, 1
Shielding Degradation, 387 Toughness, 69, 123, 179, 209, 277, 319,
Stabilizer, 277 339
Starting Toughness, 19 Fretting Damage, 455
Tip Stress Intensity, 439 Frictional/Frictionless Debonding, 1
Critical Defect Size, 289
Cyclic Geometry Effects, 53
Compression, 305 Grain Bridging, 235
Fatigue, 189, 423, 439, 465, 493, 501,
507,517 High Temperature
Behavior, 111, 165,481
Strength, 543

603
Hot-Hardness, 165 Rebinder Effect, 575
Reinforcement, 357
Indentation, 235, 501, 569 Reliability, 209
Strength Method, 339 Residual Stress, 569
Interfacial Rotary Bending, 517
Debonding, 29 Rupture, 111
Properties, 19
Interphase, 97 Shear-Lag Model, 29
Sialon, 123
JIS,277 Beta, 543
Silicon Carbide, 123, 251, 465, 481, 543
Laser Interferometric Gage, 133 /Silicon Carbide, 111
Lifetime, 219, 543 /Silicon Carbide Rupture, 97
in Cyclic Tests, 559 /Zirconia/Alumina, 179
Prediction, 535, 559 /Zirconia/Glass, 179
Long Cracks, 189 Silicon Nitride, 123, 235, 251, 465, 481,
501, 535, 543, 569
Magnesia, 305 Sintered, 423, 517
Partially Stabilized Zirconia, 189 Size Effect, 53
Martensitic Transformation, 179 Slow Crack Growth, 481, 507, 543
Matrix Cracking, 69 Soda-Lime Silica Glass, 575
Mechanical Properties, 165, 339 Spinel, 265
Microcrack Stable
Toughening, 339 Crack Growth, 305
- Macrocrack Behavior, 219 Fracture, 277
Microcracking, 371 Strength, 219, 251
Microfracture Bending, 289
Mechanism, 69 Degradation, 481
Process, 83 Subcritical Crack Growth, 189, 219, 569,
Microstructure, 165 575
Mirror-Like Region, 517 Surface
Monolithic, 251 Charge, 575
Monte Carlo Simulation, 289 Charge Density, 575

Nanometer-Size Second Phase, 165 Thermal

"Natural" Surface Flaws, 189 Shock, 189, 319
Non-Phase Transformable Ceramics, 387 Expansion Mismatch, 339
Toughening
Oxidation, 111 Mechanisms, 339, 371
Transformation, 507
Penny Crack, 29
Phase Transformable Ceramics, 387 V-K-Curve, 219
Piezoelectric Ceramics, 493
PSZ, 357 Weibull
PZT,371 Modulus, 251,559
Distribution, 535, 559
R-Curve "Work-of-Fracture" Technique, 83
Behavior, 19, 29, 69, 97, 147, 179, 189,
209, 235, 251, 265, 277, 305, 319, Zeta-Potential, 575
339, 357, 371, 387,439,455, 507 Zirconia Ceramics, 219, 507
Effect, 219
Method,289

604