AMMRC TR 72-9 IAD

SSTATIC AND CYCLIC FATIGUE

t, OF;CERAMIC MATERIALS

SAMU*L J. AC-QUAVIVA and RICHARD CHAIT

MATERIALS TEST ING DIVISION

March 1972

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ARMY MATERIALS AND MECHANICS RESEARCH CENTER
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 `7.T

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SM

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) tLPOAT T!8.CE

STATIC AND CYCLIC FATIGUE OF CERLAMIC K'A77ERIALS

4 `CFC%8PTkVE NOTVS (7Tj* af t~p~rt andinbCl8.sh dftst)

S,=ruel., J. AcquaviLva and Richard Chait

AS PORT CAIC 'U_ TOTAL NO0 011 P.CM3 #40or -. fez

Marc~h 1972 10
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Washington, 0. C. 20315
85 OSRACTStatic and cyclic fatigue characteristics were deterguned for two celramic

materials, aa alumina AD-941 and a hot-pressed boron carbide B.C. The static fatigue
limits det~rmined in three-point flexure were 23,530 psi for A1203 and 43,000 psi for
b.,C, while the cyclic fatigue limits deteimined by stressing a cnatilever-d beam werc
1700 psi for the A120 3 and 28,SOO p~.i for the Bi
I 4C.

Examination or fracture surfaces by scanning and transmission electron

microscopy revealed the fracture to bc )~f a transgranular and intcrgra~ular nature
for both matesijals. Fracture initiated at thc tension stwface ýGmd propagated immedl-
azely to failure. There was nc change in fractuxe appearance in either the ststic or
cyclic mode of failure. (Authors)

3ez1ity 1acuificstuon
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14 L'-1 - L..I,
d 6 LE*4K C
KtL ORO-
~OL•U? ROL, S UT 1
ROt.t T

Ceramic materials
Alumina
I
Boron c~rbide
Mechanical properties
Fatigue
Fracture toughness I
Mcicrostructure
Electron microscopy.f

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AMMRC TR 72-

STATIC AND CYCLIC FATIGUE OF CERAMIC MAT~f1dALS

Technical Report by
SAMNUEL J.ACJ21A
1 VI VA and RICHA RD CHAIT

March 1972

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AMICMVS 0C-oi 512E1.11.A52-X031801
Aircraft Survivability
Agency Accassion Number DA 0C4808

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MATERIALS TESTING DIVISION

ARMY MATERIALS AND MECHANICS RESEARCH CENTER
Watertown, Massachusetts 02172
. R.' Wq"-AW17
.MVTTMIVVý! TIMM.,,

A[kMY MATERIALS AND MECHANICS RESEARCH CENTER

STATIC APP GYZLIC FATIGUE OF CERAMIC MATERIALS

AB3TRACT
Static and cyclic fatigue ,-haracteriýstics were determined for two ceramic
materials, an alumina AD-94 and a hot-pressed boron carbide B4 C. The static
fatigue limits determined in three-pint flexure were 23,500 psi for A12 0 3 and
43,000 psi for B4C, while the cycii: 2atigue limits determined by stressing a
cantilevered beam were 21,700 psi fox ",h%A12 0 3 ard 28,500 psi for the B4 C.

Examination of fracture surraces by scanning and transmission electron

microscopy revealed the fracture to be of a transgranular and intezgranular
nature for both materials. Fracture initiated at the tension surface and propa-
gated immediately to failure. There was n,: change in fracture appearance in
either the static or cyclic mode of failure.
 INTRODUCTION
There is increased emphasis on the structural use of armor material as evi-
1 2
denced, for example, by the proposed Aerial Armored Reconnaissance Vehicle. ,
This vehicle utilizes monocoque construction with steel armor plate serving as
both the skin and primary structure. It is also possible that ceramic composite
armor, i.e., ceramic facing bonded to a suitable backup material may be considered
for a nonprimary but critical application, especially under severe ballistic
environment. However, add.iticnal information is needed regarding the behavior
of candidate materials that will serve in both a load-carrying and ballistic
protection capacity. A program is underway with the objective of characterizing
candidate materials. The present study covers aan initial phase of this charac-
terization of ceramic composite armor by focusing on the static and cyclic fatigue
response of two candidate ceramic materials, A12 0 3 and B4 C.

MATERIALS AND TEST PROCEDURES

Two materials were selected for investigation; (1) AD-94, a commercially

available alumina A12 0 3 , manufactured by Coors Porcelain Company, Golden, Colorado;
and (2) a hot-pressed boron carbide B4C, manufactured by the Norton Company,
Worcester, Massachusetts. -themicrostructures of these mmterials are shown 4n
Figure 1, and their properties are given in the. following table:
Table I. Physical Pr3perties
Material Flexural Strength Modulus Density !Grain Size
A1 2 0 3 38,000 psi 41.5 x 106 psi 3.71 g/cc IOU
B4C 51,000 psi_ 60 x 106 psi 2.43 g/cc 10uj

.9 41.le Ib.

9,A

a. Alumin3 94% b. Boron Carbide

Figure 1. PHOTOMICROGRAPHS OF MATFRIALS T.STED. Mdg. 50OX

 The static fatigue tests "-tre conducted in three-point bending with a dead-
weight load suspended from the center of the specimen. Tha specinen size for
both the static and cyclic fatigue tests w.as 1/4" x 1/4" x 3Y with a surface
finish of lo tis.

For purposes of this study, cyclic fatigue has been defined as an inter-
mittently applied load to a specimen such that the stress on the surface of the
specimen follows a sinusoldal excursion varying from zero to a Maxim,= tensile
or compressive stress, depending on the applied load. The dynamic test consiszed
of applying a load at the end of a cantilevered specimen. at the rate
3
of 15 cps.
The equipment utilized in this test has been describcd elsewhere.

The arbitrary cut-off limit for the cyclic test was 1 0 cycles in r1.e
event failure did not occur. Several tests beyond this arbitrary lildit were
conducted; these tests indicated that a limit of 1 x 106 cycles was justified.

RESULTS AND DISCUSSION

The flexural strength of the A12 0 3 w-.en )oaded to failure, was 38,000 psi;
th'.s will be referred to as the reference strength, Figure 2. At 7S% of th•
reference strength life was limited to !0 seconds. Decreasing the stress level
to 70% or 27,000 psi increased the static fatigue life to 13-1/2 hours. At 60_
of the reference strength or 23,000 psi, life was extended to 72 hours, at which
time the test has terminated, it being assumed that life would be infznite at
this stress level. The specimens that were not fractured in the static tests
were rtloaded to failure, with failure occuiring at 35,000 psi or Within 6 or 714
of the reference strength, indicating
that virtually no damage was incurred
5O within the test specimen during the stati.
•61 min B4test. It would thus appear that this
-material can be loaded statically at 60%
were
of the reference levei for onan BnC
indefinite
fatigue tests
40- period of time.

mStatic
X
4
conducted undei the same atmospheric con-
a. ditions as for the A1 2 0 3 , namely 72 F
30 10 sec and 35% R.H. The reference strength of
_13% hr the B4C was determined to be 51,000 psi.
94AD._ At 90% of this value or 46,000 psi, frac-
ture occurred after 61 minutes; at 75%
X ~and 73% of the refe--ence strength, static
fatigue life exceeded the arbitrary limit
of 72 hours. The specimens that did not
fracture in the static tests were re-
20 60 ell loaded, and in each case fracture oc-
Life - hours curved at 97% of the reference strength,
Figure 2. STATIC FATIGUE OF CERAMIC indicating once again that static fatigue
MATERIALS had no detriuentai effect on t.,_ z_,ength
of the material.
A.V

One of the more predaominant mech~anisms leading to frac-ture is stres;s corro-

sion,* and it is felt fur'ther tests at humidities az~proaching 100%'1 and also tests
conducted in a vacuum would el*;cidate the rGle of stress corrosion in fatigue.
Also, additional tests to de~e;`:iteiv establish the observed trend are planned.

Several techniques hav- been reported for increasing the strengti. o~ ceramic
materials. Semple-,' for example, introduce4 a compressive .tress on the surface
rf Al2 O pcmn yaha treat process, and subsequent leading of the heat-
treated specimens showed an iscreasle in strength over the tuti eated specimens.
Kirenner ez al.,- recognizing that tailures occur at surface Iflaws, treated the
surfaces by refirin~g, cheaic-4 and flame polishing, cheatical etching, and glaz~ng
These treazr.ents also proved to be beneficial in increasing the strength of th.-
treated material. The effect that these treatm'ents might have on improving the
fatigue: life of the A12 0-. and B4 C should also be investigated.

The results obtained for the cyclic 'testing of the A4120 3 and B,.C are shown
in Figure 3. The reference strengths for each material are the same as in the
stati-c tests. The threshol1d level is defined as that level of stress below which
an infinite fatigue2 life is anticipated. The threshold level for both the AlOw:
and R1.C in cyclic. fatigue was determin2d to be at 5`0 of thc reference stren-gth
for each material. The- data for A1201 compares favorably with that reported by
Williams6 where he reports a "cyclic endurance limit of 0.56 of the single stroke

Scanning electron microscopy (SEM%) of the f;.-acture surface, Figure 4, indi-

cates fracture is of both a tranisgranular anti i'ttergraniular nature. The location
of the area shown in the micrograph is approximai.ely at the center of the frac-
ture surface. Transmixsion electron microscory of the fracture surface of Al-O-.,

50k

-' 0

&.gre.3FLXUALFAIGU CRAICMA&RA4
Q Cycles

xOsuso
3ih0 .tos iws Rsdc ntttKna Cit.Mssui

O_ractur
No
 44

c Al~20M310
A. 1;OO d B C Mttj 1525X

F:Spre 4. FRACTURRE SURFACES BY SEM

19-066&I4511A.MC.71

Figure 5 indicates th-' the tran!.g:anular fracture involves cleavage. It Wotild

also appe~ar tla,,t the.- are some c~cý,vaesessoni h E irgah~
BL.C, Figpre 4. e-_-sessonIth Emirgahf
Itho
Fracture mechaznics concepts, based upon the Griffith criterion, w-ere u!!ed
to determine ;5train energy release rate andJ ceitical flaw size for the twc% mate-
rials. The strain energy release rate was determined by fracturing a V-rnotche6
specimen, 1/14"x 1/411 2-1/2", having a notch dzpth of O.OSG inch. The speci-
mens were fractured in three-point bending as outlined by iDavidgr- and Tappin'
who defilned the strain energy release rate G by

4.4
 Figure 5. FRACTURE SURFACE OF A120 3
BY TEM (CARBON REPLICA) MAag. 15,000X

4 G (-2).
-= Gr2c 1
2E
where . is Poisson's ratio; r is Young's modulus in pounds per square inch; VF
is the fracture stress in pounds per square inch; and c is the notch depth in
inches.

Notchoc specimens of both Al.03 and BtC were fractured in an Instron test-
ing machine at a crosshLad speed of 0.020 inch per minute Substituting the test
data into Equation 1, the strain energy release rate for A12 0I was 0.270 in-lb/
sq in. (4.73 - 10' erg/cm2) and for the B4C, 0.192 in-lb/sq in. (3.36 v 104 ergs/
m2). For the A12 0 3 , the strain energy release rate compares favorably with
0.302 in-lb/sq in. reported by McKinney.ý Care should be exercised in comparing
fracture energy data, since Gross and Gutshal!9 found that the strain energy re-
lease rate was grain-sFze dependent.

From the Griffith criterion

Gc = G2 ',a/E. (2)

Solving Eqtuation 2 for a, a = (GcE)/_o 2 . If a is assumed to be the fracture

stress of -n unnotched bar, then it is possible to estimate the critical flaw
size from Equatioa 2. From the test data, it was found that the critical flaw
size for A1203 was 0.003 inch, approximately 7Sum or about 8 grain diainetern;
flaws of this size should be readily detected by nondestructive techniques. The
critical flaw size for B4 C was found to be 0.0015 in.•, approximately 4 0-im, or
about 4 grain diameters. It should be pointed out that flaws of this nature
were not ob.erved in the examination of the fracture surfaces by scanning elec-
tron microscopy. Additiono' tests are planned in the area of f-acture energy
measurements.

4' 5
 SUMMARY

The static and cyclic fatigue properties of 01o materials, an alumina AD-94
and a hot-pressed boron carbide B4 C, have been studied. The static fatigue
st-rength of the A12 0 3 at 72 hours was 60% of the reference strength, and for the
B4C the static fatigue for 72 hours was 74% of the reference strength. Static
fatigue was determined by applying a dead-weight load to the center of a specimei.
of 1/4-" - I/41 x 3" dimensions; the specimen was supported at a span length of
2-1/2 inchess.

The cyclic fatigue properties were determined by applying a load to the ead
of a cantilevered sj~cimen. The specimen size correspondtd to that used for
static fatigue, with the cantilevered span being 2-1/2 inches; this ensured the
stressed volume being the same for both the static and cyclic fatigue testz.
The threshold level for safe cyclic fatigue contitions for both A12 0 3 and B4C
appears to be at 57% of the reference strength level. Examination of the frac-
ture surface revealed the fracture to be of a transgranu-ar and intergranular
nature, with the fracture initiating at the tension surface; ho;evex, no evidencc
was present of intermittent progressive crack propagation. This latter observa-
tien would indicate that once the crack was initiated, propagation was
instantaneous.

From fraciutie mechanics concepts it wa.• calculated thac the scrain energy
release rate was 0.270 in-lb/so in. for A12 0 3 and 0.192 in-lb/sq in. ior BLC,
and the criti.:al flaw size was datermined to be 75.rn for A1203 and 40,. iLor BLC.

-5
46

34°
 LITERATURE CITED

1. AAF7b, ior!: AiArcrqft,, Vert-iflight, v. 16, December 19710,

2. WONG, A. K.,* und BERMAN, 1. iqih z~cA--r-r-r - A P?_vie-w. As-my

Materi-Als aad Machanilcs Research Center, A~M-RC HS 7141, April 19711.

3. ACQUAVIVA, S. J. 2 ._'!etkxd jfor Fc-igue T-iing Mazr.~Yteri~als. Review

Of S-ientific instiumnents. rncember 1971.

4. SENPIZ, C. W. S.'-es
_1 Deter i'nation ir' A!-a'P;A Bodes. -k.4ay Matz.-
riais and Mechan~ics R#'-search Center. AukthRC TR 70-1 ., Augt~ist 190.

S. KiRCr-LiR, H. P. , CRUVER, R. M.*, and WALKZER, it. E. :.eqhEffect es .-

irng fron: urfcre T-eaz=en-t. PrTesented at Symposiur, on -the Science
2it
of Ceramic Machining and Surfacc Finishing, X-ES, Novembher 2-4, 197i). To
be prublished.

6. WILLIAM.S, L. S. Ftique zn-e-rr-ic in ~e~e f EngirseeI_ý-

o4cnc
C i~s. W. tt'orth Kriegel. and Hayne Pialniour '11, ed., Interscience
ing
P Aicatiop, New "ork - London. 1960, p. 245-A02.

7. DAVIDGE; R. W., adm -&AP!KN, G. .:fe.,tive Furface Energy o' By-,ttle

Zh
.MJa-ezia1e. Journal :uf MuzeTial Scictnce~v. 3, 196~.3 0'. 165-173.

XcKZINNEY. K. R. :'ractlure 7cug~vnez o--' ercr.:c Mateu-ials *Ysing the .5igzau-

i-j~-Nac 3rs caimen. NRL Mz mrarsiuu Report. 1931, September 1968.

n ROS5, G,. F-., and QrSAL P. 1. .'a~.E ,.ikr-nj Measuent in5;-cia

Ceyn;-cj crd Dlesian. S. J. Acquaviva al~d S. A. iortz, ech, Gord:r. and
Breach, New York, 1969. p. 149-163.