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Fracture Toughness With Various Methods
Fracture Toughness With Various Methods
The mode I fracture toughness ( K J of boron carbide (B,C) length within the guidelines of JIS R 1607.'.5.xIn the present
and titanium diboride (TiB,) was determined using four study, the standardized test procedures for the SEPB method
competing techniques. The indentation strength (IS), chev- were used to obtain K,, data for the two materials. The SEPB
ron notched beam (CNB), and indentation fracture (IF) results were then used as a basis to compare the other toughness
methods are common techniques that were compared to the techniques. Difficulties in producing and measuring SEPB pre-
recently standardized single-edge precrack beam (SEPB) cracks were encountered, and these problems will be addressed
method. The SEPB method was more difficult to apply, but in this paper.
it represents the most rigorous method for K,, determina- The indentation strength (IS): the indentation fracture (IF):
tion, because it uses few assumptions and requires a direct and the chevron notched beam (CNB)49 methods are three
measurement of crack length. The IS method was an alternate techniques commonly used to determine the K,, of
expeditious and economical alternative when low indenta- ceramic materials. Each of these methods uses assumptions
tion loads were used. CNB K,, values were virtually rate- which simplify the determination of K , L .The range of testing
independent when displacement rates less than or equal conditions within which these assumptions are valid are often
to 0.5 mm/min were used. The IF method was the least not well documented.
The IS method uses an empirically derived constant to esti-
satisfactory technique, because of high variability in K ,
mate the shape and size of an indentation-initiated crack at the
values and because of the low differentiation between the point where spontaneous failure occurs. This constant depends
two materials studied. on the residual surface stresses resulting from the indentation.
A major advantage of the IS method is that crack length mea-
I. Introduction surements are not necessary. However, IS K,, values have been
observed to depend on the indentation load used to initiate
DEALLY, mode I fracture toughness (KIC)is an inherent mate-
I rial property which characterizes resistance to propagating a
sharp crack through a material by tensile opening. K,, is an
cracking.' In this paper, the indentation load was also varied
to determine its effect on the IS K,, for the two materials
under study.
important selection criterion for brittle materials (e.g., ceram- In the CNB K,, method, a transition from stable to unstable
ics) used in engineering applications. Values of fracture tough- crack growth is assumed to occur at a particular crack length
ness obtained using different techniques can vary greatly, which should be dependent only on the specimen and the chev-
because of difficulties involved in creating and accurately mea- ron notch geometry. As with the IS technique, the CNB method
suring cracks and because assumptions used in the analysis of a is advantageous because crack lengths do not need to be mea-
particular method may not be valid for all testing conditions. In sured to determine K,, . However, difficulties in initiating stable
addition, some techniques produce a large scatter of values crack growth during CNB testing have been observed." Dis-
which limits the ability to measure subtle differences between placement rate was chosen as the most important variable for
similar materials. In spite of these difficulties, there is currently this technique, since it likely influences stable cracking and the
no recognized or recommended United States standard for presumably invariant transition point to unstable crack growth.
determining the fracture toughness of ceramics, although exten- In the case of the IF method, the cracks propagating from the
sive prestandardization work has been performed.'4 comers of a surface indent are assumed to be directly related to
One important candidate for standardization is the single- the fracture toughness of the material. Analytical and empirical
edge precracked beam (SEPB) method, which was adopted in studies have produced general equations and calibration con-
1990 as a Japanese industrial standard for fine ceramics (JIS R stants for K , which are supposed to be indentation load and
1607).' The SEPB method is considered a rigorous method material independent (where K , is defined as an approximation
because it utilizes a long, sharp, through-width precrack which of K,, for IF method).' The major advantages of the IF method
is directly measured in each test. The mechanics of this simple are that it can be performed on very small amounts of material
crack geometry have been well modeled and are used in ASTM- and it does not require mechanical testing beyond the indenta-
E399-Annex 3 for fracture toughness testing of metals in a tion test. However, K , determination is complicated by the
single-edge fatigue-cracked beam configuration.' diversity of IF K , equations reported in the literature" and the
Previous work has shown that for typical ceramic materials high degree of subjectivity involved in accurately measuring
the SEPB K,, method is insensitive to loading rate and precrack relatively short crack lengths. Variation in IF K , values with
indentation load has been documented and attributed to the
ambiguity involved in measuring surface crack lengths.' There-
J. J. Petrovic-contributing editor
fore, indentation load was also chosen as a variable in this
study.
Manuscript No. 193334. Received August 8, 1994 approved March 11,1995. 11. Materials
'Member, American Ceramic Society.
+AlfredUniversity. Titanium diboride (TiB,) and boron carbide (B,C) were cho-
'Los Alamos National Laboratom. sen as polycrystalline, armor-grade ceramics with relatively
2187
2188 Journal of the American Ceramic Society-Conzone et al. Vol. 78, No. 8
-
/Region
were precision machined into beams with dimensions of Notch
3 mm X 4 mm X 22.5 mm (Bomas Machine Specialties, +-Low
Sommerville, MA).” The average grain size of TiB, and B,C Precrack ...
.... Incldent
Front Angle
was determined to be 13 and 15 pm, respectively, using the Lighting
linear intercept method. The average projected area hardness
( H ) of TiB, and B,C was found to be 18.2 and 20.9 GPa,
respectively, using indentation loads of 9.8, 29.4, and 49 N.
Young’s modulus ( E ) of TiB, and B,C was determined to be
526 and 464 GPa, respectively, using the ultrasonic pulse-echo
technique. The authors have no knowledge that either of the
ceramics exhibit slow crack growth or R-curve behavior. Slow
crack growth is often observed in materials containing a glassy
grain boundary phase which is not present in either of the
materials under study. However, because TiB, fractures inter- Fig. 2. SEPB precrack length measurement method.
granularly, R-curve behavior may be a factor, due to the varying
effects of crack bridging.
achieved for valid testing as specified in JIS R 1607.’ First, the
111. Experimental Procedures precrack had to propagate from the starter notch and remain
within 10” of the loading plane. Second, the average precrack
length had to be in the range of 40% to 60% of the specimen
( I ) Single-Edge Precracked Beam Method height (1.2 to 2.4 mm). A minimum of five valid tests were
Procedures for the SEPB method are given in several refer- performed on each material to obtain an average value of Kic.
ence~.’.~’’Clarifications and modifications are described below. The mode I fracture toughness of each sample was deter-
All SEPB specimens were notched to a depth of 0.5 mm using mined using Srawley’s equation:6
a 0.2 mm thick diamond saw blade. Notched samples were
carefully aligned and centered on a steel bridge-anvil, as shown
in Fig. 1. The samples were compressed at a displacement rate
of 0.51 mm/min until a precrack formed (Model 1125, Instron,
Canton, MA). A distinct acoustic emission (or “pop in”) was where
generated from the release of strain energy when a crack
1.99 - (c/W)(l - c/W)[2.15 - 3.93(c/W) + 2.7(c/W)’]
advanced suddenly from the notch. A stetho~cope’~ attached to
the load cell was used to determine when precrack “pop-in” [l + 2(e/W)][1 - (C/W)3”]
occurred. “Pop in” loads ranged from 9 to 13 kN and 29 to (2)
36 kN for B,C and TiB,, respectively. Samples were unloaded
immediately after “pop in” to avoid additional slow crack and S = the lower span of the three-point bend fixture, P = the
extension which could change the characteristics of the “sharp” three-point flexural load at failure, c = the average precrack
crack front. length, B = the specimen width, and W = the specimen height.
The precracked specimens were then loaded to failure in a (2) Chevron Notched Beam Method
three-point flexure apparatus with a loading span of 19.05 mm, Details of the experimental procedures for the CNB method
satisfying Srawley’s requirement that the ratio of lower span to are given in the literat~re.~.”
Chevron notches were precision
specimen height (S/W) be greater than four.6 Each specimen machined into each of the CNB beams as shown in Fig. 3. The
was visually aligned in the three-point fixture so that the pre- dimensions a, and (I, were 0.3W and W, respectively. All CNB
crack starter notch was located directly below the top loading samples were fractured in a four-point flexure configuration
pin prior to testing. A displacement rate of 0.51 mm/min was with a major span of 19.05 mm and a minor span of 9.53 mm.
used during flexure testing. Specimens were fractured using a loading apparatus which
Optical microscopy with low-incident-angle lighting,I4 situ- exhibited the following compliance equation:
ated approximately 15” from the fracture surface plane, was
used to observe the initial precrack front. The light source was P = -2.9674 + 1.4307-0 + 8.044 X 10-3-D2
always located on the fast-fracture side of the specimen as - 3.4809 X 10-5.D3
shown in Fig. 2. The average precrack length was calculated
using three measurements taken at equal intervals across the where P = load (N) and D = crosshead displacement (pm).
width of one fracture surface. The difference between any two
of the three measurements did not exceed 10% of the average,
or the test was rejected. Additional crack criteria had to be
Tungsten
Carbide \r
Platen
Load
Load
r Notched
I
Fig. 3. Chevron notch beam cross-section view. Note that the crack
length at maximum load, a, does not need to be measured.
August 1995 Fracture Toughness of TiB, and B,C 2189
Several explanations for this rate dependence are possible. paper.I9 Specimens tested at rates 50.5 mm/min exhibited criti-
The most obvious explanation is that the CNB test is measuring cal crack lengths equivalent to the predicted length, a. How-
an inherent fracture toughness rate dependence which could be ever, for displacement rates >O.S mm/min, much smaller
related, for example, to a change in fracture mode. The fact that critical crack lengths were observed, corresponding to insuffi-
both materials display the same rate-dependent behavior at cient stable crack growth prior to catastrophic failure." When
virtually the same onset rate is suspect. In addition, no evidence spontaneous failure occurs at a crack length less than a,the
for a fracture mode change was observed on the fracture sur- value of Y* at failure is larger than the value of Y ; calculated
faces. A more likely explanation for the rate-dependent behav- from Eq. (4). Hence, using the assumed value of Y ; to calculate
ior is that one or more of the assumptions used to derive the fracture toughness is invalid under these conditions and tends
CNB equation were violated, resulting in the calculation of to underestimate the value of K,, .
erroneous K,, values. A valid range of displacement rates which can be used during
For the CNB test to be valid, stable crack growth must CNB testing has not been previously reported. Munz et a1.$
precede spontaneous failure during flexural loading. As a stable used a displacement rate of 0.05 mm/min during four-point
crack initiates and grows from the apex of the chevron notch, flexural loading of similar CNB specimens. Sung and Nichol-
the dimensionless stress intensity factor coefficient (Y*) son" suggest that displacement rates as low as 0.003 mm/min
decreases and finally reaches a minimum value (Y;) at the be used to initiate stable crack growth. Our CNB K,, data
predetermined critical crack length a. Stable crack growth suggest that Eqs. (3) and (4) are valid for displacement rates
through the chevron notch results in a specimen compliance <0.5 mm/min and down to at least 0.005 mm/min.
change, which is observed as nonlinearity (yielding) in the CNB K,, data for B4C in this range compare relatively well
load-versus-displacement data. If nonlinearity is exhibited and wih the SEPB-generated data. The CNB method also exhibited
sufficient stable crack growth occurs during a CNB test, a very low average standard deviation for B,C (2.2% of the
Eqs. (3) and (4) are valid for K,, determination. average toughness). However, the low-displacement-rate CNB
Fractography and load-displacement data from the CNB results for TiB, yielded an average K,, value which was 20%
specimens tested in this study indicate that all specimens exhib- lower than the average SEPB value. In addition, the average
ited some stable crack growth prior to failure, regardless of the standard deviation (7.6% of the average toughness) was over
displacement rate used. These data are presented in a separate twice that of the SEPB method. Since longer precracks are
utilized during SEPB testing, R-curve behavior may be a factor
in the observed differences for TiB, which fractures intergranu-
7,-- -
1 "
larly, but not for B,C which fractures transgranularly. Higher
scatter in the TiB, results could also be related to intergranular
fracture which causes variability in the transition from stable-
.h
I'
m i '1 1
I
Fig. 6. SEM photomicrograph of an IS B,C specimen indented with
a load of 490 N. Notice the transition from a nearlv full-uennv crack to
2 I ,
Indentation Load (N)
a half-penny (semielliptical) crack, which develops during loading of
the specimen to failure. Fig. 7. IF K,, versus indentation load for TiB, and B,C.
2192 Journal of the American Ceramic Society-Conzone et al. Vol. 78, No. 8
least differentiation between the fracture toughness of the two “J. Sung and P. S. Nicholson, “Valid K , , Determination via In-Test Subcriticdl
materials studied. Precracking of Chevron-Notched Bend Bars,”J. Am. Cerum. Soc., 72 [6] 1033-
36 (1989).
“C. B. Ponton and R. D. Rawlings, “Vickers Indentation Fracture Toughness
References Test Part 1 Review of Literature and Formulation of Standardized Indentation
‘G. D. Quinn, J. Salem, I. Bar-On, K. Cho, M. Foley, and H. Fang, “Fracture Toughness Equations,” Muter. Sci. Technol., 5 [9] 865-72 (1989).
Toughness of Advanced Ceramics At Room Temperature,” J. Res. Nutl. lnst. ”C. B. Ponton and R. D. Rawlings, “Vickers Indentation Fracture Toughness
Stand. Technol., 97 [S] 579407 (1992). Test Part 2 Application and Critical Evaluation of Standardized Indentation
’P. Chantikul, G. R. Anstis, B. R. Lawn, and D. B. Marshall, “A Critical Toughness Equations,” Muter. Sci. Technol., 5 [9] 961-76 (1989).
Evaluation of Indentation Techniques for Measuring Fracture Toughness: 11, ”U.S. Army MIL-STD-1942 (MR), “Flexural Strength of High Performance
Strength Method,”J. Am. Cerum. Soc., 64 [9] 53943 (1981). Ceramics at Ambient Temperature.”
’G. R. Anstis, P. Chantikul, B. R. Lawn, and D. B. Marshall, “A Critical ‘“G. D. Quinn, private communication, 1992.
Evaluation of Indentation Techniques for Measuring Fracture Toughness: I, ”A. A. Wereszczak and A. Parvizi-Majidi, “Effect of Fracture Temperature
Direct Crack Measurements,”J. Am. Cerum. Soc., 64 [9] 533-38 (1981). and Relative Crack Propagation Rate on the Fracture Behavior of Whisker-
4D.Munz, R. T. Bubsey, and J. L. Shannon Jr., “Fracture Toughness Determi- Reinforced Ceramic Matrix Composites,” Cerum. Eng. Sci. Proc., 11 [7-8]
nation of Al,O, Using Four-Point-Bend Specimens with Straight-Through and 721-33 (1990).
Chevron Notches,”J. Am. Cerum. Soc., 63 [S-61 300-305 (1980). 16D. G. Munz and J. L. Shannon Jr., “Fracture Toughness Calculation from
5JIS R 1607, “Testing Methods for Fracture Toughness of High Performance Maximum Load in Four Point Bend Tests of Chevron Notch Specimens,” Int. J .
Ceramics, Japanese Industrial Standard.” Japanese Standards Association, Fruct., 16, R1374141 (1980).
Tokyo, Japan, 1990. ”T. B. Troczynski and P. S. Nicholson, “Theory for the Load Relaxation
‘J. E. Srawley, “Wide Range Stress Intensity Factor Expressions for Technique in Fracture Studies Using Four-Point-Bend Chevron-Notched Speci-
ASTM E 399 Standard Fracture Toughness Specimens,” Int. J. Fruct., 12, mens,”J. Am. Cerum. Soc., 68 [8] 43943 (1985).
475-76 (1976). “C. L. Fuller, E. R. Fuller Jr., and S. W. Freiman, “Chevron-Notch Bend
’ASTM E 399, “Standard Test Method for Plane-Strain Fracture Toughness of Testing in Glass: Some Experimental Problems”; pp. 167-75 in Chevron-
Metallic Materials.” American Society for Testing and Materials, Philadelphia, Notched Specimens: Testing and Stress Analysis, ASTM STP 855. Edited by
PA, 1990. J. H. Underwood, S. W. Freiman, and F. I. Baratta. American Society for Testing
‘T. Nose and T. Fuji, “Evaluation of Fracture Toughness for Ceramic Materials and Materials, Philadelphia, PA, 1984.
by a Single-Edge-Precracked-Beam Method,” J . Am. Cerum. SOC.,71 [ S ] 19S. D. Conzone, W. R. Blumenthal, and J. R. Vamer, “Variation in Y: with
328-33 (1988). Loading Rate during Chevron Notch Testing,” submitted to J. Am. Cerum. Soc.
9L. M. Barker, “A Simplified Method For Measuring Plane Strain Fracture ’“J. C. Newman Jr. and I. S. Raju, “An Empirical Stress-Intensity Factor
Toughness,” Eng. Fruct. Mech., 9 [2] 36149 (1977). Equation for the Surface Crack,” Eng. Fruct. Mech., 15 [1-2] 185-92 (1981). 0