J . Am. Ceram. Soc.

, 70 [7]466-69 (1987)

High-Temperature Mechanical Properties of a Ceramic

Matrix Composite
ELLICE Y. LUH and ANTHONY G. EVANS
Materials Department, College of Engineering, University of California, Santa Barbara, California 93106

The change in mechanical properties of a fiber-reinforced ce- where KO is the matrix toughness, u is Poisson’s ratio,
ramic from notch insensitivity at room temperature to notch are the
~ ~ f / [ ~-,f)l,
( ~ E, and modulus of the
sensitivity at elevated temperature has been investigated. The
~

fiber and respectively, and is the volume fraction of

change in behavior has been attributed primarib to a ‘orre- fibers. Conversely, when the composite contains uniform fibers
spondin& large variation in the shear resistance Of the thatfail in the wake of the crack, the matrix cracking stress, mc,
tibedmatrix interface caused by oxidation effects at that inter- becomes the ultimate tensile sfrength.8.~Specifically, for long
face. The transition in behavior has been correlated with a
fracture model based on the incidence of fiber failure in the
crack wake.

I. Introduction

B RIITLE-MATRIX, fiber-reinforced composites have been shown

to exhibit damage-tolerant axial tensile characteristics when
the bond between fiber and matrix is frictional and the fiber
strength is high. Such behavior results in a stress-strain relation
(Fig. 1) with an apparent “yield point” caused by periodic cracking
of the matrix (at a stress, uo)and an ultimate tensile strength, a,,,
coincident with fiber bundle f a i l ~ r e . ~ High-failure
.~ strains and
notch insensitivity are characteristic of such composites.’ These
qualities are fully explicable in terms of the slip processes occur-
ring at the fiberfmatrix i n t e r f a ~ e .However,
~.~ such processes may
be temperature dependent because of thermal expansion-induced
residual stresses and possible environmental reactions. Prelimi-
nary investigation of the temperature-dependent changes in the
mechanical behavior of ceramic matrix composites constitutes \ STRAIN -
the focus of the present study. The composite used as a model sys-
tem consists”’ of unidirectionally oriented silicon carbide fibers*
within a lithium aluminosilicate (LAS) glass-ceramic matrix.’
The study involves an experimental investigation of various me-
chanical properties and micromechanical characteristics at elevated
temperature. The observed temperature-dependent behavior is as- MATRIX
sessed within the context of available fracture models. CRACK
Fig. 1. Tensile stress-strain
relation for the present com-
11. Theoretical Background 1 posite material at room tem-

Available models of crack extension in uniaxially reinforced

fiber composite^^-^ predict transitions in mechanical behavior. The
major property transition involves a change from notch-insensitive
behavior to notch sensitivity. This transition can be visualized on Fiber Matrix
a mechanism map (Fig. 2) contained within space expressed by the
fiber strength, S, and by the interface shear resistance, T. One of
the objectives of the present study is to assess the utility of the
fracture models used to derive such mechanism maps of actual
composite systems. For this purpose, the principal features of
fracture models are summarized below.
When fibers remain intact in the crack wake, the matrix crack-
ing stress, u,,,for long cracks is independent of crack length, a,
and is given by6.7

Received February 27, 1986; revised copy received December 16, 1986; approved
January 29, 1987. Interfacial Shear Resistance, r
Supported by the U . S . Office of Naval Research under Contract No.
N00014-85-K-0883.
*Nicalon, United Technologies Research Center, Hartford, CT. Fig. 2. Fracture mechanism map for a uniaxially rein-
‘United Technologies Research Center. forced ceramic matrix fiber composite.

466
July 1987 High-Temperature Mechanical Properties of a Ceramic Matrix Composite 467

Fig. 3. Mechanical response of notched beams in flexure: (A) room tem- H

perature, delamination from notch tip; ( B ) lOOO"C, crack extension from 0.251~1
notch tip.

cracks subject to an equilibrium fiber bridging zone
o, = KCa-li2
with
K , = K,D + (~s/~,,o)~I (3)
This change in mechanism occurs when the matrix cracking stress,
uo,exceeds,fS (Eq. (1)). Thus, a mechanism transition parameter
can be defined
M = .5/s3
where 5 has been derived as8
Ki(1 -f)"l - v2)T)(1 + v)2
t= f 'R
At the transition, M has magnitude Mo = 0.1.8 For values of
M < Mo,notch-insensitive, steady-state crack growth is predicted.
For M > Mo, fibers fail in the crack wake, resulting in notch
sensitivity. Evidently, therefore, the interfacial shear resistance, T ,
and the strength of the fibers, S, are predicted to exert important
influences on the fracture mechanism.
A second mechanism transition occurs when the fibers exhibit
appreciable statistical strength variability, whereupon fiber failures
occur remote from the crack plane (Fig. 2). For this case, fiber
pullout dominates the toughness such that4
AKc = l(rEf/R)'/' (6)
where I is the median pullout length.
Trends in the temperature dependence of the mechanical proper-
ties of the present SiC/LAS composite are evaluated within the
context of the mechanism map (Fig. 2) and the above properties.
111. Experimental Studies
The experimental aspects of the present study have two principal
objectives. In the first instance, general features of the high-
temperature mechanical behavior are evaluated using flexural tests
on notched and unnotched test specimens. Second, because of the
evident importance of various constituent properties on the me-
chanical behavior of the composite (particularly the interfacial
(2) shear resistance, T), the temperature-dependent characteristics of
such properties are addressed on a separate basis.
( I ) Flexural Tests
( A ) Procedure: For purposes of strength testing, uniaxial
composite plates were cut into bars with the fibers oriented longi-
tudinally. Samples with dimensions of approximately 3 by 3 by
50 mm were used to ensure a low shear-to-normal stress ratio in
(4) four-point flexure. One face of each test specimen was polished to
a 1-pm diamond finish. In some cases, notches were produced
with a 50-pm-thick diamond blade. Samples were mechani-
cally tested at a stress rate of 1 MPa.s-' using alumina flexure
(5) fixtures having dimensions of 25 and 5.6 mm across the outer and
inner spans, respectively. Samples were loaded in air at 1000°C.
Selected tests were interrupted and the prefailure damage
observed. Other tests were continued until a maximum load
was reached.
(B) Results and Interpretation: The essential trends in me-
chanical behavior are most readily visualized from notched beam
tests. At room temperature, delamination occurred from the notch
tip3 (Fig. 3(A)), resulting in a notch-insensitive mechanical re-
sponse (whereupon toughness has no ~ignificance).~ At lOOO"C,
the strength was determined to be a function of notch depth. Fur-
thermore, initial crack growth occurred normal to the stress axis
(Fig. 3(B)). Thus, at this temperature, the toughness has utility as
a fracture parameter, such that a toughness, K , = 5 MPa*m"',
expresses the mechanical response. This compares with a matrix
toughness3 of -2 MPa. ml", indicative of a toughness increase
caused by the fibers A K , = 3 MPa.m"'.
The corresponding force/displacement behavior of the com-
posite is summarized in Fig. 4. At room temperature, an initial
nonlinearity, observed at -300 MPa, was associated with matrix
while the ultimate strength (at -800 MPa) involved
fiber However, at 1000°C, the nonlinearity and ultimate
strength were determined to coincide at a stress rc= 400 MPa.
(Some load-bearing capability was retained beyond the ultimate
 468 Journal of the American Ceramic Society-Luh and Evans Vol. 70. No. 7

DEFL ECTlON

Fig. 4. Force-displacement behavior of composite in

flexure demonstrating the different features that occur at
room temperature and at 1000°C. ’

Fig. 5. Deflections of the crack along the specimen axis beyond the
neutral plane.

Fig. 6 . Fiber pullout on the fracture surface: ( A ) room temperature (courtesy of D. P. Johnson-Walls), ( B ) 1000°C in air.

-
-
-
I .-Sapphire

I I I I I 1 I I I I I I I I I I I vurface
Fig. 7. ( A ) Protruding fiber configuration used to measure trends in the interfacial shear resistance, T. ( B ) Schematic illustrating the use of a sapphire
hemisphere to determine the loadideflection behavior of protruding fibers.
 July 1987 High-TemperatureMechanical Properties of a Ceramic Matrix Composite
strength because the shear characteristics of the composite caused
the crack to eventually deflect along the fiber axis (Fig. 5 ) . ) Final
failure at room temperature was accompanied by considerable fiber
pullout (Fig. 6(A)), while, at 1000”C, pullout lengths were rela-
tively small (Fig. 6(B)).
(2) Interfacial Shear Resistance
(A) Procedures: Samples were prepared by cutting 2 by 2 by
10 mm blocks of composite material with fibers oriented trans-
versely. Then, by erosion of a portion of the matrix with fine
particles, fibers were displaced, resulting in a distribution of pro-
truding fibers across a flat matrix surface (Fig. 7 ( A ) ) .Thereupon,
a load was applied by means of a sapphire hemisphere (1-mm
diameter) emplaced on the protruding fibers (Fig. 7(B)). The load
displacement trends were thereby evaluated as the fibers were
displaced with respect to the matrix (Fig. 8). Experiments were
performed both at room temperature and at 1000°C in air after
exposures of -1 h.
(B) Analysis: The load ratio at fixed displacement provides
a measure of the trends in T. Specifically, the displacement, u , of
each fiber is related to the force, P,, on that fiber by’
P, = {(YT[U - Uo(i)]}”2 (7)
where a = 4.rrzEfR3, and uo is the initial separation between the
top of the fiber and the sapphire hemisphere (Fig. 7(B)).The total
force is thus
N The high-temperature degradation of this particular composite
P = ((YT)’” C [u - ~~(i)]”~
t=I
where N is the total number of fibers in contact with the hemi-
sphere at displacement u. However, since u,(i) and N are indepen-
dent of the test temperature,* T is simply proportional to P z . The
square of the ratio of the loads at given deflection (Fig. 8) thus
provides a direct measure of the variation in T between room
temperature and 1000°C. The results indicate that the interfacial
shear resistance at 1000°C is approximately 20 times that at room
temperature. Consequently, because at room temperature T is
about 2 MPa,’ T at 1000°C is estimated to be approximately
40 MPa.
IV. Concluding Remarks
The significant increase in T measured in a ceramic matrix
composite at elevated temperature is in accordance with the ob-
served decrease i n fiber pullout length and the corresponding
fracture mechanism change. Fracture models predict such a
mechanism transition from notch-insensitive to notch-sensitive be-
havior, subject to a sufficient increase in T or decrease in fiber
strength, S . Independent studies of the effect of high-temperature
exposure” indicate that the fiber strength decreases from about
2 GPa at room temperature’ to -1.0 GPa when tested at 1000°C
in air. Taken in conjunction with the corresponding change in T
from 2 to 40 MPa, ascertained in the present study, a substantial
change occurs in the dominant material parameter, S 3 / 7 (Eq. 4),
from 4 X 10” Pa’ at room temperature to 2.5 X IOl9 Pa2 at
*Clearly uo(i) and N vary spatially across a composite, resulting in appreciable
statistical variability in P(u) between tests at the same temperature. Nevertheless,
given a sufficient number of tests at each temperature, the median load provides a
unique measure of trends in 7 with temperature.
469
Displacement, 6
Fig. 8. Force-displacement characteristics of pro-
truding fibers. The load ratio, P , / P , , at given displace-
ment, provides a measure of the change in T .
1000°C. Such large changes are consistent with the existence of the
mechanism transition. However, a detailed comparison with theory
awaits statistical analysis of fiber strengths and associated pullout
contributions to the strength and toughness.
system undoubtedly involves chemical effects associated with the
environment because similar tests performed in an inert environ-
ment do not show an equivalent reduction in fiber pullout and notch
sensitivity.’ However, the detailed relations between the reaction
process and the change in T remain to be investigated. Some recent
studies” have indicated that, at 1000°C in air, the surface layer
oxidizes preferentially and thus the present measurements of the
shear resistance T presumably refer to the interfaces in that layer.
Consequently, the results may not be strictly representative of the
interfaces near the crack plane. Further research is needed to re-
solve these aspects of the problem.
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