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ABSTRACT
It is well known that mechanical character&tics of the fibre-matrix interface
in MMCs have a strong influence on various properties. However, there is
much uncertainty surrounding the question of how best to control the
structure of the interfacial region in order to optimise particular types of
composite performance. In this paper current thinking on how interfacial
characteristics affect composite properties is briefly summarised. The
importance of different types of stress relaxation processes is emphasised.
This is followed by some observations about testing procedures designed to
measure bond strength in MMCs. It is noted that these invariably involve
predominantly shear loading, whereas there is a need to explore the response
of interfaces to tensile and mixed mode conditions. Finally, some observations
are presented on interfacial chemical reactions and the development of fibre
coatings.
1 INTRODUCTION
When compared with material produced in the early 1980s, significant
improvements in the mechanical properties exhibited by metal matrix
composites (MMCs) have been obtained over the last few years. This has for
the most part been achieved by processing route improvements, leading to a
reduction in the level of gross defects such as matrix porosity and
inhomogeneities in the spatial distribution of reinforcement. Further
progress now requires a fundamental understanding of the interplay
25
Composites Science and Technology 0266-3538/9I/$03.50 1991ElsevierSciencePublishers
Ltd, England. Printed in Great Britain
26
2 THE ROLE OF T H E I N T E R F A C E IN M M C P E R F O R M A N C E
(1)
where a t is the radial stress (normal to the interface) at the point concerned,
which must be negative (compressive) if rr~ is to have a non-zero value. (This
is usually the case in MMCs as a result of differential thermal contraction.)
Under applied load parallel to the fibre axis (x-direction) differential Poisson
contraction effects often cause the value of a r to vary along the length of a
(discontinuous) fibre:
or(x) = a~aT + O',av(X)
(2)
where cry,,T is the radial stress from differential thermal contraction (see
below). It is c o m m o n to assume that the shear stresses at which both
debonding and frictional sliding take place are independent of other
27
28
T ~ Clyne, M. C. Watson
~ C t AT stresses]
+ applied
!iiiii /1
load)
,
Interfacial Vacancy
Interracial Debonding
Diffusion ~ ~CIi.~/~x
'~,
Interracial Frictional
Sliding, ~:fr= p. ~r
Interracial
Decohesion
/Cavitation
GH.
Fig. 1. A schematic view of the interracial stresses in a short-fibre MMC subjected to (a) a
temperature decrease and (b) a superimposed axial tensile load. Also shown are schematic
illustrations of some of the processes which might take place at the interface under the
influence of the stress field.
29
Applied
Stress (MPa)
Global
_ . , UnrelaxedWo~
~
Harlning
Plastg'tY.,'~"~Failure
r'~"~'/
,,:
,:"
I~
~1
Ioo/
Relaxation
U.Zi ...:.r...TF~._.~.
_ ~
[ M - ' ~ " ~ ~ S i C ~ (s=lO) I
~al
El~iic
d.s~
(a)
300Applied
Stress
(MPa)
11o~
(b)
115~ S/rain
i [ as.received SiC ]
200 -
[ pre-oxidisedSiC ] x
100
2%
4%
6%
Su'ain
tc)
Fig. 2. The influence of stress relaxation processes on the tensile stress-strain behaviour of
short-fibre or particulate MMCs: (a) a schematic curve showing the processes controlling the
shape; (b) three curves for a SiC whisker-reinforced Mg-Li alloy at differenttemperatures and
strain rates;s and (c) two curves for SiC particulate-reinforced AI alloy, with and without the
prior formation of an oxide layer on the SiC. 9
misfit between the (stress-flee) shapes of the fibre and the corresponding hole
in the matrix; this transfers load strongly to the fibre and hence raises the
load-bearing capacity of the composite.
In practice, various stress relaxation phenomena tend to be stimulated by
the resulting sharp gradients of stress within the matrix, these being
processes which transfer load back from the fibre to the matrix. An example
of how stress relaxation can affect the behaviour can be seen in the stressstrain curves of Fig. 2(b). These are for a matrix in which diffusive processes
are fast at room temperature. 7.s Testing at high imposed strain rates or low
temperature gives little scope for diffusive stress relaxation processes. The
30
effect of this is to raise the work-hardening rates but to reduce the ductility. If
the high fibre stresses caused by matrix plasticit.v are not relaxed in some way
then cavitation or fibre fracture are likely, leading to t:ailure of the specimen.
A similar type of effect is seen in Fig. 21c). In this case the provision ot'a thick
oxide laver on the interti~ce appears to p r o m o t e stress relaxation, raising the
ductility. This is probably 9 due in large part to decreased resistance to
intertitcial sliding, which also has the effect of reducing the stress in the
reinforcement. (It should, however, be noted that magnesium in the alloy
migrates to the oxidised inter[itce, reducing the age-hardening capacity of
the matrix and probably contributing to the observed effect.}
The simplest picture of stress relaxation mechanisms as a group oF
processes is obtained by considering the reduction the) effect in the misfit
strain between the shapes of fibre and hole. This is illustrated in Fig. 3 t'or
punching of prismatic dislocation loops'~'-" '~ inot to be confused with global
I- .4
!- -i
tat
a,'%
1
tbl
31
%
(a)
(b)
Fig. 4. Two photoelastic fringe patterns in the matrix around short ellipsoidal and
cylindricalfibresunder axial loading.Note the high shear stresses(high fringeorders)near the
'corners' of the cylinder.
32
77.~i C/yne, M. C. ~ t s o n
Under most loading configurations high tensile stresses build up at the fibre
ends and these can cause interracial cavitation. Conditions for cavity
nucleation and growth at a stiffinclusion are uncertain, with some attthors, 1:~
for example, predicting an increase in the critical plastic strain for cavitation
with particle size and others t.* the reverse. Nevertheless, it is again evident
that fibre ends are preferred locations, and FEM computations have been
used to explore this. is
Much of the difficulty in laying down ground rules for tailoring interracial
properties lies in establishing a criterion (related to interracial strength
parameters) for the onset of interracial debonding/cavitation lwhich is
thought to lead rapidly to composite failure by growth and link-up of
cavities). One approach is to consider the hydrostatic component of the
stress state, o H, expecting a critical {tensile) value for cavity formation.
dependent on the bond strength (but with a maximum value corresponding
to nucleation within the matrix). A variation o f o Hwith position predicted by
the Eshelby model 16'~v is shown in Fig. 5ta). This confirms the sharp peak in
the matrix at the fibre end. This may be reduced by the differential thermal
contraction stresses expected at room temperature but, on the other hand, it
will be greater when the fibre end is fiat rather than rounded. A cavity
formed at the end of a fibre lying parallel to the applied stress axis can be
seen in Fig. 5(b). It may be deduced from the above that a useful goal for
composite production would be an interface prone to sliding but resistant to
cavitation.
3 BOND S T R E N G T H M E A S U R E M E N T
Techniques for measurement of interfacial characteristics can be classified
according to the phase angle of interracial loading generated during the
test.* (Interracial critical strain energy release rates will vary with this phase
angle.) Compact tension, flexural (4-point bend) and fibre pult-out push-out
tests respectively have phase angles of about 0, re/4 and rr/2--corresponding
to pure opening (I), mixed (I + II) and pure shearing (II) modes (see Section
2.1). Most measurements on M M C s have focused on shear debonding and
sliding (often using simple variants of the shear lag theory to interpret the
data), with little or no attempt to introduce substantial mode I components
to the loading. It might be argued that an interface exhibiting a high shear
debonding stress would also be expected to resist decohesion strongly. That
this is not necessarily true can be seen from the fact that pronounced
interracial roughness is expected to raise the former (in shearing mode) while
having little effect on the latter (in opening mode), This type of argument
33
GH
""I-. I
t"7/
iii
"",..
150~P~
(a.)
(b)
Fig. 5. Cavitation is stimulated by high tensile hydrostatic stresses, particularly when these
occur at the interface.and the bond strength is not high. (a) A map of the hydrostatic stress
around an isolated ellipsoidal SiC particle in an Al matrix subjected to 100 MPa tensile load;
this prediction was obtained using the Eshelby method, t6''~ (b) A TEM micrograph showing
a cavity formed at the end of a SiC whisker in an A1 matrix after tensile straining.
34
provides an immediate insight into the dependence of Gi~ on the phase angle
of loading referred to above. It may also be noted in this context that there
may be practical benefits in promoting interfacial sliding {to encourage
energy absorption at the interface) while inhibiting decohesion and
cavitation (which tend to promote failure of the component). Under these
circumstances more sophisticated tests are required in order to monitor and
control the interracial mechanical characteristics and this is an area of
ongoing research.
(50*~ ( 5
Applied
Stress
(50
x=O
/
35
x=L
.-----.]i-
jdebonded
ent f
G_(x) = G ._+
~v(X)
121
~t (sr (x)"
L'
Fig. 6. Schematic illustration of stress distributions during the pull-out test.
The frictional sliding behaviour has also been analysed, taking account of
the effect of the Poisson contraction of the fibre in reducing the radial
compressive stress. On the basis of a crude assumption that only the fibre
carries an axial normal stress (with the resulting radial strain at the interface
producing a reduction in radial stress proportional to the matrix stiffness),
relationships are obtained between pull-out stress and length remaining
36
X=(
X=X )
debonded
Applied
Stress
G0
Displacement of
Loading Point
Or(X),= (J
(J0s~
! !ii.!
" <
u%~x, .... ~
Fig. 7.
"
+ G
'xl
i!
(o rx
.',~v0; ' 0
~TJ
37
(a)
(b)
Fig. 8. S E M micrographs of a Ti-SiC monofilament specimen afterpush-out testingwith a
conventional microhardncss machinc, showing (a) the indented fibreand (b) the pushed-out
fibre end protruding from the rcvcrsc facc.
38
T I,~-2C(vne, M. C. ~btson
Interracial
shear stress
(MPa)
i
0.08 i
!
0"061
0.04
"
Pv'r= 5
"3
~_)xperiment
L
Oo= o.29.,,P
0.02 i
[
r
ob
~.,
I
02
0.4
4-
-9,
P
0.6
0.8
1.0
Fractional distance along fibre
Fig. 9. Photoelastic measurements can be used to explore the validity of models for the
elastic behaviour during bond strength testing, From the comparison shown here it can be
seen that the Hsueh model is in fair agreement with a set of such measurements.
this way: for such large diameter fibres a quick examination in the optical
microscope will reveal whether the fibre has been displaced after the
application of a particular load. However, a difficulty then arises rrom the
uncertainty about whether the load found to be necessary for push-out
corresponds to the onset of debonding (ao,) or to frictional sliding along the
complete length (%s). An advantage of the test. however, is that a
comparison can be made with the load needed to push the partially pushedout fibre back into the matrix. The recording of a load similar to that for
initial push-out suggests that a0~ is being measured.
Again the analysis is carried out in two regimes, corresponding to the
elastic case and to pure frictional sliding. Hsueh 27 has presented treatments,
based on the shear lag analysis, for both of these. Figure 9 shows a
comparison between predicted curves and experimental data obtained with
the 3-D frozen stress photoelastic technique. These data were obtained by
using two photoelastic resins (with a stiffness ratio of about 2) for matrix and
fibre. Measurements of the fringe order, and of the principal stress
directions, as a function of position along the fibre were combined in a
simple Mohr's circle calculation to give the variation along the fibre length
of the shear stress parallel to the interface. It can be seen that this is in
reasonable agreement with the Hsueh model for this case.
The Hsueh model for the frictional sliding behaviour predicts, at least for
MMCs, a much more uniform distribution of shear stress along the fibre
length than in the elastic regime. This is a strong function of the fibre Poisson
ratio and the matrix stiffness. Figure 10 shows plots ofrrr for SiC fibres in Ti.
It is evident that for this combination (and most MMCs) the value of ~rr
39
Interracial
shear
stress 30
(MPa)
20
s= 10
(~raT ~
S=2
10
SiC monofilament in Ti |
R/r = i0
1.1.=0.3
(~r&T = " 50 MPa
I
0.2
0:4
0:6
o18
1:o
Fig. 10. The frictional sliding stress in the pull-out test varies along the length of the fibre as
a result of the Poisson expansion of the compressed fibre. The significanceof this effect is
greater for large values of the fibre Poisson ratio and matrix stiffness.Predicted variations are
shown here for SiC fibres of 100/~m diameter, with various aspects ratios, in a Ti matrix.
remains close to/tara r. A consequence o f this is that the frictional push-out
stress, O-os,is predicted to rise in an approximately linear m a n n e r with fibre
aspect ratio. Predictions for ao. and aos as a function of fibre aspect ratio are
compared in Fig. 11 with experimental data for SiC monofilaments in an assprayed titanium matrix. These data were obtained with a simple
microhardness machine, so that there is initial uncertainty as to whether the
peak loads represent the onset or completion of debonding. However, it can
be seen that the experimental data are not consistent with the predicted ao.(S)
curves but conform to those for frictional sliding with a zfr value of about
35--40 MPa. This conclusion is supported by the observation of similar loads
for push-out and push-back operations. However, one effect of the limited
variation in frictional sliding stress along the fibre length is that good
agreement with experiment can be obtained over a wide range of # and Or/,r
combinations (giving the same product zfr)3.3 The full fragmentation test
A method that has been used for M M C s is the so-called 'full fragmentation'
technique. This procedure for deducing a shear strength involves embedding
a single fibre in a matrix, then imposing a large plastic strain in tension and
measuring the m e a n aspect ratio of the resulting fibre segments. Analysis is
based on a constant z, with the Weibull modulus of the fibre taken into
account. 2s'2s One o f the problems with the method is that it is unclear
precisely what is being measured, although it is presumably related to z..
T. 14/..Clyne, M. C. Watson
40
Debonding
stress
(MPa)
1
.
Is
aft, 80o
600
,g,
"U, = 65 MPa
"
0/7"
~. .......
i:.~==~m.=~,".=di.=Pt.=cedJ,
0.1
0.2
0.3
Specimen
0.4
thickness
(mra)
(a)
Pushout
0
.
stress
(MPa)
1
.
% =oo I
|
r=50 m
R/r = 10
~ "
i
,
.
0.1
-75 MPa
./"
400
(~ = - i00 MPa
raT/
,~4
Maximum u n d i s p l a c e d J .
0.2
J.
0.3
0.4
(h)
Fig. l l . When the push-out test is done with a conventional microhardness tester, there is
uncertainty about whether the recorded minimum push-out loads correspond to debonding
or frictional sliding. It can be seen here that, for these data obtained with SiC monofilaments
in sprayed Ti, the form of the debonding curve (a) is not consistent with the observed results,
while reasonably good agreement is observed with the frictional sliding predictions (b).
41
gested a high af. value (several GPa) for AI-SiC: it certainly appears that this
bond is normally stronger than that for Ti-SiC, although the details are
probably sensitive to interfacial contamination or precipitation. More
experimental data are needed in order to confirm such effects. Various other
procedures have also been suggested, although all those for fibres tend to
generate predominantly mode II loading conditions. The development of
mixed mode loading conditions at fibre/matrix interfaces has been
discussed 31 for ceramic matrix composites, in which differential thermal
contraction can generate tensile radial stresses when the matrix has the lower
expansivity.
3.5 Some data for the Ti-SiC system
It is not appropriate here to attempt any systematic survey of published
data, but a limited comparison of results for Ti-SiC monofilament
composites is shown in Table 1. The strengths for an as-sprayed matrix
appear low and somewhat variable. These composites have little or no
interfacial reaction and the matrix also has some porosity (---5-10%),
leading to reduced radial compressive stress. The carbon-rich coatings on
the SCS fibres are expected to shear very readily when unreacted. However,
the pull-out values seem a little low and test data often appear less
reproducible with MMCs than those obtained by the push-out procedure.
The other composites were all given a heat treatment during fabrication
sufficient to form reaction layers. This raises T, compared with the assprayed composites, although further heat treatments have little effect. 23
Strength values obtained from the fragmentation test often seem a little
high; this may be a consequence of the simplifications in the analysis or of
the fact that the continued plastic flow of the matrix will raise the radial
compressive stress.
TABLE 1
Interfacial Shear Strength Data for Ti-SiC Monofilament Composites
Matrix
SiC
fibre
Ti
Ti
Ti
Ti-25AI-10Nb-3V
Ti-6AI-4V
Ti-15V-3AI-3Cr-3Sn
Ti-25Al-10Nb--3V
Ti-rAI-4V
Ti-rAI-4V
Sigma a
SCS-6 a
Sigma
SCS-6
SCS-6
SCS-6
SCS-6
SCS-6
Sigma
Fabrication
route
Spray deposit
Spray deposit
Spray deposit
Powder hot press
Diffusion bond
Diffusion bond
Diffusion bond
Hot press
Hot press
Test
procedure
r,
(MPa)
Pull-out
Pull-out
Push-out
50
5
-110
150
120
120
180
345
Push-out
Push-out
Push-out
Push-out
Fragment
Fragment
rfr
Reference
(MPa) number
12
1
35
60
90
80
50
---
32
32
33
23
24
24
24
34
34
T. W. Clyne, M. C. Watson
42
As-Received
AI
25-
-HF stripped
-SiO2 binder
.hi5
10
'0
Fig. 12. Shown here are XPS analyses of AI, Si and Mg levels in the surface layers of'Saffil'
fibres after various treatments. A brief exposure to HF acid is used to remove a thin surface
layer on the fibre, while prolonged immersion of a composite in sodium hydroxide solution
dissolves away all the matrix. These data confirm that the thin silicon-rich surface of the fibre
becomes impregnated with Mg during manufacture of the composite.
43
(a)
(b)
Fig. 13. SEM images of(a) Sigma (stoichiometric) SiC and (b) SCS-6 (C-rich surface) SiC
monofilaments after 50 h at 800C in titanium, showing thick reaction layers and extensive
cracking.
77 14":Clyne, M. C. Watson
44
I00
reacuon layer
thickness (p.m)
45
(a)
(b)
Fig. 15. Optical micrographs of Ti-SiC particulate composites after impact testing,
sectioned normal to the fracture surface, showing specimens with reaction layer thicknesses
of about (a) 0-2pm and (bt 5pro.
5 FIBRE COATINGS
T. ~~ Clyne. M. C. Watson
46
Element
X
For o_ride o f X
AGloooK
D x at tO00 K
Do at IO00 K
( k J m o l e - l)
(m 2 s - ~i
(m" s - l)
Ti
-710
--
--
A1
-893
---
--
Mg
Y
- 996
-1080
--1-3 x 10 -21
-l ' 0 x 10 -Z6
Zr
-840
1 8 x 10 -26
4-t x 10 -1'~
Hf
- 892
NA
NA
47
48
Stress
(MPa)
40O
tfoop
30O
200
, /
100
Radial
.~
0
Radial
distance
-I00
0
10
2o
30
4o
50
(~.m)
tai
Fig. 16. Predicted stress distributions ta) are shown here for W-cored SiC monofilament
with a 2-!tin yttria coating, after cooling through 500 K. That these stresses can be sufficient to
cause serious damage is evident from the SEM micrograph (b), which is of a SiC
monofilament with a yttria layer about 1-2 ~m in thickness, after cooling down from 900:C.
Both hoop and axial cracking has taken place.
metals
(TE)
Iorkwtion
Growing
deposit
Sputteting target
In-plane Stress in
Coating at Room
Temperature
Quenched-in
Vacanciesetc
-0.3 T,
t/
I-
I
-- .-
. .*
I. *-
Differential
thermal
contraction
Substrate
Temperature
ROOlll
CompressionTcmpcratun
__._.-._._._._._.-.-.-.-.-
Atomic
Peening
Fig. 17. Atomic peening during sputter deposition can induce large compressive stresses in
a coating. Shown here are (a) a depiction of the process and (b) a schematic illustration of the
effect of formation temperature on the final (in-plane) stress in a sputtered layer. for a case
where the layer has a higher expansivity than the substrate.
structure
Fig. 18.
i
I
Fig. 19.
50 t.tm
'1
51
Fig. 20. SEM micrograph showing an interface in a composite exposed to 950:C for 2 h.
The coating is intact over most of the circumference; note, however, that there is a region near
the bottom left where it has become mechanically damaged and some attack has taken place.
6 SUMMARY
The nature of the fibre-matrix interface influences the performance of
MMCs in a number of ways. The following points have been identified.
(a)
52
T. ~ Clyne, M. C. Watson
conditions. In practice, although this can be done for planar bimaterial interfaces, virtually all tests developed so far for fibre
composites involve pure shear (mode II) loading.
(d) Fibre-matrix chemical attack can have a strong effect on interfacial
mechanics. A limited degree of reaction usually seems to raise the
bond strength, but substantial attack makes the interface prone to
cracking and can render the composite very brittle. This may be
partly due in some cases to a change in the stress state caused bv the
volume change on reaction.
(e) The design of fibre coatings is a complex area currently under
intensive study. Some information has been given about the factors
to be considered in optimising the structure of barrier coatings
produced by sputter deposition for use in titanium composites.
(f) It has been emphasised throughout that an appreciation of the
interfacial stress state during fabrication and service is of
considerable importance.
ACKNOWLEDGEMENTS
The authors are grateful to a number of their colleagues, notably Dr P. J.
Withers, Dr R. R. Kieschke and Mr A. J. Reeves, for contributions to the
work described and for useful discussions. Financial support for one author
(M.C.W.) is being provided by the Interdisciplinary Research Centre for
High Performance Materials at Birmingham, and the collaboration of Prof.
M. H. Loretto, the Director of the Centre, is gratefully acknowledged.
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