MATERIALS

SCIENCE &
ENGINEERING

ELSEVIER Materials Science and Engineering A197 (1995) 19 30

A

Strength and fracture toughness of aluminum/alumina composites

with interpenetrating networks
Helge Prielipp a, Mathias Knechtel a, Nils Claussen ", S.K. Streiffer b, H. Miillejans b,
M. Rfihle b, Jfirgen R6deD*
~'Advanced Ceramics Group, Technische Universitdt Hamburg-Harburg, D-21073 Hamburg, Germany
bMax- Plam'k-htstitut ./~ir MetallJbrschung, Institut fiir Werkstoffivissenschq#, D-70174 Stuttgart, Germa*o,
Received 18 July 1994; in revised form 27 October 1994

Abstract

The mechanical properties of metal reinforced ceramics, especially AI/A1203 composites with interpenetrating networks, are
described. Key parameters to tailor the characteristics of these materials are the ligament diameter and volume fraction of ductile
reinforcement. Fracture strength and fracture toughness data are given as a function of both variables and are compared with the
corresponding values for the porous preforms. A simple model accounts for the influence of metal volume and metal ligament
diameter on the plateau toughness of the composites. The increase in fracture strength from the porous preform to the composite
is found to be much larger than the gain which can be predicted from the increase in fracture toughness alone. A discussion of
fracture strength in these composites therefore must include at least two issues, crack propagation through the matrix as well as
crack initiation at metal filled pores.

Keywords: Fracture; AI/A120 3 composites; Interpenetrating networks

1. Introduction to our current understanding. The toughening mecha-

Metal reinforced ceramics have very attractive me-
chanical properties when designed as interpenetrating
networks. Various methods are available to produce
these materials, such as squeeze casting [1], directed
metal oxidation [2], and infiltration with [3] and with-
out [4] gas pressure. Potential advantages of these
composites are high toughness and strength compared
with the untoughened matrix material. A1/A1203 pro-
duced by directed metal oxidation [5] was reported to
exhibit a fracture strength st- of 345 MPa and a fracture
toughness Kit of 9.5 M P a m 12. For A1/AI:O 3 manufac-
tured by gas pressure metal infiltration, a strength of
760 M P a and toughness of 5.8 M P a m 1:2 were observed
[6]. A fracture toughness as high as 15 M P a m ~:2 has
been reported in the W C / C o system [7].
A substantial amount of work, in the fields of both
ceramics [8 12] and intermetallics [13 16] contributes
*Present address: TH Darmstadt, Ceramics Group, D-4295 Darm-
stadt, Germany.
nism believed to be effective in ceramic/metal
composites is the plastic stretching of metallic inclu-
sions bridging the advancing crack. The bridging liga-
ments exert closure stresses which reduce the stress
intensity at the crack tip [17]. There is general agree-
ment that the toughening c o n t r i b u t i o n by plastic de-
formation of the ductile phases is governed by the
yield strength of the metal constituent and its uniaxial
flow stress as established under the constraint of a
more or less well bonded interface between metal and
brittle matrix. The change in uniaxial stress p in the
bridging ligament with crack opening 2u is represented
by a stress displacement function p(u) which uniquely
describes the reinforcement characteristic [18]. The
shape of the p(u) function determines the way in
which the crack resistance develops as the cracks
grows; hence it controls the final steady state tough-
ness.
Experimental efforts at this stage are mainly con-
cerned with the issue of crack propagation. These stud-
ies are aimed at determining the p(u) function in model

Elsevier Science S.A.

SSD1 0921-5093(94)09771-4
20 H. Prielipp et al. / Materials Science and Engineerblg A 197 (1995) 19 30
systems [10,13,14,17] or are restricted to post-fracture
investigations of the final ductile phase elongation
[9,19]. In contrast, the strengthening mechanisms
afforded by the inclusion of the ductile phase have not
yet been explored in any detail. Pickard et al. [20]
modeled the strength of A1/A1203 composites rein-
forced by SiC particles. The strength limiting defect was
quantified by the SiC particle size with no consideration
of the metal phase. Initial computations of the strength
of ductile particle reinforced brittle matrix composites
were presented by Bao and Zok [21]. The calculations
were based on the p(u) function and the assumption
that the initial flaw size Co and the elastic properties of
the matrix are the same as those of the composite. The
results showed an enhancement of toughness as well as
strength, while the toughness increases more than the
strength. Furthermore, the steady state toughness in-
creases monotonically with debond length, whereas the
strength is maximized at an intermediate value of
debond length. A correlation between the calculations
and experimental data has not yet been presented. In
contrast to this theoretical work, a reduction in the
initial flaw size in the composite was also proposed [6].
Factors which influence the toughening imparted by
a ductile phase are the volume content, ligament diame-
ter, interface properties and the metal properties such
as flow stress, work hardening and ductility. Theoreti-
cal work [7,8,12,22] suggests that the fracture resistance
will increase with volume fraction and bridge diameter.
Good experimental data are so far restricted to the field
of hard metals [7].
The intent of this paper is to provide a perspective of
the range of mechanical properties which can be
achieved with metal reinforced ceramics. Two key
parameters in tailoring the characteristics of A1/A1203
composites are investigated, the metal volume fraction
and metal ligament diameter. Metal infiltration affords
an opportunity to study the influence of these parame-
ters on the strength and toughness. Finally, this manu-
facturing method also makes it possible to examine the
influence of metal properties and interface behavior on
these same properties.
2. Experimental approach
The A1/A1203 composites were prepared by gas pres-
sure metal infiltration. Three materials of different mi-
crostructural scale (termed small (s), medium (m) and
coarse (c)) were produced with a metal content of
25 vol.%. Materials with medium-scale microstructure
and varying metal content from 10 to 40 vol.% A1 were
also produced. An additional batch of the coarse-
grained material was prepared with 35 vol.% metal.
A1203 bodies with small pore channels were manu-
factured using a reaction bonded alumina (RBAO) [23],
starting with 55 vol.% A1 and 45 vol.% A1203 (Ceralox
HPA 0.5). After attrition milling in acetone with alu-
mina balls of 3 mm diameter for 9 h, the sieved and
dried powder mixture was uniaxially pressed into plates
at 5 0 M P a and then cold isostatically pressed at
250 MPa. The plates were reaction bonded with the
following heating schedule: 7 h to 450 C, then 20 h to
1150C and a dwell time of 6h. Sintering at 1275 C
for 30min yielded a porous alumina body with a
density of 75% theoretical density (TD). Medium- and
coarse-sized microstructures resulted from slip cast
medium (Alcoa CT 2000 SG) and coarse (Alcoa CL
5000) grained alumina powders respectively. Slurries
with 45 vol.% solid content were cast into plates of
dimensions 50 x 30 x 10ram 3. In contrast to the
medium-grained alumina powder, the coarse powder
was first attrition milled in ethanol with alumina balls
of 3 mm diameter for 4h, and a gummi arabicum
binder was added to the slurry. Sintering for l h at
1450 C (medium-grained powder) and 1650 C (coarse-
grained powder) yielded bodies with a density of 75%
TD.
The porous plates were ground to dimensions of
50 x 30 x 5 m m 3 and then infiltrated with pure A1
(99.999%) in a specially designed gas pressure metal
infiltrated furnace with an incorporated hydraulic ram
(Fig. 1). The plates were originally held in a fixture
which was immersed in a crucible filled with metal
chips. The furnace was heated past the melting point of
A1 (671 C) up to 1050 C in vacuum, and an argon
pressure of 15 MPa was applied for 30 min to facilitate
infiltration (Fig. l(a)). Subsequently, the furnace was
cooled and, at 700 C, the infiltrated plates were lifted
out of the melt (Fig. l(b)). The pressure was not
released before the temperature decreased below the
melting point in order to suppress leakage of liquid
metal from the preform. The metal infiltrated medium
scale (m) and coarse scale (c) composites are compared
with porous and dense A1203 of about equal grain size.
sampleholder
crucible I graphite-heater
ceramic body
fullyinfiltrated
uninfiltrated
infiltrated moltenmetal
a) b) crucible support
Fig. 1. Schematic diagram of gas pressure metal infiltration furnace
during infiltration (a) and after infiltration (b).
 H. Prielipp et al. / Materials Science and Engineering A 197 (1995) 19 30
The composites with medium microstructural scale are
compared with a fine-grained alumina (Taimei T M -
DAR). This A1203 powder was uniaxially and subse-
quently cold isostatically pressed into bars. Sintering at
1350C for 15rain yielded bodies with a density of
greater than 99% TD. The manufacturing process is
described in more detail elsewhere [24]. Sintering of the
slip cast medium-grained A1203 powder (CT 2000 SG)
compacts at 1650C for 6 h yielded coarse-grained
alumina with a density of greater than 98% TD. This
A1203 was compared with the c composites.
Densities were measured geometrically and by the
Archimedes method using water as the immersion
medium. The pore size distributions were determined
by mercury porosimetry (poresizer 9320, Micrometrics).
Microstructures of the porous and dense alumina
were revealed by thermal etching in air at 1300 C for
15 min and 1340 C for 20 rain respectively. The grain
sizes were determined by a linear intercept technique
[25].
Optical microscopy of polished surfaces was used to
characterize the microstructures. Scanning electron mi-
croscopy (SEM) was employed to investigate both frac-
ture surfaces and surfaces which were polished and
thermally etched. S, m and c composites with 25 vol./o
metal content were further characterized by conven-
tional transmission electron microscopy (TEM) using a
J E O L 2000FX operated at 200 kV. T E M samples were
prepared by standard dimpling and Ar ion-milling tech-
niques. Bonding at AI-A1203 m e t a l - c e r a m i c interfaces
in all three scale materials with 25 vol.% metal content
was investigated by spatially resolved electron energy-
loss spectroscopy (EELS) in a dedicated scanning trans-
mission electron microscope (STEM). This instrument
has a beam diameter of less than 1 nm and an energy
resolution better than 0.8 eV which allows investigation
of near-edge structures in spectra with high spatial
resolution (Vacuum Generators, V G HB501). Three
spectra were recorded for each interface: one at the
interface, one in the nearby metal and one in the
adjacent alumina grains. The spectrum measured at the
interface also contains components from both materials
owing to the size of the electron beam. These compo-
nents can be removed by subtracting the two reference
spectra. The remaining component of the spectra repre-
sents the bonding of the atoms directly at the interface.
Further details of this spatial difference method as
applied to interfaces are provided by Bruley [26], Bruley
et al. [27] and Mfillejans and Bruley [28].
Elastic properties of metal/ceramic composites with
25 vol.% and 35 vol.% AI were determined using a
non-destructive ultrasonic technique [29]. Measure-
ments were performed using plates with a thickness not
less than 5 mm.
The fracture strength was measured in four-point
bending according to G e r m a n standard D I N 51110 but
21
1oo
80 s
60
o- 40
[J_
20
0
10-2 10-1 10 0 10-2
Pore size [pm]
Fig. 2. Intrusion pore size distributions of small (s, density 75 vol.%),
medium (m, density 60 90 vol.%) and coarse (c, density 65 and
75 vol.'7,,) grained alumina.
with rectangular bars cut from the plates, of reduced
length (25 x 4 x 3 m m 3) and with loading spans of 10
and 20 mm. The tensile side was polished to a 3 ~tm
surface finish and the edges were beveled.
The fracture toughness was determined using the
single edge precracked beam (SEPB) method ( D | N
51109) using five bars of the same size as described
above. The precracks were 1 2 m m long. Samples were
renotched before testing to leave metal-ligament bridg-
ing lengths Cu of less than 25% of the total (including
the notched) crack size c. The selected normalized
bridging lengths Cb/C were in the range 0.2 0.25 and
the normalized crack lengths, were in the range 0.25
0.5. According to Zok and H o l m [30], the measured
toughness is thereby overestimated by 10%-30%.
3. Results
3.1. M i c r o s t r u c t u r e o f porous prefi)rms
All three A1203 types with a porosity of 25% exhib-
ited a rather narrow distribution of the intrusion chan-
nel size. The corresponding values for the median
intrusion channel size were 0.08 lam, 0.25 lam and
0.8 ~tm for s, m and c materials with a porosity of 25%
respectively. With varying porosity, the median pore
size also changed but still remained in a rather narrow
distribution band. Fig. 2 shows bands of pore sizes for
two extreme density values for m and c materials
compared with the pore size distribution of the s mate-
rial with 25% porosity. The pore size distributions are
not overlapping as revealed by median values between
0.1 and 0.25 ~tm for the m and between 0.8 and 1 lam
for the c samples. For the medium-grained alumina in
the range 2 5 % - 4 0 % porosity, the median channel di-
ameter is nearly constant (d = 0.25 ~tm). With decreas-
ing porosity from 25% to 10% and 35% to 25%, the
pore size will decrease for the m alumina from 0.25 to
0.1 gm and for the c alumina from 1 to 0.8 ~tm respec-
tively.
22 H. Prielipp et al. Materials Science and Engineering A 197 (1995) 19 30
The grain sizes for the porous alumina bodies pre-
pared with the medium- and coarse-grained powder
were 1.2 and 4.0 ~tm respectively. This holds for densi-
ties ranging from 60% to 90/,, TD.
The fine-grained dense A1203 (Taimei T M - D A R )
exhibited an average grain size of 1.7 mm which is
nearly the same as that of porous m alumina. Sintering
of the slip cast medium-sized AI203 powder yielded an
average grain size of 1.2 ~tm in the porous and 3.8 ~tm
in the dense (greater than 98%) alumina. This is com-
parable with the grain size of the porous A1203 bodies
prepared with the coarse-grained A1203 powder.
3.2. Effect of metal ligament diameter
Representative micrographs of the m and c A1/AI 203
composites are provided in Figs. 3(a) and 3(b) respec-
tively. The pores were nearly fully infiltrated so that the
composite bodies had a porosity level of about 1%. The
microstructures display good homogeneity and are con-
sistent with the results of the narrow intrusion pore size
distribution. The intrusion pore sizes used to describe
Fig. 3. Optical micrographs of medium-grained (a) and coarse-
grained (b) AI/AI203 composites with 25 vol.% A1. The bright phase
is the metal, the dark phase the alumina grains.
the three porous Al203 bodies represent bottlenecks.
Average ligament diameters as measured from polished
sections give values which are about a factor of 5 higher
than the intrusion pore sizes. Nevertheless, irrespective
of the parameter used to characterize the scale, com-
parisons between different scale microstructures indi-
cate a true scale invariance.
TEM confirmed that the A1 Al203 interfaces were
well bonded in all three samples, and no interfacial
failures were observed in the approximately 30 50
metal-filled pores examined in each specimen. This is in
contrast to the observations in C u / A I 2 0 3 composites
prepared by gas pressure metal infiltration where micro-
cracking was observed at about 50% of interfaces in the
large-scale composite, but was not detected in the
smaller scale composites [31]. Representative bright
field micrographs are shown in Fig. 4(a)-(c). The pores
of the matrix are usually filled with single-crystal A1.
Microfaceting of the A1203 grains was found in all of
these samples, as is shown in Fig. 5. EELS spectra for
all three specimens investigated were identical within
statistical accuracy. Typical spectra are shown in Fig. 6.
The presence of the interface component and the
faceting (TEM) indicate that new interfaces have
formed, which suggests strong bonding between metal
and ceramic. The structure of the interface component
is being investigated further and compared with calcu-
lated spectra based on simple structural interface mod-
els.
Observations of fracture surfaces reveal scale invari-
ent metal deformation (Fig. 7(a) and (b)). The metal
ligaments neck to a point or ridge and cave out near the
interface. Little debonding is visible at AI A1203 inter-
faces. In contrast to the monolithic alumina, essentially
transgranular fracture of the A1203 grains can be ob-
served.
Fracture strength and fracture toughness (here
defined and reported as plateau toughness) values of
porous preforms as well as of the AI/AI2 03 composites
containing 25 vol.% metal are given in Fig. 8(a) and (b).
AI infiltration increases the fracture strength from val-
ues between 130 and 150 MPa for the porous preforms
to values from 510 to 710 MPa for the composites.
The maximum fracture strength occurs for the
composite with medium ligament diameter (Fig. 8(a)).
The fracture toughness (Fig. 8(b)) increases from
1.5 1 . 9 M P a m 1/2 for the porous alumina to 2.9
7.4 MPa m ~/2 for the metal-reinforced ceramics. Fur-
thermore, the fracture toughness of the composites
increases with increasing metal ligament diameter.
In stress intensity factor notation, the equilibrium
crack configuration with an applied stress intensity
factor KA, a crack length c, and dependent fracture
toughness KR(C) can be written as
 H. PHelipp et ell. /Materials Science and Engineering A 197 (1995) 19 30 23

Fig. 5. TEM image of AI20 ~ microledges at the A1 A120 ~ interface

(medium-scale microstructure, 25 vol.% metal).

ate for the respective crack configuration K~,i(c) can be

expressed as

K~,i(c) = g(c,r)pi(r)dr (3)

While the underlying description in Eq. (3) appears

very informative, it is not fundamental. The closure
stresses p(r) are a function of the crack opening dis-
placement (COD) 2u and will therefore change with
crack length (which will affect the local COD). The
notation of mechanical energy release rate G which
implicitly includes closure stresses as a function of
COD, may therefore be more applicable. The crack
resistance term R(c) is written as the sum of a crack tip
resistance term Ro and microstructural terms R~,,(c)
which, again in equilibrium, is balanced by GA:

GA = R0 q- Z R , , i ( c ) = R ( c ) (4)
i

I ' I ' I ' i I ,

5 Al203

4 ~nterlaceAI/AI203

g
3
x

2 ~'~ int~~ce~.~n~t x4
Fig. 4. Bright field TEM images of the (a) fine scale, (b) medium
scale and (c) coarse scale microstructures containing 25 vol.% A1.

-0 .J
KA = Ko + Y' K~,, (c) = KR(c) (2) 7o 8'o 9'0 1do 14 o 12o
i"
Energy Loss (eV)

The fi'acture toughness is seen as being composed of a
crack tip toughness term Ko and microstructural terms
K/,i(c), which sum up the closure stresses p,(r) of all
reinforcements with a weight function g(c, r) appropri-
Fig. 6. Typical electron energy-loss spectra of the AI L edge. By
subtracting the two reference spectra measured in the metal and in
the ceramic from the interface spectrum, the interface component is
obtained which contains information about the bonding between
metal and ceramic.
24 H. Prielipp rt al. / Materials Science and En#wering Al97 (1995) 19-30

Combining Eqs. (4) and (6), the fracture toughness at

the plateau of the R-curve KS,, given at a crack length
c,, where the first active bridge fails, can be written as

KS = ]Ki + EL RI,. matrix(c) + EL R,,, mrtaJ* (7)

where

K,, = (R, EL)!*

is the crack tip toughness of the composite.

SEM fracture surface observations reveal that in all
composites with metal content greater than 20 vol.%,,
alumina grains fracture essentially in a transgranular
manner. Transgranular as well as intergranular fracture
is observed only with a metal fraction of 10 vol.%.
Accordingly, the toughening contribution by grain
bridging can be neglected, and Eq. (7) can be reduced
to

K, = [K:, + KR,,. ,,,cta,(~)l~~ (9)

Furthermore, TEM and EELS investigations predict
strong AlPA120, interfaces independent of metal liga-
ment diameter. In addition, the metal reinforcements
exhibit scale invariant plastic deformation. Under the
assumption that the mechanical properties are also
independent of ligament diameter, the toughening con-
tribution of the ductile phase is only governed by
geometry, i.e. volume fraction and ligament diameter
given metal/ceramic system.
Fig. 7. Representative fracture surfaces of medium-grained (a) and
coarse-grained (b) AI!A120, composites with 25 vol.%, Al: I, AIZOq;
2, Al.

.*
R,,,(c) results from the J-integral formalism [36] (Eq.
(5)) where u* is the opening at the last active bridge: 800

R,,, = 2j;
s
0
I P,(u)du

The stress displacement function p(u) uniquely de-

600

400

scribes the reinforcement characteristics [18] and is 200

responsible for the increasing fracture resistance with
increasing crack length R(c). The toughening contribu- 0
tion by plastic deformation of the ductile phases is Porosity 25 vol-% Al 25 vol-%
governed by the mechanical properties of the metal, the
interface properties (debonding), the metal ligament
diameter and its volume fraction j In the case of
intercrystalline fracture of the matrix, interlocking
grains will remain in contact across the crack faces and
possibly form bridges providing additional crack clo-
sure stresses [37,38].
In the elastic case or elasticcplastic case under small-
scale yielding conditions, we can use the relation be-
tween applied stress intensity factor KA and mechanical
energy release rate G, (with EL Youngs modulus under
plane strain conditions): Porosity 25 vol-% Al 25 ~01-96

Fracture strength (a) and fracture toughness (b) of AI/AI,O,

composites with 25 vol.% metal and varymg hgament diameter com-
pared with the corresponding values for the porous preforms.
 H. Prielipp et al..' Materials Science and Engbteerh~g, A 197 (1995) 19 30 25

compared with an alumina prepared from fine-grained

A1203 powder of similar medium grain size. The frac-
ture strength decreases from 560 to 100MPa with
decreasing porosity (Fig. l l(a)) following an exponen-
tial relationship according to Rhyskewitsch [32]:
c~t.= ao e x p ( - n P ) (1)
where n is an adjustable parameter, P is the fractional
porosity and a0 is the fracture strength of the dense
alumina. It is interesting to note that the fracture
strength of A1 reinforced A12 03 is even higher than that
of dense alumina. In the range 10 25 vol.% A1, the
fracture strength reveals a constant value of about
700 MPa. With the metal fraction increasing from 25 to
40 vol.%, the strength increases approximately linearly
to 800 MPa.
The fracture toughness (Fig. l l(b)) decreases linearly
with increasing porosity from 3.6 to 0.8 MPa m 1'2 for
the alumina with 40% porosity. The fracture toughness
increases monotonically with increasing metal content,
up to 7 MPa m 1'2 at 40 vol.% A1. This is an improve-
ment of nearly 100% compared with the dense alumina.
c composites exhibit a similar trend, i.e. both the
fracture strength and fracture toughness are enhanced
(Fig. 12(a)) to 5 1 0 M P a (25vo1.% AI) and 650 MPa

Fig. 9. Optical micrographs of medium-grained AI/AI20 ~ composites

with (a) 10 vol.% and (b) 40 vol.% AI.

3.3. Roh, o f metal content

Optical micrographs of alumina with medium liga-

ment diameter infiltrated with 10 vol.% and 40 vol.%
aluminum are shown in Fig. 9(a) and (b). The mi-
crostructures are homogeneous and it appears that a
transition from islands of metal to islands of ceramic
takes place (at least in a two-dimensional view). The
average ligament diameter, as measured for polished
sections, is also approximately a factor of 10 larger
than the intrusion pore size (cf. Section 3.2). Fig. 10(a)
and (b) compares fracture surfaces of the microstruc-
tures shown in Fig. 9. At low metal contents the
ligaments deform by necking to a sharp point (separate
ligaments), while at higher metal contents deformation
to chisel edges (connected ligaments) takes place. For
composites with metal content greater than 20 vol.%,
fracture is essentially transgranular. With a metal con-
tent of 10 vol.% transgranular as well as intergranular
fracture was observed (Fig. 10(a)).
The results of fracture strength and fracture tough-
ness of the medium-scale materials vs. porosity and
volume fraction of A1 are shown in Fig. l l(a) and (b).
In order to minimize the influence of grain size on Fig. 10. Fracture surfaces of medium-grained AI/AI203 composites
fracture strength and toughness, the m composites are with (a) 10 vol.% and (b) 40 vol.% AI.
26 H. Prielipp et al. /Materials Science and Engineering A 197 (1995) 19 30

1000 r r
medium grained
0- porous "r
800 ~. coarse grained 650-+ 6(
800 [3 - i n f i R r a t e d
, ~ i ~,
rl
:E 600
t-

(-
400 .o,,o

....... "~. . . . . . ~ . . . . . . . . . . O" = 560 exp(-4 P) -

200
o -' / 7
dense 25 vol-% 35 vol-% 25 vol-% 35 vol-%
10 20 30 40
a) Porosity AI content
a) Porosity/AI content [vol-%]

12 10.5 +-0.7
8 Coarse grained
medium grained [ EL 10 / 7.40.5
O- porous /
D - infiltrated o_ 8 ~
0 i3!ii:ill
t~
[3
6 / 4.6t 0.5 iiiii!ii
D- m u~ i" / i;i~i~il;_
i
~ 4 1.St 0.2 1.5t 0.1 ~:~:~:~:~:
(,9
09
cm 2 / ::i:::i:::i:i
............ "~"..... 5"...........
~- 2 ~- 0
CO
dense 25 vol-% 35 vol-% 25 vol-% 35 vol-%
o
i i i i
0
b) Porosity AI content
o 10 20 30 40

b) Porosity/AI content [vol-%] Fig. 12. Fracture strength (a) and fracture toughness (b) of A1/AI20~
Fig. 11. Fracture strength (a) and fracture toughness (b) of AI/AI303 composites with coarse ligament diameter and varying metal content
composites with medium ligament diameter and varying metal con- compared with the corresponding values of the porous preforms.
tent compared with the corresponding values for the porous pre-
forms. as grains can reinforce a ceramic matrix by providing
closure stresses in the crack wake shielding the crack tip
(35volY0) and to 7 . 4 M P a m ~/2 (25vo1.% AI) and from the applied stress. Process zone shielding [33] and
10.5 MPa m 1/2 (35 vol.% ) (Fig. 12(b)). The strength and crack deflection [34] are further possible mechanisms;
toughness of monolithic alumina with a grain size of however, they have only small toughening potential in
4 mm decreases with increasing porosity from 370 MPa these composites when compared with crack bridging
for the dense alumina to 70 MPa for coarse-grained [8,35].
alumina with a porosity of 35% and from 4.6 to
1 . 5 M P a m ~/2 respectively. In comparison with the 4.2. Long crack toughness
dense alumina, the A1 reinforcement yields an improve-
ment in strength and toughness of more than 100%. Observations on fracture surfaces of different scale
Independent of metal ligament diameter, the Young microstructures point to scale invariant metal deforma-
modulus decreases from 260 GPa to 230 GPa for 25
and 35 vol.% AI respectively. Poisson's ratio remains
roughly constant at 0.28. With E = 400 GPa for alu-
mina, E = 70 GPa for A1 and a Poisson's ratio of 0.28
for both, the Young modulus can be evaluated for all O"
the composites, using the arithmetic median of Paul's
lower and upper Young's modulus of the composite.
The computed data show a relatively good agreement
with experimental measurements. crack

4. Discussion
(I
~iiiY
4.1. Fracture mechanics
Fig. 13. Schematic diagram showing possible crack bridging mecha-
Possible reinforcement mechanisms in metal ceramic nisms in metal ceramic composites: bridging by ductile phases (1) and
composites are shown in Fig. 13. Ductile phases as well bridging by matrix grains (2).
 H. Prielipp et al. Materials Science and Engineering, A 197 (1995) 19 30 27

_rntai,,x[
metal is a linear function of volume fraction 1/1 as well
as of metal ligament diameter d owing to the mi-
crostructural scale invariance of plastic deformation.
crac~ This implies according to Eq. (9) that variations in
fracture toughness with metal content should obey a
square root dependence on Vf for a given microstruc-
tural scale of the metal phase. Fig. 15 demonstrates
good agreement between theory and experiment, except
medium coarse
for the coarse-grained composite with a metal content
a) of 25 vol.%. In order to estimate R~...... ,,~ from Eq. (5),
the p(u) function was assumed to be constant up to a
m a x i m u m crack opening where the first ligament fails.
According to literature results [10] this opening is about
C
P R .**/o.-- ........ the same size as the ligament diameter, which in turn
,." m can be estimated from optical micrographs to be

f roughly a factor of 5 larger than the pore channel size

measured with mercury porosimetry. Thus the solid
lines of Fig. 15 correspond to ligament diameters of 0.4,
1.25 and 4 jam. Combining Eqs. (9) and (5) results in a
U closure stress for the AI of 400 MPa, which exceeds the
b) c) yield stress of pure AI by an order of magnitude. The
Fig. 14. Schematic diagram describing p(u) functions (b) and R- authors relate this fact to the constrained plastic defor-
curves (c) for metal reinforced ceramics with varying ligament diame- mation as well as the minute microstructural scale of
ter (a), based on the assumption of scale independent metal the single-crystal ligaments.
deformation.

4.3. Composite .fracture strength

tion and debond lengths. Consequently, p(u) functions
can be derived from one assumed function and trans- The increase in fracture strength with metal content
formed into another microstructural scale simply by may seem surprising at first, since AI has a yield
stretching the crack opening parameter in accordance strength much below the strength of alumina, thus any
with the ligament diameter (Fig. 14). Large reinforce- rule of mixture does not apply. To understand the
ments will therefore lead to smaller crack closure strength of metal/ceramic composites, one needs to
stresses at given small COD, which will be maintained appreciate that, in interconnecting networks, the ce-
up to higher crack opening displacements. This will ramic provides the failure site at the largest flaw, and
result in R-curves for large reinforcements which can be the metal provides the fracture toughness. In the fol-
characterized by small initial slope with a high peak lowing sections, qualitative descriptions are provided
thoughness. Therefore, the long-crack fracture tough- for trends of composite strength, with the assumption
ness (as measured by SEPB) will increase with ligament that the initial flaw size of the porous alumina is the
diameter. same as that of the respective composite.
The SEPB method yields fracture toughness values
for bridged cracks of lengths between 200 and 400 jam,
which for our materials is near the plateau of the 12
R-curve and can therefore be represented by Eq. (9). &- small I
- medium I ~
The crack tip toughness Ko can be determined by a
-e ~ EqarSe ~ _ m
procedure [18] which relies on a measurement of near m 8
0-
crack tip opening displacements and use of the crack
/) 6
profile description of Barenblatt [39]. A crack tip /)
toughness of 2 . 0 M P a m 12 for A1/A1203 composites o~
c- 4
,=
produced by direct metal oxidation has been estim- c~
"~ 2
ated [40] which can be compared with values of o
I-
2.0 MPa m ','2 for alumina [18]. Fig. 15 shows the results 0
of the fitting procedure according to Eq. (9), taking Ko 0 10 20 30 40
as 2.0 MPa m ~'2 for all composites and assuming that AI content [vol-%]
crack bridging is due to ductile reinforcements only Fig. 15. Influence of metal ligament diameter and volume fraction on
(Section 4.2). The sole assumption required is that the steady state toughness of AI/AI20~ composites. Full lines are repre-
fracture energy contribution R t..... lal of the ductile sentations of Eq. (9).
28 H. Prielipp et al. / Materials Science and Engineering A 197 (1995) 19 30

Gm Gs Gc
G,R ..... //
// ////
G, R ~ " " increased metal
............ /,.::~<:'.:~........................... a c // ...../~, "/ ..,, . / ~ " fraction
// //].~#~"

,~! ........~>..,'
.,"/ Rm
/ /-~ /

.....' .";'::!';;;"
......., " "~.~:.......................................
Rs
y('*
/ " ,.,;.S,I ,,** ....::..::-IS .....
IL

C C
Fig. 17. Schematic diagram describing R-curves of metal reinforced
Fig. 16. Schematic diagram describing R-curves of metal reinforced
ceramics with varying metal content. The tangency condition of the
ceramics with varying metal ligament diameter. The tangency condi-
applied energy release rate GA (straight, dashed lines) with the
tion of the applied energy release rate GA (straight, dashed lines) with
R-curves yielded the respective instability points.
the R-curves yields the respective instability points.

4.3.3. Effect of flaw bridging

4.3.1. Effect of metal ligament diameter
Our qualitative considerations describe only the
In describing the fracture strength, the actual slope
trend of strength as a function of ligament diameter as
of the R-curve, as well as the initial flaw size, are
well as of volume fraction. Assuming the same initial
important factors. Inserting the values for toughness,
flaw sizes for the composites as for the corresponding
as measured with SEPB, and strength in Griffith's
porous alumina, the instability criterion (tangency con-
equation and solving for the crack length yields almost
dition of the applied stres intensity factor with R-
identical flaw sizes for the s, m and c alumina with
curve) predicts an enhancement of the composite
25% porosity. In the schematic diagram in Fig. 16,
strength directly proportional to the fracture toughness
identical initial flaw sizes are therefore used for all
at the instability crack length. This statement is consis-
composites. The c composite exhibits a rather shallow
tent with the initial modeling from Bao and Zok [21].
R-curve so that crack instability occurs with a large
Quite on the contrary, however, our results show a
degree of stable crack growth; hence in spite of a large
larger enhancement of strength than of toughness ow-
plateau toughness the strength is rather low. The fine-
ing to metal infiltration, as demonstrated in Fig. 18 by
grained micostructure exhibits only a very small R-
the mechanical property data normalized to the data of
curve height, so that the increase in strength is not as
the porous preform.
dramatic. Conversely, the m material appears to com-
The above model assumes that the initial flaw is not
bine initial flaw size and slope of the R-curve most
bridged by the ductile phase. Based on investigations
favorably and therefore has the highest fracture
on the fracture strength of alumina [24], where the
strength of 710 MPa.
largest pore determines the failure origin, we assume
Due attention must be paid to the scale of the initial
that the site of the initial flaw remains unchanged but is
flaw size. In cases where this parameter is increased (as
converted to a metal filled cavity. Therefore the crack is
in thermal shock), the large-scale microstructure may
initially bridged by metal with a volume fraction fb of
prove to be advantageous compared with the fine- or
medium-scale counterparts [41].
10
medium grained .o
4.3.2. Effect of metal content ~8 - Strength ..
[] - Toughness O' El
A large metal content results from a preform
/' " "
with high porosity. In applying the Griffith equation,
. .O" . ..,,D
it appears that the initial flaw size increases with
....O ...... .. ....
increasing porosity. Depending on the exact inter-
action of initial pore size and slope of the R-curve, ~( ~ 2 ,:::: ::::::? ......
an increase or decrease in strength with metal content
may result. In the case of AI reinforcement, the R- 10 20 30 40
curves are steep enough to compensate for the small AI content [vol-%]
increase in initial flaw size and therefore yield an in-
crease in strength with increasing metal content as Fig. 18. Effect of AI content on the relative enhancement of the
composite strength and toughness. The composite properties were
shown schematically by the tangency condition in Fig.
normalized to the corresponding values for the porous alumina
17. preforms.
 H. Prielipp et al./ Materials Sciem'e and EnghwerhTg A 197 (1995) 19 30
metal
finitial : fb = 1 0 0 %
fb = F(C) > f
1 1
fb = f = const.
C ness of one sample microstructure and then scaling the
Fig. 19. Hypothesis for crack initiation in metal/ceramic composites
where failure-causing pores are eliminated and failure initiates at
large metal filled cavities.
100% (Fig. 19(a)). As the crack extends into the matrix,
it will consecutively encounter an increasing number of
metal ligaments (Fig. 19(b)). If the crack length is large
with respect to the metal filled cavity, the metal bridg-
ing fraction is constant (f, = J ) (Fig. 19(c)). Inclusion of
the change in metal volume fraction leads to a modifi-
cation of Eq. (5), where now f has to be replaced by
f(c):
ti*
R,,= 2f(c)
Ij pi(u)du
The foregoing discussions on the influence of the matrix
(10)
on fracture are therefore still valid, but have to be
augmented by the closure effect of the large metal filled
pore. In addition, the initial slope of the R-curve is
steeper than that of a long-crack R-curve (Fig. 20(a)
and (b)). This qualitative description, by separating
small- and long-crack fracture toughness, can explain
the fact that the composite strength increases more than
the (measured) long crack fracture toughness would
predict (tangency condition in Fig. 20(b)).
5. Conclusion
A1/AI203 composites can be produced with widely
differing microstructures (especially metal volume and
metal ligament diameter) by gas pressure metal infiltra-
29
long crack small crack
G, R ,/' G,R .
/,/'/
// /
a) c b) c
Fig. 20. R-curves (a,b) explain schematically the short crack
anomaly (b) compared with long crack behavior (a).
tion into tailored porous preforms. These materials
exhibit fracture toughnesses up to 10.5 MPa m j'2 and
fracture strength up to 810 MPa. In contrast to metal
matrix composites (e.g. [42]), both the fracture strength
and fracture toughness are increased with second phase
content. TEM and EELS characterization show contin-
uous, microcrack-free bonds in all composites of vary-
ing microstructural scale. Long-crack fracture tough-
ness data can be inferred by using the plateau tough-
toughness with respect to ligament diameter and metal
volume, where the observation of scale invariant plastic
deformation is utilized. Trends in fracture strength as a
function of metal content and metal ligament diameter
can be explained. A striking result, however, is the fact
that the fracture strength increases more pronouncedly
by metal infiltration than the plateau toughness derived
from long crack measurements. This fact is attributed
to large closure stresses during and after crack initia-
tion at metal filled cavities associated with plastic defor-
mation of these large metal spheres.
Acknowledgements
We thank Maria Sycha for preparing the TEM spec-
imens and Christina Scheu for performing part of the
experiments and analysis. S.K.S. wishes to thank the
Alexander von Humboldt-Stiftung for financial sup-
port. This work was supported by the Deutsche
Forschungsgemeinschaft under contract number Ro
954/1-1 and the Volkswagen Foundation under con-
tract number 1/66 760.
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