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J. Am. Ceram. Soc.

, 92 [5] 1087–1092 (2009)

DOI: 10.1111/j.1551-2916.2009.03036.x
r 2009 The American Ceramic Society

Processing of Oxide Composites with Three-Dimensional
Fiber Architectures
James Y. Yang, Jared H. Weaver, and Frank W. Zokw
Materials Department, University of California, Santa Barbara, California 93106

Julia J. Mack
Teledyne Scientific Company, Thousand Oaks, California 91360

Fabrication of oxide fiber composites is accompanied by the fiber preform. Even with multiple infiltration cycles, the me-
development of drying cracks in the matrix following slurry in- chanical integrity of the resulting matrices is inferior to that of
filtration. The cracks are a result of the inherent shrinkage in monolithic ceramics. Consequently, matrix-dominated compos-
particle compacts during drying coupled with the mechanical ite properties rarely achieve their full potential.
constraints imposed on the matrix by the fibers. The effects are (iii) When slurry infiltration is used, shrinkage of the green
most pronounced in systems with three-dimensional fiber archi- matrix during drying coupled with the constraints imposed by
tectures. A mitigation strategy based on the addition of coarse the fibers invariably lead to the formation of matrix cracks
matrix particles to the fine particulates has been devised and with large opening displacements (ca. 10 mm).13–15 Once formed,
demonstrated. Among the various implementation strategies ex- these cracks are irreparable by subsequent impregnation and
plored, the most effective involves combining the two particle pyrolysis of ceramic precursor solutions. Their presence has im-
types (coarse and fine) into a single slurry and coinfiltrating the plications in hermeticity, thermal conductivity, and matrix-
slurry through sequential vibration- and vacuum-assisted pro- dominated mechanical properties. Additionally, when subjected
cesses. Regardless of the infiltration route, the SiC particles to thermal gradients, the cracks produce nonuniform tempera-
have no apparent detrimental effect on the fiber bundle proper- ture distributions which can, in turn, lead to further matrix
ties. Additionally, they increase the through-thickness thermal damage.16 Strategies for the mitigation of these cracks is the
diffusivity by 50%–100%. focus of the present article.
The nature of the cracking problem is illustrated in Fig. 1.
The figure shows a typical cross-section through an oxide CFCC
I. Introduction with Nextel 720t fibers in an 8-harness satin weave (8 HSW)
and a mullite/alumina matrix. (Processing details are summa-
C ONTINUOUS fiber ceramic composites (CFCCs) with two-di-
mensional (2D) fiber architectures are vulnerable to delam-
ination when subjected to out-of-plane thermal or mechanical
rized in a subsequent section.) Drying cracks are oriented in the
through-thickness direction, i.e., crack plane normals lying in
stress.1–7 The vulnerability is particularly acute in composites the plane of the fiber weave. Similar cracks have been observed
with porous matrices.1,2,5,7 One obvious remedy is to incorporate in virtually all oxide CFCCs with 2D architectures.13,14,17–22
fibers in the third (out-of-plane) direction. Indeed, the use of this Cracks are not formed in-plane because of the absence of
reinforcement strategy has impressive precedents in polymer– through-thickness constraint.
matrix composites reinforced by glass and carbon fibers.8–12 Drying cracks are inherently more problematic in 3D CFCCs
Implementation of this strategy for CFCCs, however, presents because of the additional constraint imposed by fibers in the
unique fabrication challenges: third principal direction. Figure 2 shows an example of a com-
(i) Weaving complex architectures with ceramic fibers is posite with a 3D orthogonal weave of Nextel 720t fibers and the
problematic because of the high stiffness of these fibers, espe- same mullite/alumina matrix. In this case, the through-thickness
cially relative to that of glass. Nevertheless, with appropriate drying cracks are somewhat longer than those in the 2D material
handling precautions and attention to architectural design, the (because of the larger intertow spaces) and exhibit larger open-
weaving problems can be overcome. Indeed, the preforms used ing displacements. In-plane drying cracks are also evident. These
in the present study (detailed below) were of exceptional quality are concentrated near the panel mid-plane but are also present
with minimal fiber damage. along fiber tow/matrix boundaries at other through-thickness
(ii) Processing of ceramic matrices usually involves some
combination of chemical vapor infiltration, particle slurry infil-
tration and precursor solution impregnation and pyrolysis (the
notable exception being melt infiltration of Si alloys into SiC
fiber-reinforced systems). Each of these routes on its own is ca-
pable of only partially filling the available void space within the

R. Hay—contributing editor

Manuscript No. 25363. Received October 15, 2008; approved February 11, 2009.
This work was financially supported by the U.S. Air Force Research Laboratory
through a subcontract from Siemens Power Generation (award number 442490–59855,
monitored by Drs. M. Cinibulk and G. Fair at AFRL and Drs. J. Lane and G. Merrill at Fig. 1. Backscatter electron image of a composite with a mullite/
Siemens) and the Air Force Office of Scientific Research (award number F49550-05-1-0134, alumina matrix and NextelTM 720 fibers in an 8-harness satin weave.
monitored by Dr. B. L. Lee).
Author to whom correspondence should be addressed. e-mail: zok@engineering. Drying cracks are oriented in the through-thickness direction, perpen- dicular to the plane of the fibers.
1088 Journal of the American Ceramic Society—Yang et al. Vol. 92, No. 5

and spherical particles of radius R, the unconstrained shrinkage

strain would be t/R. Particle rearrangement during drying may
lead to additional shrinkage. The implication is that, provided
t is independent of R, shrinkage can be reduced by use of larger
The requirements that the particles be large enough to reduce
the shrinkage to an acceptable level yet small enough to pene-
trate between the fiber tows indicate a need for a bimodal size
distribution: coarse particles for filling the large intertow spaces
and fine ones for infiltration both into the fiber tows and be-
tween the coarse particles. But, even with a bimodal distribu-
tion, the size of the coarse particles is limited by the size of the
channels available for transport between tows (typically, B100
mm). Provided the concept is implemented properly, only the
fine particulates will be present within the tows and hence the
fiber bundle properties should be unaffected by the presence of
the coarse particles.
A secondary benefit of the bimodal distribution is an en-
hancement in the efficiency of particle packing within the large
matrix pockets.24 As a consequence, if subsequent matrix dens-
Fig. 2. (a) Extensive matrix cracking in an as-processed three-
ification is desired, less additional material is required to achieve
dimensional oxide continuous fiber ceramic composites. (b)–(c) In- the targeted density. But, as demonstrated by porosity measure-
plane drying cracks resulting from the constraint of the Z-yarns. (Fiber ments presented below, this benefit is small (about 3%).
weave illustrated in Fig. 4.)

locations. The latter cracks (not present in the 2D weave) are III. Implementation Via Vacuum-Assisted Infiltration
attributable to the constraint imposed by the through-thickness
The preceding concept was implemented using an established
vacuum-assisted slurry infiltration method, described else-
Two strategies for mitigating drying cracks have been pro-
where13,14,21 and summarized in the flowchart in Fig. 3 (along
posed. The first is to fill the large matrix-rich pockets between
route labeled I). The baseline method begins with preparation of
tows with high aspect ratio chopped fibers. In one implementa-
a dispersed slurry of B1 mm mullite (MU-107, Show Denko
tion, 2D cloths were coated with a paste of chopped alumina
K.K., Tokyo, Japan) and 0.2 mm alumina particulates (AKP-50,
fibers before stacking the cloths and infiltrating the matrix con-
Mitsui Mining Co., Tokyo, Japan), in a ratio of 4:1 (by volume),
stituents.13 Although somewhat successful in reducing the pro-
and with a total solids loading of 30% in deionized water. Nitric
pensity for matrix cracking, the use of pastes in this manner
acid was added to achieve a pH of 3, thereby assuring a well-
is inherently restricted to 2D laminates. This approach also re-
dispersed slurry. Agglomerates were broken down through a
duces the fiber content that can be achieved. The second is based
combination of stirring and ultrasonication for about 1 h. The
on freeze-drying. Specifically, the slurry carrier fluid is frozen
slurry was poured onto the preform, vacuum degassed, and then
immediately after infiltration into the fiber preform and re-
infiltrated via a vacuum-assisted process. Once infiltration was
moved by sublimation.23 Cracking is prevented because of the
complete (typically 3–4 h), the green composite was dried and
absence of capillary forces during carrier removal. Although
fired in air in a box furnace (1 h at 9001C). With the mullite/
some encouraging progress has been made using camphene as
alumina proportions used here, the mullite particles form a con-
the carrier fluid (selected for its high sublimation temperature), a
tiguous network that inhibits densification during subsequent
critical assessment of the viability of this route for fabrication of
oxide CFCCs has yet to be performed.
The objective of the present article is to present an alternate
strategy for mitigating shrinkage cracks in 3D CFCCs. Two as-
pects of the fabrication process feature prominently: (i) incor-
poration of coarse (410 mm) matrix particles in addition to the
smaller particulates (r1 mm); and (ii) use of vibration to facil-
itate infiltration. Secondary goals include identifying possible
fiber degradation mechanisms associated with the processing
route and probing the effects of the coarse particles on through-
thickness thermal diffusivity.
The remainder of the article is organized in the following way.
First, the rationale for combining coarse and fine particles in the
matrix is described. Then, an assessment is made of the efficacy
and the deficiencies of coinfiltration of these particles into fiber
preforms using an established vacuum-assisted route. With lim-
itations of the vacuum-assisted route exposed, an augmentation
based on vibration-assisted infiltration is devised and demon-
strated. Finally, measurements of the in-plane tensile properties
and through thickness diffusivity are presented.

II. Strategy for Crack Mitigation

The distribution of matrix particle size plays a central role in
controlling drying shrinkage. Following infiltration of a dis-
persed slurry into a fiber preform, the matrix particles remain Fig. 3. Flowchart summarizing the standard processing method (route
surrounded by the dispersing liquid, even at points of particle I) and those used to incorporate coarse SiC particles (routes II–IV). M,
contact. Assuming a liquid layer of thickness t at the contacts mullite, A, alumina.
May 2009 Processing of Oxide Composites with Three-Dimensional Fiber Architectures 1089

heat treatment whereas the alumina particles form sintered

bridges between neighboring mullite particles. For additional
matrix strengthening, the composite was impregnated with an
alumina precursor solution (aluminum hydroxychloride) and
pyrolyzed in air (2 h at 9001C). In the present implementation,
the precursor solution concentration was selected to produced a
mass yield of 8% alumina after pyrolysis (higher concentrations
producing solutions with unacceptably high viscosity25). Two
precursor impregnation and pyrolysis cycles were used. The
plates were subjected to final heat treatment of 2 h at 12001C
in air. The heating and cooling rates were 101C/min for all heat
To assess the efficacy of large matrix particles in mitigating
cracks, SiC particles (Norton Company, Worcester, MA) with
an average size of 1373 mm (500 grit) were added to slurries
with a 4:1 mullite/alumina ratio and the same processes used for
slurry infiltration and subsequent matrix strengthening (route
IV in Fig. 3). The SiC content was selected to ensure that all of
the intertow interstices could be filled. The total solids content
was initially set at 30 vol% (the same as that of the mullite/
alumina slurries), although slight variations were explored, as
described below. The initial assessment was made using a seven- Fig. 4. Three-dimensional orthogonal weave used in the present study.
layer stack of 3000 denier 8 HSW Nextelt 720 cloths (3M Top, perspective schematic; Bottom, plan view of preform. Weave con-
Company, St. Paul, MN), about 3 cm  9 cm and 3 mm thick. sists of six layers of straight warp yarns, seven layers of straight fill yarns
The same process was then applied to comparably-sized pre- and interlacing Z-yarns. Fiber volume fractions: 12.5% warp, 12.4%
forms of the 3D orthogonal weave illustrated in Fig. 4. weft, 4.2% Z-yarns (d, denier; ppi, picks per inch; epi, ends per inch; dpi,
Polished cross-sections through a series of 8 HSW composites dents per inch). Weaving by 3TEX, Cary, NC.
are presented in Fig. 5. The particles filled virtually all of the
intertow spaces. Additionally, these regions were devoid of dry- the SiC-containing composites was slightly reduced, from 2.8 to
ing cracks, consistent with the improvement expected from in- 2.65 g/cm3, a result of the lower mass density of SiC relative to
creased particle size. In regions where packing of the SiC was the oxide constituents.)
not complete, drying cracks were present, but exhibited lower Upon closer inspection of the cross-sections, subtle differ-
opening displacement than that in the SiC-free composites. The ences are evident in the packing efficiency of the mullite/alumina
mitigation of matrix cracking is directly attributable to the role particulates. Using slurries with comparatively high solids load-
of the coarse SiC particles in reducing the (unconstrained) dry- ing (35%), the oxide particles pack exceptionally well between
ing shrinkage. A secondary benefit derived from combining the SiC particles in the matrix-rich regions but experience some
coarse and fine particles was a slight increase in the packing difficulty in penetrating the spaces between fibers, manifested
density of particles in the matrix-rich regions. The latter effect as fine intratow pores. Evidently the degree of this porosity di-
was inferred from measured porosities: 22.5%70.5% and minishes as the slurry solids loading decreases. Concurrently,
19.0%70.8% for the SiC-free and SiC-containing composites, however, the efficiency of packing of the oxide particulates be-
respectively. (Despite the improved packing, the bulk density of tween the SiC particles decreases slightly, resulting in increased

Fig. 5. Effects of solids loading on particle packing in the two-dimensional (8-harness satin weave) fabric. The particles had been coinfiltrated by the
vacuum-assisted route. Drying cracks are almost completely eliminated in all cases. Subtle changes in inter- and intratow porosity are evident.
1090 Journal of the American Ceramic Society—Yang et al. Vol. 92, No. 5

Fig. 6. Vacuum-assisted coinfiltration of the mullite/alumina/SiC slurry

into the three-dimensional preform. Inset shows section orientation with
respect to the fiber weave.

intertow porosity. An optimal condition appears to be obtained

for solids loading in the range 28%–30%. Although the mech-
anisms associated with the formation of these defects and their
dependence on solids loading are not presently understood, no
additional effort was made to probe them further, largely be- Fig. 7. Two orthogonal sections through a three-dimensional preform
cause of problems encountered in fabricating 3D CFCCs with following vibration-assisted infiltration of SiC slurry (without mullite/
this route (described below) as well as the rather low ‘‘concen- alumina) and epoxy impregnation. Light gray regions are SiC.
tration’’ of such defects.
Use of the same vacuum-assisted coinfiltration procedure
The second alternative (route III in Fig. 3) was essentially
with the 3D preform proved partially successful (Fig. 6); only
a hybrid of routes II and IV in the sense that it involved coin-
about half of the intertow volume was filled with SiC particles.
filtration of all particles and used vibration to facilitate infiltra-
Incomplete infiltration is attributable to two related factors.
tion. In this case, a slurry containing the desired mix of mullite,
First, although in principle slurry infiltration is not a line-
alumina and SiC was poured onto the preform and degassed,
of-sight deposition process, the large size of the SiC particles
and the assembly then vibrated for about 20 min. This was
prevent them from remaining suspended in solution for time
followed by vacuum-assisted infiltration, drying, firing and
periods needed for infiltration. As a result, there is a greater
strengthening with the precursor-derived alumina. This process-
tendency for the particles to settle into positions directly beneath
ing route proved to be the most effective and reproducible.
their settling trajectory. Secondly, shadowing effects in the 3D
Regardless of their size, the SiC particles packed well within the
preform (especially those associated with the crowns of the
intertow spaces while the mullite and alumina particles infil-
Z-yarns) are more pronounced than those in the 2D fabric.
trated virtually all of the fine interstices both in the SiC-rich re-
Notwithstanding these limitations, matrix cracking had been
gions and within the fiber tows (Fig. 10). Consequently, the level
suppressed in the SiC-rich regions. The inference is that the
of extraneous porosity (caused by poor packing) and the degree
cracking could be further reduced if the SiC particles were to
of cracking were minimal.
completely infiltrate all available space.
A further assessment of the efficacy of the SiC particles in
producing high quality matrices was made by producing com-
posite panels following an identical vibration- and vacuum-
IV. Vibration-Assisted Infiltration assisted process, but using only the oxide particulates. In this
case, there was no apparent benefit of the vibration in suppress-
Two alternatives were devised to enhance space filling by the SiC ing cracking (Fig. 11). This result reaffirms that the reduced
particles. In the first (route II in Fig. 3), infiltration was initially propensity for cracking in the preceding cases is indeed due to
performed with only SiC in the slurry. After pouring the slurry the presence of the coarse SiC particles; using vibration with
onto the preform and degassing, the infiltration fixture was only fine particulates does not yield an improvement.
placed on a commercial vibrating table (78-RK Vibrator, Han-
dler Mfg. Co., Westfield, NJ) for about 20 min. Visual inspec-
tion revealed that, during this period, virtually all SiC particles
had settled. Furthermore, the thickness of the SiC cake on top of
the preform remained unchanged for the last 10 min of vibra-
tion, indicating that the infiltration process had gone to com-
pletion. Following drying of the SiC/fiber preform under a heat
lamp, the mullite/alumina matrix was vacuum infiltrated and
strengthened with the alumina precursor solution (route I in
Fig. 3). In some cases, the green SiC/fiber preform was infil-
trated with a low viscosity epoxy, for subsequent sectioning
and polishing and assessment of the SiC particle distribution.
Experiments were conducted with particle ranging ranging in
average size from 9 to 30 mm (600–320 grit).
Vibration assistance proved to be extremely effective in pack-
ing the SiC particles into all large intertow spaces (Fig. 7),
regardless of particle size. Subsequent infiltration of the mullite/
alumina slurry, however, was problematic in cases where smaller
SiC particles (r17 mm diameter) had been used. Evidently the Fig. 8. Three-dimensional continuous fiber ceramic composites pro-
tight packing within the SiC/fiber preform prevents ingress of the duced by vibration-assisted infiltration of 23-mm-diameter SiC particles
mullite/alumina slurry. In contrast, infiltration of the mullite/ followed by vacuum infiltration of the mullite/alumina slurry. Dashed
alumina slurry was largely successful with the coarser SiC par- lines in (b) and (c) denote boundaries between weft tows and adjacent
ticles (  23 mm diameter), as illustrated in Figs. 8 and 9. matrix-rich pockets.
May 2009 Processing of Oxide Composites with Three-Dimensional Fiber Architectures 1091

Fig. 11. All-oxide three-dimensional composite fabricated by sequen-

tial vibration- and vacuum-assisted slurry infiltration of the mullite/al-
umina slurry.

tests were performed in an Ar atmosphere (because the graphite

coating oxidizes B6001C). Measurements were made on the 2D
Fig. 9. (a) Three-dimensional continuous fiber ceramic composites pro- and 3D composites both with and without SiC particles, up to
duced by vibration-assisted infiltration of 30 mm diameter SiC particles
followed by vacuum infiltration of the mullite/alumina slurry. (b, c)
temperatures of 10001–12001C.
Higher magnification images of regions indicated in (a). The test results are summarized in Fig. 12. With the 2D ar-
chitecture, the addition of the coarse SiC particles yielded an
elevation in diffusivity of about 50% over the entire temperature
V. Property Assessment
range. The magnitude of the elevation was even greater in com-
A preliminary assessment was made of the fiber bundle strength posites with the 3D weave: almost 100% at ambient tempera-
in the 3D CFCCs, with a view to identifying possible degrada- ture, diminishing to about 60% at 10001C.
tion mechanisms associated with SiC infiltration (caused by
abrasion of the fiber surfaces during vibration). Because of lim-
ited material volume, tensile tests were performed on hourglass- VI. Conclusions
shaped specimens. Each specimen had a gauge width of 9 mm
and a radius of curvature of 75 mm. Test specimens included The addition of coarse matrix particles to the fine particulates
ones with and without SiC particles and tested in both principal normally used for oxide CFCCs is effective in mitigating drying
fiber directions. From about ten such tests, the average fiber cracks. The two particle types can be coinfiltrated into 2D fiber
bundle strength (taken as the ratio of composite strength to the
fiber volume fraction aligned with the loading direction) was 1.6
780750 MPa. This range is comparable to that obtained with
(a) 8 harness satin weave
the same fibers in the 8 HSW weave (690760 MPa).26 There 1.4
Thermal diffusivity (10–6m2/s)

was no apparent detrimental effect of the SiC particles.

The through-thickness thermal diffusivity was measured us- 1.2
ing the laser flash method with a Netzsch Instruments Laser
Flash Apparatus 427. Circular samples, 12.6 mm in diameter,
were cut from the composite panels using a core drill. A thin 0.8 With SiC
graphite coating was applied to the broad surfaces in order to
increase opacity and enhance absorption of the laser on the in- 0.6
cident face. To enable measurements at high temperatures, the
Without SiC

0 200 400 600 800 1000 1200 1400
Temperature (°C)

(b) 3D orthogonal weave
Thermal diffusivity (10–6m2/s)


With SiC


0.4 Without SiC


0 200 400 600 800 1000 1200 1400
Temperature (°C)
Fig. 10. (a) Coinfiltration of 23-mm-diameter SiC particles and mullite/ Fig. 12. Effects of fiber architecture and presence of coarse SiC parti-
alumina mixture by sequential vibration- and vacuum-assisted infil- cles on through-thickness thermal diffusivity of (a) 2D and (b) 3D
tration. (b, c) Higher magnification images of regions indicated in (a). composites.
1092 Journal of the American Ceramic Society—Yang et al. Vol. 92, No. 5
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