Fusion Engineering and Design 83 (2008) 713–719

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Fusion Engineering and Design

journal homepage: www.elsevier.com/locate/fusengdes

Polymer impregnation and pyrolysis process development for improving

thermal conductivity of SiCp/SiC–PIP matrix fabrication
S.G. Lee ∗ , J. Fourcade, R. Latta, A.A. Solomon
School of Nuclear Engineering, Purdue University, West Lafayette, IN 47906, USA

a r t i c l e i n f o a b s t r a c t

Article history: The polymer impregnation and pyrolysis (PIP) method is optimized to consolidate particulates, and to
Received 9 July 2006 produce a continuous SiC network to yield high thermal conductivity monoliths from particulates. The
Received in revised form 29 January 2008 process as presently employed, consists of impregnating a polymeric precursor into a cast sample or a
Accepted 17 April 2008
pressed pellet, pyrolyzing, and crystallizing at high temperature to a final form. The use of gas pressure
Available online 30 June 2008
in the polymer impregnation step was found essential to improve the density of the matrix, provided
that the nature of the gas and the pressure applied were optimized. Thermal conductivity of this matrix
Keywords:
indicated that higher crystallization temperatures improve the conductivity by removing impurities and
SiC
Consolidation increasing crystallite size. The impregnation process also permits bonding of solids to produce complex
Thermal conductivity engineering shapes if high temperature crystallization is possible.
Polymer impregnation and pyrolysis © 2008 Elsevier B.V. All rights reserved.
Bonding

1. Introduction should undergo isotropic dimensional changes under irradiation

SiC has the advantages of stability in severe environments, lack
of reaction with zircaloy up to 1773 K, high thermal conductivity,
low neutron absorption, radiation stability, and compatibility with
many oxides up to reasonably high temperatures [1,2]. Due to its
good thermo-mechanical properties, SiC was tested as a structural
material for fusion reactors [3], and considered as a candidate for
inert matrix fuel (IMF) and for PWR oxide fuel with enhanced ther-
mal conductivity [4]. However, the fabrication of dense SiC bodies
cannot be easily obtained through conventional powder sintering
techniques because of oxidation reactions that occur above a cer-
tain temperature. Dense SiC can only be obtained by high isostatic
pressing (HIP) and/or sintering at very high temperature under
controlled atmosphere.
An alternative route to produce relatively dense SiC bodies is
to use the polymer impregnation and pyrolysis or PIP process. PIP
is widely used to consolidate ceramic matrix composites, and to
join ceramic pieces since it produces a relatively dense SiC phase at
lower temperatures [5–11]. The PIP process is simple to employ, and
yields high purity ␤-SiC which has a cubic crystal structure which
∗ Corresponding author. Present address: R&D Center of Samsung Engineering Co.
Ltd., 415-10, Woncheon-Dong, Youngtong-Gu, Suwon-City, Gyounggi-Do 443-823,
Republic of Korea. Tel.: +82 31 260 6037; fax: +82 31 260 6009.
E-mail address: sgleehong@gmail.com (S.G. Lee).
for its range of phase stability. Furthermore, it is able to yield large
and complex shapes for structural and other nuclear applications.
Finally, although there are many organic precursors, a commercial
source exists for the formation of SiC.
The PIP process, in the present study, consists in impregnating
the polymeric precursor into a particulate bed, a porous solid or
a fiber preform; heating to decompose and pyrolyze the polymer,
and crystallizing following a firing schedule. An alternative process
consisted of pressing powders wetted with an appropriate quantity
of precursor.
The following stages are reported [5–13] to occur during pyrol-
ysis and crystallization: (1) removal of moisture and volatile
oligomers at low temperatures, (2) loss of H2 from SiH2 groups,
and cross-linking of the polymer, to form a network structure, (3)
extensive structural rearrangement, which is accompanied by loss
of mainly H2 but also some C and Si-containing species, and (4)
crystallization. To obtain high thermal conductivity, the SiC must
be as dense, pure, and large-grained as possible [14]. However, it is
very challenging to obtain bodies with high density without many
repeated impregnation cycles because of the high shrinkage of the
organic precursor during processing, and possible closure of the
interconnected porosity in the body being impregnated. The PIP
method followed the general methods given by the vendor [10],
Starfire, Inc., with some important modifications described below.
In the present study, we first optimized the PIP method to fabri-
cate reasonably dense SiC samples; and then, we used our method

0920-3796/$ – see front matter © 2008 Elsevier B.V. All rights reserved.
doi:10.1016/j.fusengdes.2008.04.008
714 S.G. Lee et al. / Fusion Engineering and Design 83 (2008) 713–719
to consolidate ␣-SiC powders in order to produce SiC composite
matrix (designated as SiCp/SiC–PIP) with high conductivity matrix.
2. Sample fabrication
2.1. Materials
Among many organic precursors, we selected the allyl-hydrido-
poly-carbo-silane, called SMP-10 [10], which is the synthesis of a
polycarbosilane that has nominally a 1:1 Si:C ratio, and with H as
the only other component. It has the advantage of a high ceramic
“yield” (weight of ceramic to that of polymer) of near stoichiometric
SiC [10–13].
For consolidating SiC particulates, we used two types of SiC
powders: one submicron ␤-SiC purchased from HC Starck, and one
coarser ␤-SiC powder (average size of powder is 10 microns) con-
tributed by Superior Graphite.
2.2. Inert gas solubility measurement
As mentioned, several successive impregnations are neces-
sary to overcome the shrinkage of the polymer with pyrolysis
and crystallization and fill the porosity; however, the difficulty of
impregnation increases with the number of impregnations due to
the formation of very narrow paths or blockage of channels after
several PIP cycles.
To overcome this problem, gas pressure was applied to the sam-
ples submerged in the polymer to help force the liquid through
the narrowing paths. However, gas may also dissolve in the poly-
mer and ultimately decrease its density. Moreover, under the action
of any internal gas pressure, significant amounts of polymer can
be pushed out of the pores during the pyrolyzing step when the
external pressure is reduced.
The solubility of helium and argon in the polymer was measured
at various pressures to find the critical pressure beyond which the
polymer density is reduced. The weight change due to the pressur-
ization was immediately measured after pressurized to various gas
pressures for 30 min in a closed vessel.
2.3. Pure SiC sample preparation
Because of the sensitivity of the polymer to atmospheric con-
tamination, oxidation, and reaction with ambient moisture, all
operations in this work were performed under ultra high purity
argon atmospheres.
To make “pressed” SiC specimens using the PIP process, we
mechanically mixed the ␤-SiC powders (∼55 vol%) with the liquid
polymer (∼45 vol%), and pressed the mixture to form a green pellet.
Different compaction pressures were tested.
We also prepared “cast” samples, in which the polymer was
introduced into a packed powder in a mold. We used a mold made
of stainless steel, and the impregnation was done inside a vacuum
chamber by first evacuating the powder mass, introducing the poly-
mer, and then allowing atmospheric pressure to push the polymer
into the powder.
We measured the bulk density of the powder packing. The loose
density was about 30% of the theoretical density of SiC (%TD), and
the packed density was about 50%TD. The submicron powder was
discarded for the cast method since its packing density remained
too low (about 30%TD).
To make cured samples, both the pressed pellets and the cast
samples were pyrolyzed at temperatures up to 1123 K in ultra high
purity argon (UHP Ar) to prevent the formation of oxides or reaction
with water vapor.
Fig. 1. Schematics of polymer impregnation system.
2.4. Polymer impregnation and pyrolysis
We developed the impregnation system, Fig. 1, which allowed
us to degas simultaneously both the polymer and the solid sam-
ples prior to impregnation. Moreover, the degassed samples are
impregnated without exposing to air. The system was composed of
two independent but interconnected chambers A and B. Chamber
A was used to degas the polymer, while chamber B was used to dry
and evacuate the porous samples.
Note that the chamber A was heated at 333 K, and that the
precursor liquid was agitated with a magnetic stirrer to improve
the degassing the polymer. The pretreatment of the polymer was
stopped when the vacuum reached about 60–100 mTorr, and when
visible gas bubbles were no longer formed inside the liquid. The
polymer preheating was necessary to increase the impregnation
of the polymer by reducing its viscosity. The viscosity of the pre-
treated polymer at room temperature was measured at ∼0.08 Pa s,
while its viscosity as-received was measured at ∼0.1 Pa s. Note that
polymer that had aged for several months in a freezer presented an
even larger viscosity (∼0.15 Pa s).
Meanwhile in the B chamber, the samples are evacuated to
20 mTorr. The polymer is then introduced into the samples using
the pressure difference between the two chambers. UHP Ar is intro-
duced into the chamber A to raise the pressure to 1 atm while the
samples stay under vacuum inside the chamber B. We call this the
“vacuum impregnation” step. After vacuum impregnation, the sam-
ples still submerged in the polymer were transferred to a pressure
vessel and pressurized with gas while submerged; we call this step
“gas pressure impregnation”.
2.5. Sample characterizations
To improve our knowledge of the pyrolyzed polymer, we mea-
sured the solid density of the crystallized product. Note that we only
considered the solid density without the open porosity for charac-
terizing the pyrolyzed polymer product. Moreover, we evaluated
the crystallinity of the solid formed after crystallization with XRD.
Several crystallization temperatures were tested.
For SiCp/SiC–PIP samples, the bulk density was measured by the
Archimedean method (so called “immersion density”). Since three
 S.G. Lee et al. / Fusion Engineering and Design 83 (2008) 713–719
Table 1
Sample list for thermal conductivity measurements
ID SiC powder Polymer Crystallization
impregnation
kSiC1 10 ␮m (55 vol%) Vacuum and 4 MPa PIP (1573 K)
(Ar gas)
kSiC2 10 ␮m (55 vol%) Vacuum and 4 MPa PIP (1773 K)
(Ar gas)
kinds weight values (dry weight, weight in liquid and saturated
weight) were measured, the open porosity was considered as part
of the sample for the bulk density.
Thermal conductivity measurements were performed by a laser
flash method [15] at Idaho National Laboratory (INL) on the sam-
ples listed in Table 1. In this technique, the thermal diffusivity of
each sample was measured at several temperatures in Ar gas envi-
ronment. The thermal expansion was measured independently to
estimate the evolution of density over the test temperature range.
The specific heat was calculated on a mass-weighted mixture of the
phases. Thermal conductivity (k) was then determined accordingly
to the following relationship;
k = ˛Cp
where ˛ is thermal diffusivity,  is density, and Cp is specific heat.
We observed the microstructure of the produced samples with
optical microscope (OM) and scanning electron microscope (SEM).
3. Results and discussion
3.1. PIP process optimization
3.1.1. Polymer impregnation
According to the gas solubility measurement shown in Fig. 2,
He gas showed higher solubility into the polymer than UHP Ar gas.
The dissolved gas quantity rapidly increased for He gas pressure
higher than 3 MPa, while UHP Ar showed low gas solubility up to
4 MPa. Therefore the impregnated solid can be pressurized up to
4 MPa when UHP Ar was used, while the pressure would be limited
to 2 MPa when we used He gas. Note that He gas solubility at 1 MPa
is higher than Ar gas solubility at 4 MPa.
The Hagen–Poiseuille equation for fully developed laminar flow
under steady-state conditions with no gravity or capillarity effects
Fig. 2. Helium and Ar gas solubility depending on the applied gas pressure.
715
Density
∼85%TD
∼85%TD
Fig. 3. SMP-10 weight changes up to 1773 K pyrolyzed in UHP argon gas flow.
was used to estimate impregnation time [16];
32L2
tHagen-Poiseuille (sec) =
PD2
tpractical (sec) = Tortuosity × tHagen-Poiseuille
where L, the impregnation length, was taken as half the sample
height or 5 mm, ‘P’ pressure difference, ‘D’ pore diameter, and
‘tHagen–Poiseuille ’ the time to fill the pore.
Considering the tortuosity as 2 (since the range of tortuosity is
1–2 [17]) and measured the viscosity () as 0.08 Pa s, pores as small
as 0.1 ␮m in diameter are expected to be fully impregnated under
about 4 MPa of gas pressure in 60 min (Tpractical ). This was used for
the processing time in the gas pressure impregnation step.
3.1.2. Pyrolysis
Several critical temperatures have been reported [5] to occur
during pyrolysis for the rapid decomposition of the polymer
and/or for phase transitions. To identify the transitional temper-
atures, we measured the weight loss of SMP-10 and the solid
density of the pyrolyzed products after heating to different max-
imum temperatures. Samples were heated with ramp rates of
0.5–3 K/min, and maintained for 2 h at the maximum tempera-
ture.
As shown in Fig. 3, the largest weight loss occurred between
573 and 873 K, and no further significant weight loss was observed
from 873 to 1250 K. The second weight loss was observed
above about 1500 K, which is related to carbothermic reduction
[5].
The weight loss between 573 and 873 K is generally believed to
be due to the decomposition and cross-linking of the polymer [5].
Since slower heating in this temperature range was reported to be
essential to increase cross-linking instead of volatilization of the
lighter organic species, and thus ceramic yield [18], a slow heating
rate was used for the pyrolysis cycle up to 873 K. The heating rate
in each step was controlled as shown in Table 2.
3.1.3. Characteristics of pyrolyzed product of polymer
As shown in Fig. 4, higher temperature pyrolysis of the precur-
sor produced larger and more interconnected pores. As shown in
Fig. 5, the pyrolyzed product also became denser at higher temper-
ature, and the density reached its maximum of about 80%TD above
Table 2
Thermal cycle control for PIP (polymer impregnation and pyrolysis)
Up to 473 K: (before polymer boiling) 1–3 K/min
573–873 K: (polymer decomposition and cross-linking) 0.5–1 K/min
873 and more: solid body (solid phase transformation) 3 K/min
Cooling 3–5 K/min
716 S.G. Lee et al. / Fusion Engineering and Design 83 (2008) 713–719
Fig. 4. Optical microstructure observation of product of polymer pyrolyzed (a) up
to 873 K and (b) up to 1523 K.
1573 K. The large and open pore structure due to higher tempera-
ture pyrolysis would be benefit for the subsequent PIP cycle.
The XRD study showed, Fig. 6(a), the broad peaks representing
the formation of ␤-SiC (cubic form) for the PIP product crystallized
at above 1523 K, which is consistent with the results reported by
Starfire [10]. Using the half width of the broad (1 1 1) peaks and
the Debye and Scherrer formula [19], we calculated the crystallite
size. In Fig. 6(b) we report the crystallite size as a function of the
crystallization temperatures and time. The crystallite size appeared
to depend more on the crystallization temperature than on the time
duration at temperature.
The pyrolyzed product also appeared to retain small amounts
of free carbon (C), as observed in the XRD in Fig. 6(a). On the
other hand, although crystobalite was reported to form during PIP,
Fig. 5. The density change in the organic precursor as a function of final temperature.
Fig. 6. (a) XRD pattern of crystallized SiC and (b) crystallite size depending on
various crystallization conditions.
with its quantity increasing with time [4], no distinct peaks for
crystobalite were observed in the present work. Nonetheless, very
small amount of SiO or SiO2 unresolved by XRD could exist in the
SiCp/SiC–PIP due to high temperature oxidation because UHP Ar
contains about 0.2 ppm of oxygen as an impurity. At high temper-
ature, the crystobalite and free carbon can be removed owing to
carbothermic reaction [20,21].
3.2. Density evolution of SiCp/SiC–PIP matrix during PIP process
Surface damage was observed after pyrolysis when the powder
was compacted at high pressure (above 150 MPa). The damage is
believed to be due to the gas release that has difficulties to escape
from the samples. Compacts pelletized at 50 MPa were used for
PIP.
As the starting constituent in both pelletizing and casting
types was similar, bulk densities of the cured samples were about
60–62%TD of SiC for both methods. This value appeared to be
reasonable considering the starting composition and the changes
in volumes and densities of the pyrolyzed polymer. The dif-
ference between the measured (60–62%TD) and the calculated
(61.5–65%TD) would be attributed to inaccuracy of the starting
composition. Considering that SiC powders are assumed to be inert
during the process, the density of the cured specimens was calcu-
 S.G. Lee et al. / Fusion Engineering and Design 83 (2008) 713–719 717

Table 3
Designation of SiCp/SiC–PIP samples for density evolution

ID SiC powder Polymer impregnation

SiC1 Submicron Vacuum and 1 MPa (He gas) PIP (1573 K)

SiC2 10 ␮m Vacuum and 1 MPa (He gas) PIP (1573 K)
SiC3 10 ␮m Vacuum and 4 MPa (Ar gas) PIP (1573 K)
SiC4 10 ␮m Vacuum and 4 MPa (Ar gas) PIP (1773 K)

lated as follows;

Density = volume fraction of SiC powder × density of powder

+volume fraction of PIP × density of PIP

The following values are required for the calculation:

volume fraction of SiC powder: 0.55,

density of powder: 3.21 g/cc = 100%TD of SiC,
volume fraction of polymer: 0.45,
volume change of polymer due to pyrolysis up to
1123 K(measured): 0.35,
density of PIP at 1123 K (measured): 2.12 g/cc = 66%TD of SiC, and
density of cured specimen = 0.5 (or 0.55) × 3.21 + 0.45 (or 0.5: vol-
ume fraction of polymer) × 0.35(volume shrinkage) × 0.66 (%TD
of PIP product pyrolyzed at 1123 K as measured) × 3.21 = 1.98 or
2.09 g/cc (∼61.5%TD or ∼65%TD).

The cured samples were retrievable from the mold without

damage owing to the processing shrinkage (∼3%) in the curing
process. These cured samples were further impregnated with the
polymer, subsequently pyrolyzed and crystallized to form dense
SiCp/SiC–PIP matrix.
As shown in Fig. 7, the SiCp/SiC–PIP matrix became denser with
the successive PIP cycles. The achievable maximum densities varied
with fabrication conditions and polymer impregnation methods;
however, the density evolution rate (the slope in the curves) at the
initial period was same regardless of the fabrication conditions.
Since the starting density is similar in all the samples, the den-
sity evolution rate should depend on the pyrolyzed polymer mass
added in each cycle. The same rate in the density evolution thus
indicated the mass gain by successive PIP cycles was not affected
by the impregnation pressure at the initial periods. However, after
certain number of PIP cycles, there was no improvement of sample
density, which indicated that further impregnation was impossible.
Table 3 shows the sample designations. As observed in Fig. 7,
with the low pressure impregnation (1 MPa) no further density
improvement was observed after 3 cycles and 6 cycles for SiC1 and
Fig. 7. Density evolution of SiC powder consolidation samples.
Fig. 8. Inhomogeneous microstructure, (a) submicron SiCp/SiC–PIP samples and (b)
10 ␮m SiCp/SiC–PIP samples; after 6 cycle of PIP with 1 MPa of He gas pressurization
impregnation.
SiC2, respectively, which showed the starting pore size due to differ-
ent powder size affects polymer impregnation in the process with
the low gas pressure impregnation. With the high pressure impreg-
nation (SiC3), the density improvement continued up to 12th PIP
cycle. The maximum densities obtainable with the process were
about 82%TD and 87%TD with the impregnation pressures of 1 MPa
(SiC2) and 4 MPa (SiC3), respectively.
As shown in Fig. 8(a), dense phase was formed only at the
periphery of SiC1 (with submicron powder). Similarly, for SiC2,
made with 10 ␮m powder and impregnated with low gas pres-
sure, the phase near the surface was dense without noticeable
pores; but, pores were observed at the center, as shown in Fig. 8(b).
For SiC3, due to the higher pressure (4 MPa) of Ar gas used for
impregnation, the sample microstructure was homogeneous, as
shown in Fig. 9(a) and (b). This trend can be attributed to the
fact that the time of impregnation (1 h) was not sufficient to allow
the complete penetration of the polymer at low pressure. Hence,
only the surface of the sample was polymer impregnated. The
incomplete impregnation became even more serious when the
pore size was smaller like in SiC1, in which the smaller pow-
der used led the cured form to have smaller pore sizes than in
SiC2.
718 S.G. Lee et al. / Fusion Engineering and Design 83 (2008) 713–719

Fig. 10. SiCp/SiC–PIP samples: (a) curing and (b) after 6 cycle of PIP with high
Fig. 9. Homogeneous density, 10 ␮m SiCp/SiC–PIP samples; after 6 cycle of PIP with pressurization impregnation.
4 MPa of Ar gas pressurization impregnation; (a) low magnification and (b) high
magnification.
SiCp/SiC–PIP matrix crystallized at 1573 and 1773 K were 10 and
50 W/mK at 1273 K; respectively. This may be related to the fact
The microstructure observation of SiCp/SiC–PIP matrix revealed
that the crystallization temperature increased crystallite size and
that the pore size became smaller with the number of PIP cycles,
may have improved its purity.
as shown in Fig. 10(a) for as-cured samples, and in Fig. 10(b) after 6
Low thermal conductivity may have resulted not only from the
full PIP cycles to 1573 K. For the cured samples, which were con-
very fine pores and crystallites, but also from impurities [14,22,23].
solidated by one cycle of PIP (1123 K), the pore size was about
As observed in XRD study, the crystallite size of PIP product was
20–100 ␮m whereas after 6 cycles of PIP to1573 K, we measured
increased with the crystallization temperature; high temperature
about 1–2 ␮m diameter pores (Fig. 10(b)).
crystallization also removed free carbon that may be retained in
The comparison between the measured density and the max-
imum density calculated with the polymer yield confirmed that
the process was done ideally when high gas pressure (4 MPa
of UHP Ar gas) was used for impregnating the polymer into a
porous body. Since the volume fraction of SiC particles was about
0.55, the theoretical maximum density in this case should be
about 89%TD (the volume fraction of SiC powder × density of SiC
powder + the volume fraction of PIP product × density of PIP prod-
uct = 0.55 × 3.21 + 0.45 × 2.5 = 2.85 g/mL). The 2–4% difference in
the density from the theoretical maximum are probably due to
fabrication defects (closed porosity) produced during PIP.

3.3. Thermal conductivity measurements of SiC matrix

The thermal conductivity of SiCp/SiC–PIP matrix increased with

crystallization temperature. As shown in Fig. 11, although the bulk
density of the samples was the same, thermal conductivities of Fig. 11. Thermal conductivity measurement of SiCp/SiC–PIP samples.
 S.G. Lee et al. / Fusion Engineering and Design 83 (2008) 713–719
pyrolyzed product. When samples only have small amounts of the
free carbon, the free carbon can be removed by the following car-
bothermic reaction at above 1673 K [20,21];
SiO2 + C(s) = SiO(g) + CO(g)
4. Summary
Polymer impregnation and pyrolysis (PIP) method was effective
for consolidating powders when the process was optimized. Gas
pressurization in the impregnation step was effective to obtain high
densities for the given pore structures. UHP argon was better than
helium for gas pressurization in the impregnation step, since argon
gas showed lower solubility in the polymer even at relatively high
pressure. For argon, the optimized gas pressure was found to be at
4 MPa in the present work.
SiCp/SiC–PIP matrix was obtained as high as 87%TD of SiC using
the optimized PIP process. Crystallization temperature as high as
1773 K was necessary to produce high thermal conductivity the
matrix since the higher temperature crystallization process helped
produce larger crystallites of SiC–PIP and remove carbon impurities.
Although SiC fiber was not introduced in the present study, con-
sidering that if the size of fiber is similar to that of the powder, as
soon as uniform mixing is obtained and the fiber is stable up to
1773 K, we expect high dense and thermal conductive SiCf /SiC–PIP
composite can be produced with the PIP process developed by the
present work.
Acknowledgments
The authors would like to thank Mitchell Meyer, Rory Kennedy
and Andrew Madison of the Idaho National Laboratory for their
help in conducting the thermal property measurements, and the
USDOE for their financial support of this work, under the DOE–NERI
program. (Project No. 02-180 Award DE-FG07-02ID22613).
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