Aerospace Science and Technology 26 (2013) 185–191

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Aerospace Science and Technology

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Development and characterization of polymer–ceramic continuous fiber reinforced

functionally graded composites for aerospace application
Suresh Kumar ∗ , K.V.V.S. Murthy Reddy, Anil Kumar, G. Rohini Devi
Ceramic Matrix Composite Division, Advanced Systems Laboratory, DRDO, Hyderabad, 500058, India

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

Article history: Functionally graded materials (FGMs) have continuous change in the composition across the thickness
Received 31 October 2010 which results in gradual change of the properties. The ability of the FGMs to perform more than
Received in revised form 29 October 2011 one contrasting functions as an integral structure makes them an attractive material for aerospace
Accepted 4 April 2012
applications. So far the research focus has been on the functionally graded coatings and particulate
Available online 10 April 2012
reinforced functionally graded composites. In this study, continuous fiber reinforced functionally graded
Keywords: composites (FGCs) have been prepared using quartz fabric reinforcement for thermo-structural aerospace
Composite structure application. Silicone resin and fused silica powder have been used to obtain graded matrix. The FGC
FGM laminates have been characterized for mechanical and thermal properties. The laminates were also
Aerospace materials evaluated for thermal shock resistance and thermal insulation properties by exposing to infra-red
heating lamps under high heating rate of about 800 ◦ C/s and high heat flux of 0.6 W mm−2 for 70 s.
FGC laminates did not de-laminate or charred. Temperature drop across the laminate of 8 mm thickness
was found to be 600 ◦ C. The concept of FGC fabrication process is demonstrated to fabricate scaled down
typical airframe sections also.
© 2012 Elsevier Masson SAS. All rights reserved.

1. Introduction
Advanced aerospace structures require materials capable of
serving multi-functions. Quest for developing materials with multi-
functions has led to the concept of functionally graded materi-
als (FGMs) wherein several contrasting functions are incorporated
into a single material; like, toughness of the polymeric materials
and temperature capability of the ceramics. FGMs have continuous
change in composition and microstructure across the thickness,
the outer-most layers (both surfaces) essentially being the pure
composition of the components of the FGM [8,11]. FGMs were
developed first time by Japanese scientist Niino and coworkers
in 1984 as a means of preparing thermal barrier materials for
space structures, fusion reactors, space plane systems and turbine
engines [11]. It is the monolithic FGMs which have been under
focus for many researchers to develop useful systems for differ-
ent uses [6,12]. Fiber reinforced plastics (FRPs) are widely used as
structural materials for aerospace applications in view of their high
strength to weight ratio. However FRPs have the limitation with
respect to their use beyond 200 ◦ C temperature [2,13,14]. Service
temperature of ceramics is higher but their limited strengths and
toughness limits their use for structural applications [2,13]. Mate-
rials for aerospace applications should have high specific strength
* Corresponding author. Tel.: +91 40 24306994; fax: +91 40 24306498.
E-mail address: sureshtanwar@rediffmail.com (S. Kumar).
along with high service temperature. In principle, two layer struc-
tures may be obtained by bonding ceramic and polymer layers
to utilize high service temperature capability of the ceramics and
high strength of the polymers. Due to the large difference in the
coefficient of thermal expansion (CTE) of the polymers and ceram-
ics, their two layer structures generate a large amount of thermal
stresses which can cause de-bonding at the interface [4,5]. To avoid
the large CTE mismatch between the polymer and ceramic these
materials may be graded across the thickness keeping the two op-
posite surface layers as pure polymer and pure ceramic. Toughness
and mechanical strength of the graded material may be further
enhanced by reinforcing with a suitable fibrous reinforcement to
obtain functionally graded composites (FGCs).
Silicone resins are capable of with-standing temperature up
to 400 ◦ C and may provide good strength when reinforced with
quartz fabric. Quartz–silica (silica–silica) composites can with-
stand temperature up to 1500 ◦ C in air without much degradation
in mechanical properties [10]. A suitably designed FGC may exploit
mechanical strength of quartz–silicone composites and tempera-
ture capability of quartz–silica composites. Quartz–silicone com-
posite layer may be used as a structural material while quartz–
silica composite layer as a high temperature capable material.
The matrix may be graded across the thickness of the FGC laminate
by adding fused silica powder into silicone resin in an appropriate
ratio.
Aim and scope: In this paper research efforts are made to fabri-
cate quartz fiber reinforced FGC laminates and some typical shape

1270-9638/$ – see front matter © 2012 Elsevier Masson SAS. All rights reserved.
http://dx.doi.org/10.1016/j.ast.2012.04.002
186 S. Kumar et al. / Aerospace Science and Technology 26 (2013) 185–191
Table 1
Thermo-structural properties of matrix materials being used for FGC preparation.
S. No. Material Strength
(MPa)
1. Quartz–silicone 250–300
2. Quartz–silica 50–70
Fig. 1. Flow sheet for FGC preparation.
Fig. 2. Scheme of functionally graded composite.
scale down airframes. The FGC laminates shall be tested for ther-
mal and mechanical properties. Thermal shock and thermal insu-
lation performance of the FGC laminates shall also be evaluated
under high powered IR heating lamps simulating a high heating
rate and high heat flux environment for about 70 s.
2. Experimental
2.1. Raw materials
2.1.1. Reinforcement
Quartz fabric of twill weave textile pattern was used as rein-
forcement for FGC laminates. In twill weave textile pattern two
yarns are placed up and down alternately; each yarn consists 340
quartz filaments of nine micron diameter. The yield strength of
a monofilament is 3.1 ± 15% GPa while modulus is 75 ± 5% GPa.
2.1.2. Matrix
Three components were used to obtain matrix system for the
FGC laminates viz. (i) Dow Corning 4-3136 binding silicone resin;
(ii) four micron sized fused silica powder; (iii) colloidal silica. Dow
Corning 4-3136 binding silicone resin flakes were used to obtain
100% polymeric matrix while colloidal silica was used to obtain
100% silica matrix. Fused silica powder was used to obtain grading
of silica content in the matrix system. Colloidal silica is a stable
dispersion of nano-sized amorphous silica powder in water with
sodium ion stabilizer and alcohol as gelling retardant. pH of the
colloidal silica was in the range of 8.0–9.0, density was 1.3 g/cc
and solid silica content was about 40% by weight. The matrix ma-
terials have been chosen due to their low thermal conductivity and
high temperature capability (Table 1).
Thermal conductivity Service temperature
(W/m K)
0.23 Up to 400 ◦ C
1 .0 Up to 1500 ◦ C
2.2. FGC laminate fabrication
The process of FGC laminate/shaped component fabrication in-
volves prepregging, molding and impregnation with colloidal sil-
ica. The various process steps are shown with the help of a flow
sheet (Fig. 1). A typical reinforcement and matrix lay up scheme of
an FGC laminate is shown in Fig. 2.
2.2.1. Prepreg preparation
The silicone resin flakes were dissolved into laboratory grade
acetone to obtain brush-able resin paste. Fused silica powder was
added in the silicone resin paste as per the grading requirement
(Table 2) to obtain different matrix composition resin systems.
Each type of resin and powder system was applied over four quartz
fabric layers with the help of a hand brush. The layers were dried
at room temperature; these layers are termed as prepregs.
2.2.2. Molding of FGC laminates
The dried prepregs of size 200 × 200 mm along with four layers
of quartz fabric were stacked in a predetermined order (Table 2)
to obtain a desired gradation of silica and silicone matrix con-
tent across the thickness of the FGC laminate. The stack of the
prepregs was kept in a stainless molding die and was pressed at
about one ton load. Under pressing condition temperature of the
stack was raised at the rate of 2 ◦ C/min till the prepregs softened
at around 110 ◦ C; up to 5 tons additional load was applied grad-
ually to obtained fiber volume fraction in the range of 50–55%.
The temperature was further raised up to 300 ◦ C at 5 ◦ C/min and
the stack was held for 3 hours under the heat and the applied
load.
 S. Kumar et al. / Aerospace Science and Technology 26 (2013) 185–191
Table 2
Matrix gradation scheme.
Reinforcement
High temperature resistance Quartz fabric
Layer; Silica surface
Graded matrix zone Quartz fabric
Quartz fabric
Quartz fabric
Quartz fabric
Structural layer; Silicone surface Quartz fabric
Fig. 3. Kinetic heating test setup.
2.2.3. Impregnation of colloidal silica
The molded laminate was removed from the die and clamped
between perforated stainless steel (SS) plates. The stack along with
perforated plates was impregnated by colloidal silica under vac-
uum (1 mm Hg absolute). The laminate which is to be impregnated
was kept into a vessel and vacuum was applied. After achieving ab-
solute pressure of the order of 1 mm Hg at the laminate, colloidal
silica was transferred into the vessel. The laminate was soaked
in the colloidal silica for 1 hour followed by drying at 120 ◦ C in
an oven. After two impregnation–drying cycles, the plates were re-
moved followed by another three cycles of vacuum impregnations
and drying. After impregnation a dense FGC laminate was obtained
which got one face as 100% silicone resin matrix and another one
100% silica matrix while reinforcement was kept same throughout
the thickness. The FGC laminates were characterized for mechani-
cal and thermal properties. FGC laminates are termed at category-I
laminates.
Apart from FGC laminates, four other matrix compositions
based laminates were also prepared and termed as category-II to V
viz. (category-II) – 100% silicone resin, (category-III) – 80% silicone
resin and 20% silica powder, (category-IV) – 60% silicone resin and
40% silica powder, and (category-V) – 40% silicone resin and 60%
silica powder. These laminates were used to generate property data
which will be discussed later.
2.2.4. Quartz–silica laminate
Colloidal silica impregnation was also used for fabricating
quartz–silica composite laminates. Quartz fabric layers (equivalent
to 50–55% fiber volume fraction) were stacked between perforated
SS plates and impregnated with colloidal silica followed by dry-
ing up to 500 ◦ C. Impregnation–drying cycles were carried out for
8 times to obtain laminates of density 1.9 g/cc. The quartz–silica
laminates are termed as category-VI laminates.
2.3. Characterization
2.3.1. Thermal conductivity
Thermal conductivity of the laminates of category-I, II and
VI was measured from 50 to 350 ◦ C using hot-guard-steady-state
187
Fused silica Silicone resin
(% w/w) (% w/w)
0 0
(Silica derived from
colloidal silica)
80 20
60 40
40 60
20 80
0 100
technique [1]. Cylindrical discs of diameter 25 mm, thickness 5
and 10 mm were cut from the laminates in the direction per-
pendicular to the fabric plane. For each thickness three samples
were tested. Fused quartz was used as a reference material during
the test (thermal conductivity of fused quartz = 1.0 W m−1 K−1 ).
2.3.2. Coefficient of thermal expansion (CTE)
CTE was measured up to 600 ◦ C in NETZSCH DIL 420C equip-
ment with alumina probe for laminates of category-II to cate-
gory-VI. Laminates of each category were cut into specimens of
size 25 × 5 × 5 mm in the direction parallel to the fabric plane.
Temperature of the specimens was raised at the rate of 5 ◦ C/min.
The change in the specimen length (resulting due to temperature
rise) was measured. The coefficient of the linear thermal expan-
sion was calculated as CTE = ( L / L )/ T ; where  L / L is the frac-
tional change in length of the specimen due to the temperature
change  T .
2.3.3. IR lamp (kinetic heating) testing
The ability of FGC laminates to with-stand sudden and intense
possible heating in aerospace applications was evaluated under
infra-red heating setup termed as kinetic heating. A schematic
of the test is shown in Fig. 3. The test setup is capable of sim-
ulating a typical high temperature (> 1000 ◦ C), heat flux up to
0.9 W mm−2 and heating rates of the order of 800 ◦ C/s. FGC lami-
nates having thickness of 8 mm were cut into size of 50 × 50 mm
plate and mounted on a fixture. K-type thermocouples were fixed
at both the surfaces of the FGC plate with the help of high tem-
perature adhesive cement for continuous recording of the sur-
face temperature during the test. The fixture was positioned at
about 150 mm apart from IR heating lamps in such a way that
the silica surface of the FGC plate was exposed to the heating
lamps for about 70 seconds at heat flux of 0.6 W mm−2 . The
temperature at both the surfaces of the plate was recorded and
plotted against the time. Similar tests were also carried out on
quartz–silicone (category-II) and quartz–silica (category-VI) lami-
nates to compare the thermal insulating properties of the FGC
laminate with the two extreme matrix composition based com-
posites.
188 S. Kumar et al. / Aerospace Science and Technology 26 (2013) 185–191
Fig. 4. FGC shaped components.
Table 3
Thermal conductivity of FGC with temperature.
Temperature at silica surface, ◦ C 80
Temperature at silicone surface, ◦ C 39.6
Average temperature across the FGC 59.8
thickness (10 mm)
Thermal conductivity, W m−1 K−1 0.458
2.3.4. Flexural strength testing
FGC laminates and the laminates of category-II and category-VI
were tested under 3-point bending load at room temperature.
The laminates of category-II and category-VI were cut into rect-
angular bars of size 4 × 10 × 60 mm while FGC laminates were
cut into bars of size 7 × 10 × 60 mm. Bend test was carried out
on a span length of 40 mm in each case with 0.5 mm/min cross
head speed using universal testing machine (Instron model 8801).
Three-point bending behavior of FGC bars was studied for both the
cases, i.e., (i) silicone matrix surface under compression and (ii) sil-
ica matrix surface under compression.
3. Fabrication of FGC shaped component
Fabrication process for FGC was also demonstrated for a typical
scaled down airframe sections. Match-mold metallic dies were fab-
ricated (Fig. 4) and contour woven socks of quartz yarn suited to
the dies were fabricated. Solution of predetermined composition
of silicone resin and fused silica powder was prepared and ap-
plied over socks with hand brush. The solution impregnated socks
were stacked over the male mold in wet condition one by one
in pre-decided order. Silicone resin rich socks were laid first on
to the male mold (becomes innermost surface of the component)
followed by socks impregnated with solution having gradual in-
creasing silica powder content, at the last, three socks without
any solution were also kept as the outer-most layers. The layup
stack was allowed to dry. The female mold was placed over the
layup of the prepregs and tightened with male mold. The layup
stack was cured under compression at up to 300 ◦ C, the die was
held at 300 ◦ C for 3 hours followed by natural cooling. The com-
ponent was extracted and post curing was carried out at 350 ◦ C
for 2 hours. The component was impregnated with colloidal silica
with the help of vacuum (1 mm Hg) to impart silica matrix in the
outer-most quartz socks. Feasibility study to develop shaped FGC
158.4 243.0 330.7
71.3 106.7 138.1
114.85 174.85 234.40
0.441 0.439 0.435
components was carried out successfully to demonstrate continu-
ous fiber reinforced FGM (Fig. 4).
4. Results and discussions
4.1. Laminate preparation
Density of the FGC laminates is higher than the density of lam-
inates of category-II and VI but lower than the density of the lami-
nates of category-V. Density of the FGC laminates was in the range
of 1.95–2.0 g/cc while density of the laminates of category-II
and VI was in the range of 1.70–1.72 g/cc and 1.85–1.90 g/cc
respectively. The density of the laminates found to be increased
as silica powder loading increased; density of the laminates of
category-V was found in the range of 2.15–2.18 g/cc. Variation in
the density of the laminate is due to the effective density of the
matrix system. It may be noted that the densities of silicone matrix
and silica powder are 1.25 g/cc and 2.2 g/cc respectively. On ad-
dition of silica powder, effective density of the matrix increases.
As laminates of category-I to V were prepared under compression
therefore their porosity is less than 5%. In case of the laminates of
the category-VI, these are prepared by repeated vacuum impregna-
tion of colloidal silica. The colloidal silica goes inside the pores of
the laminates due the capillary pressure and applied pressure gra-
dient. As the density increases the size of the pores in the laminate
gets reduced followed by choking of the pores at the mouth. There-
fore the laminates of the category-VI cannot be densified closer to
their theoretical density limit of 2.2 g/cc; porosity in these was as
high as 14%.
4.2. Thermal conductivity
Thermal conductivity of the laminates of FGC, category-II and
category-VI was found to be in the range of 0.435–0.458, 0.2–0.23
and 0.98–1.0 W m−1 K−1 respectively. Thermal conductivity of FGC
 S. Kumar et al. / Aerospace Science and Technology 26 (2013) 185–191
Fig. 5. CTE of quartz fabric reinforced silicone–silica powder matrix laminates.
laminate measured with temperature is given in Table 3; it de-
creases marginally with temperature. Trends were similar for other
laminates also. FGC shows very low thermal conductivity which
may help for its intended thermal insulating properties. Low and
decreasing thermal conductivity may be explained as follows.
Thermal conductivity of the solids depends on the electronic
and lattice vibrations. In the case of FGC laminates, electronic con-
tribution is zero due to absence of any free electron. Lattice con-
tribution depends on the product of the mean free path, the speed
of the sound in the solid and the specific heat of the solid per unit
volume. Value of the thermal conductivity of the polymeric mate-
rials is very low due to flexibility in the polymer chain therefore
low speed of the sound. Thermal conductivity of the polymers has
been reported lower than 0.2–0.5 W/m K [3]. Thermal conductiv-
ity of the fused silica and quartz fabric is also low (1.0–1.2 W/m K)
due to amorphous in nature therefore effective mean free path is
very less [7]. Therefore FGC composites have thermal conductiv-
(a)
(b)
Fig. 6. (a) Temperature profile of category-II and VI laminates under kinetic heating test. (b) Temperature profile of FGC laminates under kinetic heating test.
189
ity in between the silicone resin and fused silica but dominated by
the thermal conductivity of silicone resin due to the high thermal
contact resistance of silicone resin and silica powder.
4.3. Coefficient of thermal expansion
CTE values for the laminates of the category-II to V were found
to be in the range of 4.5 × 10−6 to 1.5 × 10−6 K−1 (Fig. 5). It is
the highest (4.5 × 10−6 ) at 200 ◦ C and the least (1.5 × 10−6 K−1 ) at
500 ◦ C for the laminates of category-II. CTE value has decreased as
proportion of fused silica powder increased in the matrix. For all
the laminates of category-II to V, it initially increases up to 200 ◦ C
and then remains constant in the temperature range of 200–300 ◦ C
followed by decreasing trend. CTE of the laminates of category-VI
was the least (1.0 × 10−6 /K) and remains almost constant for en-
tire temperature range. CTE is directly proportional to the specific
heat of the material at constant volume and inversely proportional
to the bulk modulus of the material [9]. Therefore CTE of the poly-
mers is the highest followed by the metals, ionic and covalent
nature solids. CTE of the composites in direction parallel of fibers
largely depends on the CTE of the fibers but microstructure and
porosity of the matrix also have considerable effect on the CTE [9].
It may be noted that the porosity in the laminates of the category-I
to V was about 5% but in the laminates of the category-VI it was
as high as 14%. Higher the porosity, lower is the CTE [9]. Although
the fiber volume fraction is 50–55% in all the laminates but CTE
is higher for the laminates based on the silicone resin matrix net-
work compared to the silica matrix network. This may be due to
the higher porosity of quartz–silica; porosity absorbs the expan-
sion and net expansion of the specimen remains very low. While
in case of silicone resin based laminates the porosity is small and
the expansion of the polymers is higher in general compared to
190 S. Kumar et al. / Aerospace Science and Technology 26 (2013) 185–191
Fig. 7. Quartz–silicone laminate after kinetic heating test.
Fig. 8. FGC laminate after kinetic heating test.
the ceramics which results into higher CTE for all the laminates of
the category-II to V.
Though CTE of the FGC could not be measured due to limi-
tation of sample preparation of the required dimensions but its
value must be in between the CTE values of the laminates of
the category-II and VI as these two categories represent the two
extreme compositions (surface matrix) of the FGC. The FGCs are
expected to be used at service temperatures above 500 ◦ C, at that
temperature difference in CTEs of fused silica powder filled quartz–
silicone and quartz–silica composites is very less, which will help
in preventing thermal-shear-stress during actual use of FGCs.
4.4. Kinetic heating test
Temperature profile of the laminates of the category-II, VI and I
are shown in Figs. 6a and 6b. It is evident from the tempera-
ture profiles that the temperature drop per unit thickness of the
quartz–silicone (category-I) laminate is the highest and the least
in case of quartz–silica (category-VI). Laminates of the category-II
exhibited the highest temperature drop across the thickness of
6 mm; which is of the order of 850 ◦ C. The laminate of the
category-VI exhibited a steep rise of back surface temperature af-
ter 20 seconds and temperature drop across thickness of 8 mm
was found only 400 ◦ C after 70 seconds of exposure. In case of
FGC, surface temperature shoots up to as high as 850 ◦ C at silica
surface in first 60–70 seconds but temperature drop across 8 mm
thickness was recorded of the order of 650 ◦ C. Temperature profile
behavior of these laminates may be explained as per their thermal
conductivity. Thermal conductivity of the silicone resin is lower as
compared to silica (Table 1). Due to the lower thermal conduc-
tivity quartz–silicone composite does not conduct to the extent as
Fig. 9. Stress–strain curves for (1) quartz–silicone, (2) quartz–silica, and (3) FGC.
Fig. 10. Stress–strain curves for FGC.
quartz–silica. Hence temperature drop is the highest in the quartz–
silicone and the least in the quartz–silica. The drop is moderate in
case of FGC or in other words temperature drop was found to be
inversely proportional to the thermal conductivity as expected.
The surface of quartz–silicone facing the lamps was completely
pyrolyzed and indicates that the composite of that category may
not be suitable for repeated use under the tested conditions
(Fig. 7). Temperature drop was the least through the laminates
of category-VI; back face temperature rises above the acceptable
value; however the specimen remains intact. Hence use of quartz–
silica composites may not be preferable for longer duration; while,
FGC plate did not show any physical change either in the form
of de-lamination or pyrolysis (Fig. 8). This further strengthens
the suitability of the FGC under high heat flux and high heat-
ing rate environments. This corroborates the thermal conductivity
data. In combination thermal properties of FGC are superior to the
quartz–silicone and quartz–silica.
4.5. Flexural strength
Flexural strength was found to be in the range of 240–279 MPa
for quartz–silicone, 23–29 MPa for quartz–silica and 83–93 MPa
for FGC laminates. Comparative stress–strain curves under three-
point bending for quartz–silicone (1), quartz–silica (2) and FGC
laminates (3) are shown in Fig. 9. The strain at failure is the least
(0.002 mm/mm) for quartz–silica, while it was the highest for
quartz–silicone (0.015 mm/mm). Strain values of FGC laminates
were found to be in between the strain values of quartz–silica and
quartz–silicone laminates. It shows that the effect of the matrix
composition is prominent on the magnitude of the strain at the
failure. Polymers in general show high strain than ceramics. There-
fore, in spite of the similar fiber volume fraction in both the lam-
inates (quartz–silica, quartz–silicone); strain in the quartz–silicone
laminates is higher compared to the quartz–silica laminates.
FGC laminate samples were tested in two modes; (i) silica face
was under compression, (ii) when silica face was under tension;
silicone resin face is under compression. Stress–strain curves for
FGC laminates under three-point bending are shown in Fig. 10.
 S. Kumar et al. / Aerospace Science and Technology 26 (2013) 185–191
Fig. 11. Three-point bend tested FGC specimen.
Strain at failure of the FGC laminates is largely dominated by
quartz–silicone in both the modes. At the ultimate failure load the
specimen failed in shear mode (Fig. 11) at the interface where
composition of silica in the matrix is the highest. The fracture
propagates in the direction parallel to the fabric plane. It has also
been observed that FGC does not fail catastrophically and contin-
ues to take load even after initiation of failure which resembles
the very characteristics of a composite.
5. Summary and conclusions
The concept of monolithic FGM and functionally graded coat-
ing has been successfully extended to develop continuous fiber
reinforced functionally graded composites. Quartz fabric reinforced
polymer–ceramic FGM using grading of silicone resin and silica
matrix across the thickness has been fabricated. The FGC lami-
nates are tested for thermal conductivity, CTE, thermal shock and
flexural properties. The properties are found to be better than the
pure polymer/ceramic matrices based composites. The FGC lam-
inates have shown very good thermo-structural capability under
kinetic heating test and shown promising features for high tem-
perature reusable structures. The FGC process technology has also
been successfully demonstrated to fabricate shaped products.
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