Fusion Engineering and Design 109111 (2016) 11741178

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Fusion Engineering and Design

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

Fabrication of short SiC ber reinforced SiC matrix composites with

high ber volume fraction
Joon-Soo Park a, , Hiroshi Nishimura b , Daisuke Hayasaka a,b , Ju-Hyeon Yu b ,
Hirotatsu Kishimoto a , Akira Kohyama a
a
OASIS, Muroran Institute of Technology, Muroran 050-8585, Japan
b
Graduated School of Engineering, Muroran Institute of Technology, Muroran 050-8585, Japan

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

Article history: Short ber reinforced SiC/SiC composites with high ber volume fraction were fabricated by NITE process.
Received 5 September 2015 The effects of ber length and sintering condition on microstructure and mechanical properties were
Received in revised form investigated. Although, high sintering temperature promotes the densication of SiC matrix but leads to
16 December 2015
the degradation of F/M interface. The exural strength of SF-SiC/SiC with long ber length shows higher
Accepted 23 December 2015
exural strength compared to those of SF-SiC/SiC with short ber length. SF-SiC/SiC composites with
Available online 14 January 2016
complicated shape have been successfully fabricated by pseudo-HIP.
2016 Elsevier B.V. All rights reserved.
Keywords:
NITE process
SiC/SiC composites
Short ber

1. Introduction case of fusion reactor environments, thermal gradient inside the

Continuous SiC ber reinforced SiC matrix (SiC/SiC) compos-
ites are one of promising structural materials for nuclear energy
and aerospace application due to their excellent properties such as
light weight, high strength, reliability under high temperature, low
after heat, low radioactivity and so on [1]. In recent, it is encour-
aged to use SiC/SiC components by the commercialization of high
crystalline and high purity SiC bers as well as the development of
their innovative fabrication process, like Nano Inltration and Tran-
sient Eutectic (NITE) process [24]. NITE-SiC/SiC composites are
consisted of well densied SiC matrix and well aligned continuous
SiC ber with thin pyrocarbon (PyC) coating as ber/matrix (F/M)
interface. Due to its dens microstructure and high mechanical prop-
erties, it is considered as one of nuclear grade SiC/SiC composites
[5].
In the other hand, we must carefully discuss on the anisotropic
properties of SiC/SiC composites for their practical use. Because,
the thermo-mechanical properties of continuous ber reinforced
composites strongly depend on ber reinforcing architecture. In
Corresponding author.
E-mail addresses: jspark@mmm.muroran-it.ac.jp, demecadarby@gmail.com
(J.-S. Park).
material occurred by a high heat ux. This thermal gradient gives
differential swelling under irradiation, as well as differential ther-
mal expansion, resulting in the complicated stress eld inside the
material [6,7].
Thus, the evaluation of off-axial mechanical properties of SiC/SiC
composites is one of the important technical issues for fusion
application. Actually, it is well known that the specimen with uni-
directional ber (UD) reinforcing architecture shows quite low
strength in non-ber direction.
In the other hand, short ber reinforced composites, there is
no need to consider about the anisotropy due to their randomly
aligned ber architecture. Moreover, it provides many advantages,
such as high productivity of practical components with large sizes
and complicated shapes, shorter process time and lower cost.
Although, there are many advantages of short ber as mentioned
above, but only limited data concerned on short ber (SF) SiC/SiC
composites have been reported [8]. The production of homoge-
neous SF-SiC/SiC composites with high ber volume fraction (Vf )
is quite difcult, because of the entanglement of short bers. As a
result, Vf of SF-SiC or C/SiC was usually under 40% and it may be
difcult to obtain sufcient effects of ber reinforcing [810].
The purpose of this work is the process development of high
Vf SF-SiC/SiC composites based on NITE process. The effects of
ber length and sintering conditions on the microstructure and

http://dx.doi.org/10.1016/j.fusengdes.2015.12.060
0920-3796/ 2016 Elsevier B.V. All rights reserved.
 J.-S. Park et al. / Fusion Engineering and Design 109111 (2016) 11741178 1175

Fig. 2. Conceptual diagram of fabrication process for near net shaped SF-SiC/SiC by
P-HIP.

Bar type specimens with dimensions of 3 mmw

Fig. 1. Fabrication process of SF-SiC/SiC composites.
mechanical properties of SF-SiC/SiC were investigated. Near net
shaping of SF-SiC/SiC composites with complicated shape was also
performed by pseudo-hot isostatic press (P-HIP) method.
2. Experimental procedures
Highly crystallized SiC ber, Cef-NITETM (GUNZE LIMITED,
Japan), has been used as a reinforcing ber. Fiber diameter is
approximately 10 m. Number of ber laments per bundle is
800. As F/M interface, thin PyC coat (thickness < 500 nm) has been
formed on ber surface by conventional chemical vapor deposition
(CVD) method.
SiC powder, small amount of oxide additives and SiC based poly-
mer binder were used as raw materials for SiC matrix. In this study,
cut prepreg sheet has been used for the intermediate materials
for SF-SiC/SiC. Prepreg sheets consisted of uni-directionally aligned
continuous ber bundles impregnating with SiC matrix precursor
(SiC powder, additives and binder). It has the controlled weight
ratio of ber and matrix in order to obtain SF-SiC/SiC with high Vf
(approx. 45 vol%). The thickness and bulk density of prepreg sheets
are about 0.35 mm and 1.6 g/cm3 respectively.
Short ber including SiC matrix precursor was prepared by
cutting of narrow prepreg sheet (width 23 mm). In order to inves-
tigate the effects of ber length, cut prepreg sheet with different
lengths (5 mm and 10 mm) were prepared. And then, 20 g of cut
prepreg sheets was lled into the carbon mold for hot pressing
(HP). Dimension of carbon mold is 40 mm 40 mm. The condition
of HP temperatures are 1820, 1830 and 1840 C. Maximum pres-
sure, holding time and atmospheric condition are 20 MPa, 1.5 h and
vacuum, respectively. The ow of fabrication process and the key
conditions of SF-SiC/SiC composites are shown in Fig. 1 and Table 1.
26 mmL 1.2 mmt were machined, from the sintered body. 5
samples per each specimen were prepared to obtain average value.
All samples in the same specimen were cut with the same direction.
The effect of cutting direction was ignored in this study. Flexural
strength was measured by the three point bending test using UTM.
(Type 205R, INTESCO Co., Ltd., Japan.) The span of support pins and
test speed are 16 mm and 0.5 mm/min, respectively. After bending
test, the fracture surfaces of tested specimens were observed by
FE-SEM (JEOL, JSM-6700F, Japan).
In order to investigate the feasibility of near net shaping of SF-
SiC/SiC composites, SF-SiC/SiC with dome shape with dimensions of
outer diameter 40 mm inner diameter 38 mm length 50 mm
has been fabricated. Conceptual diagram of its fabrication process
is shown in Fig. 2. Preform was prepared using short bers (length
10 mm) and metallic dies with groove.
It is essential to add isostatic pressure for the homogeneous den-
sication of preform with complicated shapes. Thus, P-HIP has been
selected as sintering method. Although inert gas in HIP is usually
used as pressure transmitter, carbon powder is used in P-HIP [4,11].
During hot press, unidirectional load is transmitted to the pseudo
isostatic pressure by carbon powder.
3. Experimental results and discussions
Fig. 3 shows the appearance of SF2 specimens as an example of
SF-SiC/SiC composites fabricated in this work. The unique architec-
ture of randomly aligned short bers, which are prepared by cutting
of prepreg sheet, can be conrmed from the naked eye observation
of plate surface.

Table 1
Fabrication conditions of SF-SiC/SiC specimen.

ID Sintering Fiber length Density Flexural strength

temperature [ C] [mm] [g/cm3 ] [MPa]

SF1 1820 5 2.82 100

SF2 1830 5 2.76 96
SF3 10 2.87 135
SF4 1840 5 2.88 99
SF5a 5 2.94 100
Fig. 3. Appearance of NITE-SiC/SiC composites prepared with short bers (ber
a
Repeat of SF4. length: 5 mm).
1176 J.-S. Park et al. / Fusion Engineering and Design 109111 (2016) 11741178

Fig. 4. Effects of sintering temperature on the exural strength and density of SF- Fig. 6. Effects of ber length on the exural strength and density of SF-SiC/SiC.
SiC/SiC.

of inter bundle macro pore and large variation of strength data in

3.1. Effects of sintering temperature
SF1.
On the other hand, highly densied SiC matrix including small
Fig. 4 shows the effects of sintering temperature on the ex-
amount of intra-bundle micro pores can be observed at the
ural strength and density of SF-SiC/SiC composites. There is little
microstructure of SF4 and SF5. But, the signicant loss of F/M inter-
difference in the exural strength of each specimen. The exural
face is also observed at the microstructure of SF5. These results
strengths of SF-SiC/SiC composites were about 100 MPa. The speci-
indicate that higher sintering temperature promotes the SiC matrix
mens sintered at 1840 C show relatively high density (2.94 g/cm3 )
densication, but it leads to the degradation of PyC interphase.
compared with the others.
Fig. 5 shows the fracture surface observation results after the
exural test. Every specimen shows complicated crack branching 3.2. Effects of ber length
and deection, which is one of general toughening mechanisms in
CMCs (Ceramic Matrix Composites). From the specimens sintered The specimens with different ber length have been prepared
at lower temperature, macro pores are usually found at inter ber to investigate the effects of ber length. In order to avoid the loss
bundles. It was estimated that the interference between SiC ber of F/M interface and ber damage, specimens were sintered at
bundles suppressed the pressure transition required for the densi- 1830 C. Fig. 6 shows the effects of ber length on the exural
cation of SiC matrix and it is one of main reason of the remaining strength and density of SF-SiC/SiC.

Fig. 5. FE-SEM observation results of SF-SiC/SiC composites sintered at different temperatures.

 J.-S. Park et al. / Fusion Engineering and Design 109111 (2016) 11741178 1177

Fig. 7. FE-SEM observation results of SF-SiC/SiC composites with different ber

length.

Flexural strength of SF2 and SF3 are 96 MPa and 135 MPa,
respectively. The strength and density of SF3 with long ber length
shows slightly higher than those of SF2. However, the strength of
SF3 is still lower than that of NITE-SiC/SiC composites reinforced
by long continuous ber. The exural strength of unidirectional
(UD) and cross-ply (0/90) NITE-SiC/SiC composites are <500 MPa
and <200 MPa, respectively [12,13].
Fig. 7 shows the results of FE-SEM observation. Inter bundle
macro pores are also found from the microstructure of SF3. In usual,
longer reinforcing ber leads to more complicated and long crack
deection, which make it possible to improve the mechanical prop-
erties. But, clear difference was not found from the microstructural
observation. Further investigation is required to clear the effects of
ber length on the fracture manner of SF-SiC/SiC.
3.3. Near net shaping of SF-SiC/SiC
SF-SiC/SiC with dome shape has been sintered by P-HIP. Fig. 8
shows the appearance of specimen after P-HIP and the results of
fracture surface observation. It was conrmed that SF-SiC/SiC sin-
tered by P-HIP has sound F/M interface as well as highly densied
SiC matrix. Because of random ber alignment, high Vf and sound
F/M interface, it shows very rough and complicated fracture sur-
face. But, further study is needed to quantication of its mechanical
properties including strength and fracture resistance.
4. Summary
Based on NITE process, the fabrication method for SF-SiC/SiC
composites with high Vf has been discussed in this study. We have
succeeded in fabricating of SF-SiC/SiC composites with High Vf
(approx. 45 vol%) by using of cut prepreg sheets. It was revealed
that high sintering temperature promotes the densication of SiC
matrix but leads to the degradation of F/M interface. SF-SiC/SiC
Fig. 8. Appearance and FE-SEM observation results of SF-SiC/SiC composites sin-
tered by P-HIP.
composites with long ber length shows higher exural strength
(135 MPa) than those of shorter one. It was also shown that SF-
SiC/SiC with complicated shape can be obtained by using P-HIP.
Further study is still needed to optimize the process condition of
SF-SiC/SiC and to clarify/quantify their mechanical properties.
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