J. Mater. Sci. Technol., 2011, 28(3), 234-240.

Preparation of SiC Fiber Reinforced Nickel Matrix Composite

Lu Zhang, Nanlin Shi, Jun Gong and Chao Sun†

Institute of Metal Research, Chinese Academy of Sciences, Shenyang 110016, China
[Manuscript received March 7, 2011, in revised form July 2, 2011]

A method of preparing continuous (Al+Al2 O3 )-coated SiC fiber reinforced nickel matrix composite was pre-
sented, in which the diffusion between SiC fiber and nickel matrix could be prevented. Magnetron sputtering
is used to deposit Ni coating on the surface of the (Al+Al2 O3 )-coated SiC fiber in preparation of the precursor
wires. It is shown that the deposited Ni coating combines well with the (Al+Al2 O3 ) coating and has little
negative effect on the tensile strength of (Al+Al2 O3 )-coated SiC fiber. Solid-state diffusion bonding process
is employed to prepare the (Al+Al2 O3 )-coated SiC fiber reinforced nickel matrix with 37% fibers in volume.
The solid-state diffusion bonding process is optimized and the optimum parameters are temperature of 870◦ ,
pressure of 50 MPa and holding time of 2 h. Under this condition, the precursor wires can diffuse well, com-
posite of full density can be formed and the (Al+Al2 O3 ) coating is effective to restrict the reaction between
SiC fiber and nickel matrix.

KEY WORDS: SiC fiber; Composite; Diffusion barrier layer; Precursor wire

1. Introduction et al.[11] deposited yttria by chemical vapor deposi-

Nickel alloys are widely used in aerospace and
turbine engines due to their excellent mechanical
properties at elevated temperatures. However, high
density and poor creep-resistance limit their further
applications[1] . Composites can reduce the density
and meanwhile improve the high-temperature me-
chanical properties of the matrix[2–4] , which makes it
an effective way to overcome those problems in nickel
alloys.
With respect to SiC fiber reinforced nickel alloy
composites, the diffusion reaction between SiC fiber
and the matrix is so intense that the reinforced ef-
fect of SiC fiber in nickel matrix is degraded[5–7] . A
diffusion barrier layer on the surface of fiber can pre-
vent the diffusion between SiC fiber and matrix[8,9] .
Lin et al.[10] deposited Al2 O3 coating on the surface
of the short SiC fiber by arc ion plating, which alle-
viated the reaction between the fibers and Ni. How-
ever, macroparticles produced in the process had neg-
ative influences on the quality of the film. Larkin
† Corresponding author. Prof., Ph.D.; Tel.: +86 24 83978081;
E-mail address: csun@imr.ac.cn (C. Sun).
tion (CVD) to restrict the reaction between the SiC
fibers and NiAl matrix. Nevertheless, their research
was only focused on short SiC fibers, which cannot
satisfy the requirement in practical applications. In
order to solve these problems, (Al+Al2 O3 ) coating
was deposited on the surface of continuous C-coated
SiC fiber as diffusion barrier layer by reactive mag-
netron sputtering in our previous work[12] . It is feasi-
ble to use this kind of fiber to prepare nickel matrix
composite.
Solid-state diffusion bonding (SDB) is an impor-
tant technology for preparing metal matrix compos-
ite. It is a micro-deformation process in which metal
matrix and reinforcement is vacuum hot pressed to-
gether at an elevated temperature below the melting
point of the matrix. The key process in this method
is to prepare the preform of the composite. Physical
vapor deposition (PVD) is widely employed to pre-
pare precursor wire which can be easily arranged into
preform[13–15] . During PVD, precursor wire is pre-
pared by directly depositing matrix material on the
fiber. PVD can be used to solve the problem in pro-
ducing foil or powder with high melting point, e.g.
 L. Zhang et al.: J. Mater. Sci. Technol., 2011, 28(3), 234–240.
Fig. 1 Schematic diagram of procedure of preparing composite
nickel alloys, and it is also easy to control the vol-
ume ratio of fiber in composite. Magnetron sputter-
ing (MS) is one of the most widely applied methods
of PVD, which can deposit high-quality film and has
little influence on mechanical properties of sputtered
samples since the process is preformed at lower tem-
perature.
In this paper, MS was used to prepare precursor
wire by depositing nickel on the surface of continuous
(Al+Al2 O3 )-coated SiC fiber and SDB was employed
to prepare the composite. The influence of MS on
mechanical property of (Al+Al2 O3 )-coated SiC fiber
was examined. Meanwhile, preparation technology of
composite, the effect of (Al+Al2 O3 ) coating to restrict
the diffusion between SiC fiber and nickel matrix, and
the plastic flow mechanism of nickel matrix in SDB
process were discussed.
2. Experimental
Continuous (Al+Al2 O3 )-coated SiC fiber with Al
coating (∼50 nm in thickness) and Al2 O3 coating
(∼900 nm in thickness) on the surface of continu-
ous C-coated (∼2.5 μm in thickness) SiC fiber (IMR,
China) of ∼100 μm in diameter was used. The pu-
rity of Ni used as sputtering target was 99.99% and
the target was rectangular with a size of 272 mm×68
mm. The processing chamber was evacuated to a base
pressure of 3×10−3 Pa by mechanical pump and mole-
cular pump before sputtering. Argon was introduced
to the chamber by flow controller to keep the working
pressure 0.5 Pa during the sputtering. The sputtering
power was supplied by a pulsed power supply with a
power of 670 W and a pulse frequency of 30 kHz.
In the experiment, SDB was used to prepare com-
235
posite. As shown in Fig. 1, the precursor wires
(Fig. 1(a)) were arranged tightly in a plane and fixed
to be a precast slab (Fig. 1(b)) by a special binder.
The slab was then cut into smaller pieces and piled up
to be a preform (Fig. 1(c)) which fitted for the size of
the die in vacuum hot press equipment (Fig. 1(d)).
The preform was finally compressed to a compos-
ite by SDB (Fig. 1(e)). To avoid oxidation of the
metal, the vacuum hot pressing chamber was evacu-
ated to 5×10−2 Pa by mechanical pump and oil dif-
fusion pump during the heating stage. The temper-
ature in SDB process is in the range of 850–880◦ C,
the pressure is in the range of 30–70 MPa, and the
holding time is in the range of 1–2 h.
The morphologies and microstructures of the
precursor wires and composites were observed by
scanning electron microscopy (SEM) (Hitachi S-
3400N) and X-ray diffractometer (XRD, SHIMADZU,
D/Max-2500PC). Line-scanning results of cross sec-
tion were inspected by electron dispersive spec-
troscopy (EDS) (Hitachi S-3400N). Tensile strength
of the precursor wires and fibers was measured by us-
ing a miniature tensile machine, and the number of
the test samples was forty in one group.
3. Results and Discussion
3.1 Precursor wire
In our previous work[12] , (Al+Al2 O3 ) coating was
deposited as a diffusion barrier layer on the continuous
SiC fiber by MS. The results showed that (Al+Al2 O3 )
coating protected C-rich layer of SiC fiber and it is
beneficial of reducing surface residual stress of SiC
fiber. Meanwhile, it has little influence on mechanical
236 L. Zhang et al.: J. Mater. Sci. Technol., 2011, 28(3), 234–240.
Fig. 2 Surface and cross section morphology of precursor wire: (a) surface, (b) cross section)
property of SiC fiber. Thus, continuous (Al+Al2 O3 )-
coated SiC fiber is desirable to prepare precursor wire
of SiC fiber reinforced nickel matrix composite.
The surface and cross section morphology of pre-
cursor wire are shown in Fig. 2. In Fig. 2(a), the de-
posited nickel coating by MS process is in the form of
columnar crystal growing in radial direction. Fig. 2(b)
reveals that the nickel coating combines well with the
(Al+Al2 O3 ) fiber surface layer. Good combination
between (Al+Al2 O3 )-coated SiC fiber and nickel ma-
trix coating avoids abscission of matrix coating and
is beneficial to prepare composite in SDB process. In
addition, the diameter of SiC fiber is about 100 μm
and the thickness of nickel coating is about 32 μm.
Therefore, the volume ratio of SiC fiber in precursor
wire was about 37% by calculation.
At room temperature the average tensile strength
of (Al+Al2 O3 )-coated SiC fiber was 3.39 GPa. Thus,
the theoretical tensile strength of the precursor wire
was 1.38 GPa, according to the rule of mixture in
composite:
σc = σf Vf + σm (1 − Vf ) (1)
where, σc is the tensile strength of precursor wire, Vf
is volume ratio of SiC fiber in precursor wire, and σm
is the tensile strength of nickel target (σm =0.205 GPa
in our experiment).
Tensile testing results showed that the tensile
strength of the precursor wires prepared in the ex-
periment was 1.18 GPa, about 85.5% of the theoret-
ical value. After Ni coating of the precursor wire
was removed by corrosion, the tensile strength of
(Al+Al2 O3 )-coated SiC fiber was 3.30 GPa, which
was near to the value before the deposition process.
Therefore, the process of depositing nickel matrix
has little negative influence on tensile strength of
(Al+Al2 O3 )-coated SiC fiber.
In sum, the MS process is a proper way to prepare
the precursor wires for (Al+Al2 O3 )-coated SiC fiber
reinforced nickel matrix composite; the deposited Ni
coating combines well with the (Al+Al2 O3 ) coat-
ing and does not degrade the tensile strength of
(Al+Al2 O3 )-coated SiC fiber.
3.2 SiC fiber reinforced nickel matrix composite
In SDB process, the important technology para-
meters are temperature, pressure and holding time.
The temperature should be between 0.5 and 0.7 of
melting point of pure nickel (in absolute tempera-
ture), which is 1453 K[16] . Thus the recommended
SDB temperature is in the range of 590–935 ◦ C. On
one hand, high temperature helps to accelerate dif-
fusion rate of nickel matrix and shorten the time of
preparation. On the other hand, if the selected tem-
perature is too high, it will induce the undesirable
reaction at interface. With respect to the pressure,
higher pressure increases the plastic flow of nickel ma-
trix and decreases the amount of voids, while too high
pressure will damage either the coating on the surface
of the fibers or the fibers themselves. In addition,
holding time should be appropriate to achieve the re-
quired density but avoid the degradation of properties
of the interface and the composite. To these regards,
these three parameters should be optimized according
to practical SDB process.
Fig. 3 shows the morphology of the compos-
ites produced with different combinations of tem-
perature, pressure and holding time, including
850 ◦ C×30 MPa×1 h in Fig. 3(a), 850 ◦ C×
50 MPa×2 h in Fig. 3(b), 870 ◦ C×30 MPa×2 h
in Fig. 3(c), 870 ◦ C×50 MPa×2 h in Fig. 3(d),
880 ◦ C×50 MPa×2 h in Fig. 3(e), and 870 ◦ C×
70 MPa×2 h in Fig. 3(f). Voids with different shapes
and sizes are observed at the interface between precur-
sor wires in Fig. 3(a), Fig. 3(b) and Fig. 3(c), although
the fibers keep intact. The occurrence of these voids
at the interface between precursor wires indicates that
precursor wires did not diffuse adequately. Compared
with the quantity of voids in composite prepared at
850 ◦ C×30 MPa×1 h (Fig. 3(a)), the quantity of voids
in the composite prepared under higher pressure and
 L. Zhang et al.: J. Mater. Sci. Technol., 2011, 28(3), 234–240.
Fig. 3 Morphology of composite prepared at: (a) 850 ◦ C×30 MPa×1 h, (b) 850 ◦ C×50 MPa×2 h, (c) 870 ◦ C×
30 MPa×2 h, d) 870 ◦ C×50 MPa×2 h, (e) 880 ◦ C×50 MPa×2 h, and f) 870 ◦ C×70 MPa×2 h
longer holding time, i.e. 850 ◦ C×50 MPa×2 h
(Fig. 3(b)), does not obviously decrease. How-
ever, most of the voids became smaller, and
their shape changes from polygonal to triangular.
In contrast, when the temperature improved, i.e.
870 ◦ C×30 MPa×2 h, only some quite small voids
are observed, as shown in Fig. 3(c). With both
improved temperature and improved pressure, i.e.
870 ◦ C×50 MPa×2 h, no void is observed (Fig. 3(d))
and furthermore fibers are arranged in order, reveal-
ing that precursor wires diffused completely under
this condition. With further increased temperature,
i.e. 880 ◦ C×50 MPa×2 h, Fig. 3(e) shows that the dif-
fusion of precursor wires was adequate, but the mar-
gin of SiC fibers was not as smooth as that before
SDB process. At 870 ◦ C×70 MPa×2 h (Fig. 3(f)), the
fibers lost the original shape and (Al+Al2 O3 ) coat-
ing was not intact. These two samples revealed that
there are temperature and pressure limits in the SDB
process. When the temperature or the pressure is
higher than the limit, the effect of diffusion barrier
would be weakened and lead to undesirable diffusion
between SiC fiber and nickel.
Fig. 4 shows the SEM line-scanning of the interface
between SiC fiber and nickel matrix in the composite
prepared at 870 ◦ C×50 MPa×2 h. C-rich layer and
(Al+Al2 O3 ) coating were both as intact as that in
precursor wire, showing that Si did not diffuse to the
matrix and Ni did not react with the fiber. Calculated
by thermodynamics formula:
ΔGφ298 = ΔH298
φ φ
− T ΔS298 <0 (2)
Al2 O3 , SiC and Ni can coexist under 1000 ◦ C.
237
Thus, this intact (Al+Al2 O3 ) coating could restrict
interdiffusion of Ni and SiC, and protect SiC fiber.
As analyzed above, the optimum SDB parameters
for the nickel matrix composite with 37% volume ra-
tio of SiC fiber is obtained as 870 ◦ C×50 MPa×2 h
in the present experiment, under which adequate dif-
fusion of precursor wires is obtained and the effect of
the barrier layer (Al+Al2 O3 ) maintains.
Fig. 5 shows the XRD spectrum of nickel in pre-
cursor wire and in composite prepared at 850 ◦ C×
50 MPa×2 h. There are three crystal orientations
of nickel in XRD spectrum, including (111), (200)
and (220). In precursor wire, intensity ratio of (111),
(200) and (220) is 100:30.8:20.1, which is away from
100:43.2:18.0 in PDF card (No.65-2865). It indicates
that in precursor wire, Ni grains grow in preferred ori-
entation (111), which accords with the result shown
in Fig. 2(a). After SDB process, the intensity ratio
changes to 100:34.6:17.04, showing that the trend to
grow on (111) weakens. Meanwhile, the morpholo-
gies of tensile fracture surface in composite prepared
at 850 ◦ C×50 MPa×2 h (Fig. 6) indicated that the
columnar crystal of nickel existed near the void that
formed at the interface between precursor wires, and
disappeared if the precursor wires diffused completely.
Therefore, adequate diffusion of precursor wires dur-
ing SDB process weakens the preferred orientation of
Ni coating that forms during the preparation of pre-
cursor wires and will favor the mechanical properties
of the composite.
3.3 Plastic flow mechanism of nickel matrix
Derby and Wallach[17,18] developed a model of
238 L. Zhang et al.: J. Mater. Sci. Technol., 2011, 28(3), 234–240.

Fig. 5 XRD spectrum of nickel in precursor wire and in

composite prepared at 850 ◦ C×50 MPa×2 h

diffusion bonding and evaluated several mechanisms

Fig. 4 Line-scanning pattern of cross section of compos-
ite prepared at 870 ◦ C×50 MPa×2 h
which close the voids in the process. Based on
their model, Chen et al.[19] developed a model for
matrix-coated fiber reinforced composite, in which the
matrix-coated fibers are arranged in square hexago-
nal. This model shows a good agreement with the
experimental results of the consolidation process of
sapphire fiber-reinforced NiAl composites. The mech-
anisms developed in these two models were: (i) sur-
face diffusion, (ii) volume diffusion from surface, (iii)
evaporation-condensation, (iv) grain boundary diffu-
sion, (v) volume diffusion from interfacial sources, (vi)
power-law creep, and (vii) plastic flow.
Fig. 7 shows the process of plastic flow mechanism
of nickel matrix in our experiment. At the first stage
(Fig. 7(a)) before the pressure was applied, precur-
sor wires rearranged in hexagonal symmetry and a
quadrangular void formed between the adjacent pre-
cursor wires. Surface diffusion, volume diffusion, and
evaporation-condensation were the main mechanisms

Fig. 6 Different morphologies of nickel matrix in tensile fracture surface of composite prepared at
850 ◦ ×50 MPa×2 h: (a) columnar crystal of nickel; (b) columnar crystal of nickel disappeared
 L. Zhang et al.: J. Mater. Sci. Technol., 2011, 28(3), 234–240.
Fig. 7 Plastic flow mechanism of nickel matrix
controlling this stage[20] . Among these mechanisms,
volume diffusion was the most important mechanism
which caused the apiciform voids in the composite.
At the second stage (Fig. 7(b)) after pressure was
applied, the two surfaces bond immediately contacted
due to the very high contact stress and the quadrangle
void turned into two triangular voids. Plastic defor-
mation controlled this stage and it ceased when the
contact area at the interface was sufficient to support
the applied load, i.e. the local stress falls below the
material s yield stress.
At the third stage, the triangular void became
smaller (Fig. 7(c), (d)) and finally disappeared
(Fig. 7(e)). This stage was a time-dependent process,
and most of the seven mechanisms contributed to
the diffusion bonding, especially power-law creep and
grain boundary diffusion. Power-law creep mecha-
nism was developed from microcreep of asperities at
high temperature, and stress had much influence on
it. Grain boundary diffusion was affected by the grain
size.
During SDB process, all the mechanisms work to-
gether to influence the diffusion of precursor wires and
these mechanisms are affected by temperature, pres-
sure and holding time. Although higher temperature,
higher pressure and longer time contribute to the dif-
fusion of matrix, they are not of benefit to protect
diffusion barrier layer (Al+Al2 O3 ) or SiC fiber. Thus,
these three parameters should be optimized and con-
trolled under the limit values, as discussed in Section
3.2.
4. Conclusions
A method to prepare continuous (Al+Al2 O3 )-
239
coated SiC fiber reinforced nickel matrix composite
was presented in this paper. This method is advanta-
geous to prevent the diffusion between SiC fiber and
nickel matrix by using the MS in preparation of pre-
cursor wires and optimize SDB process in preparation
of the composite. The main conclusions can be drawn
as follows:
(1) MS process is a proper way to prepare the
precursor wire by depositing Ni coating in thickness
about 32 μm on the surface of (Al+Al2 O3 )-coated
SiC fiber; Ni coating combined well with (Al+Al2 O3 )
coating and it has little negative influence on tensile
strength of (Al+Al2 O3 )-coated SiC fiber.
(2) SDB process was optimized to prepare the
(Al+Al2 O3 )-coated SiC fiber reinforced nickel ma-
trix composite. The obtained optimum parameters
were 870 ◦ C×50 MPa×2 h when the volume ratio
of SiC fiber in precursor wires was about 37%. Un-
der this condition, precursor wires diffused adequately
and (Al+Al2 O3 ) coating effectively restricted the re-
action between SiC fiber and nickel matrix.
REFERENCES
[1 ] S.T. Mileiko, V.M. Kiiko, A.A. Kolchin, A.V. Sere-
bryakov, V.P. Korzhov, M. Yu Starostin and N.S.
Sarkissyan: Compos. Sci. Technol., 2002, 62(2), 167.
[2 ] J. Doychak: JOM, 1992, 44(6), 46.
[3 ] Y.C. Fu, N.L. Shi, D.Z. Zhang and R. Yang: Mater.
Sci. Eng. A, 2006, 426(1–2), 278.
[4 ] X.H. Lu, and Y.Q. Yang: Trans. Nonferrous Met.
Soc. China, 2006, 16(1), 77
[5 ] T. Yamada, H. Sekiguchi, H. Okamoto, S. Azuma, and
A. Kitamura: in Proc. 2nd Int. Symp. on Ceramic
Materials and Components for Engines, 1986, 441.
[6 ] R.C.J. Schiepers, F.J.J. Van Loo and G. de With: J.
 240 L. Zhang et al.: J. Mater. Sci. Technol., 2011, 28(3), 234–240.
Am. Ceram. Soc., 1988, 71, 284.
[7 ] T.C. Chou, A. Joshi and J. Wadsworth: J. Mater.
Res., 1991, 6, 796.
[8 ] W.M. Tang, Z.X. Zheng, H.F. Ding and Z.H. Jin: J.
Chin. Ceram. Soc., 2003, 31, 287. (in Chinese)
[9 ] Y.Q. Wang and B.L. Zhou: Compos. Pt. A-Appl. Sci.
Manuf., 1996, 27, 1139
[10] H.T. Lin, N.L. Shi, C. Sun, J. Gong and X.D. Sun:
Acta. Metall. Sin., 2007, 4, 444. (in Chinese)
[11] D.J. Larkin and L.V. Interrante: J. Mater. Res., 1990,
5(11), 2706.
[12] L. Zhang, N.L. Shi, J. Gong, Z.L. Pei, L.J. Gao and C.
Sun: Acta. Metall. Sin., 2011, 47, 497. (in Chinese)
[13] P.R. Subramanian, S. Krishnamurthy, S.T. Keller and
M.G. Mendiratta: Mater. Sci. Eng. A, 1998, 244, 1.
[14] Z.X Guo and B. Derby: Prog. Mater. Sci., 1995, 39,
411.
[15] Y.M. Wang, Y.C. Fu, N.L. Shi, D.Z. Zhang and R.
Yang: Acta. Metall. Sin., 2004, 40, 359. (in Chinese)
[16] C.S. Lee, H. Li and R.S. Chandel: J. Mater. Process.
Technol., 1999, 89–90, 326.
[17] B. Derby and E.R. Wallach: Met. Sci., 1982, 16, 49.
[18] B. Derby and E.R. Wallach: Met. Sci., 1984, 18, 427.
[19] H. Chen, Y. Zhong, W. Hu and G. Gottstein. Mater.
Sci. Eng. A, 2007, 452–453, 625.
[20] Y.M. Wang: Study on Fabrication, Interface Reaction
and Tensile Strength of Continuous SiC(f) /Ti-6Al-4V
Composite, Ph. D. Thesis, Institute of Metal Research,
Chinese Academy of Sciences, 2005. (in Chinese)