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 ber reinforced nickel matrix composite was presented, in which the diusion between SiC ber and nickel matrix could be prevented. Magnetron sputtering
is used to deposit Ni coating on the surface of the (Al+Al2 O3 )-coated SiC ber 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 eect on the tensile strength of (Al+Al2 O3 )-coated SiC ber. Solid-state diusion bonding process
is employed to prepare the (Al+Al2 O3 )-coated SiC ber reinforced nickel matrix with 37% bers in volume.
The solid-state diusion 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 diuse well, composite of full density can be formed and the (Al+Al2 O3 ) coating is eective to restrict the reaction between
SiC ber and nickel matrix.
KEY WORDS: SiC ber; Composite; Diusion barrier layer; Precursor wire

1. Introduction
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 mechanical properties of the matrix[24] , which makes it
an eective way to overcome those problems in nickel
alloys.
With respect to SiC ber reinforced nickel alloy
composites, the diusion reaction between SiC ber
and the matrix is so intense that the reinforced effect of SiC ber in nickel matrix is degraded[57] . A
diusion barrier layer on the surface of ber can prevent the diusion between SiC ber and matrix[8,9] .
Lin et al.[10] deposited Al2 O3 coating on the surface
of the short SiC ber by arc ion plating, which alleviated the reaction between the bers and Ni. However, macroparticles produced in the process had negative inuences on the quality of the lm. Larkin
Corresponding author. Prof., Ph.D.; Tel.: +86 24 83978081;
E-mail address: csun@imr.ac.cn (C. Sun).

et al.[11] deposited yttria by chemical vapor deposition (CVD) to restrict the reaction between the SiC
bers and NiAl matrix. Nevertheless, their research
was only focused on short SiC bers, 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 ber as diusion barrier layer by reactive magnetron sputtering in our previous work[12] . It is feasible to use this kind of ber to prepare nickel matrix
composite.
Solid-state diusion bonding (SDB) is an important technology for preparing metal matrix composite. It is a micro-deformation process in which metal
matrix and reinforcement is vacuum hot pressed together 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 prepare precursor wire which can be easily arranged into
preform[1315] . During PVD, precursor wire is prepared by directly depositing matrix material on the
ber. PVD can be used to solve the problem in producing foil or powder with high melting point, e.g.

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235

Fig. 1 Schematic diagram of procedure of preparing composite

nickel alloys, and it is also easy to control the volume ratio of ber in composite. Magnetron sputtering (MS) is one of the most widely applied methods
of PVD, which can deposit high-quality lm and has
little inuence on mechanical properties of sputtered
samples since the process is preformed at lower temperature.
In this paper, MS was used to prepare precursor
wire by depositing nickel on the surface of continuous
(Al+Al2 O3 )-coated SiC ber and SDB was employed
to prepare the composite. The inuence of MS on
mechanical property of (Al+Al2 O3 )-coated SiC ber
was examined. Meanwhile, preparation technology of
composite, the eect of (Al+Al2 O3 ) coating to restrict
the diusion between SiC ber and nickel matrix, and
the plastic ow mechanism of nickel matrix in SDB
process were discussed.
2. Experimental
Continuous (Al+Al2 O3 )-coated SiC ber with Al
coating (50 nm in thickness) and Al2 O3 coating
(900 nm in thickness) on the surface of continuous C-coated (2.5 m in thickness) SiC ber (IMR,
China) of 100 m in diameter was used. The purity of Ni used as sputtering target was 99.99% and
the target was rectangular with a size of 272 mm68
mm. The processing chamber was evacuated to a base
pressure of 3103 Pa by mechanical pump and molecular pump before sputtering. Argon was introduced
to the chamber by ow 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-

posite. As shown in Fig. 1, the precursor wires

(Fig. 1(a)) were arranged tightly in a plane and xed
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 tted for the size of
the die in vacuum hot press equipment (Fig. 1(d)).
The preform was nally compressed to a composite by SDB (Fig. 1(e)). To avoid oxidation of the
metal, the vacuum hot pressing chamber was evacuated to 5102 Pa by mechanical pump and oil diffusion pump during the heating stage. The temperature in SDB process is in the range of 850880 C,
the pressure is in the range of 3070 MPa, and the
holding time is in the range of 12 h.
The morphologies and microstructures of the
precursor wires and composites were observed by
scanning electron microscopy (SEM) (Hitachi S3400N) and X-ray diractometer (XRD, SHIMADZU,
D/Max-2500PC). Line-scanning results of cross section were inspected by electron dispersive spectroscopy (EDS) (Hitachi S-3400N). Tensile strength
of the precursor wires and bers was measured by using 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 diusion barrier layer on the continuous
SiC ber by MS. The results showed that (Al+Al2 O3 )
coating protected C-rich layer of SiC ber and it is
benecial of reducing surface residual stress of SiC
ber. Meanwhile, it has little inuence on mechanical

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Fig. 2 Surface and cross section morphology of precursor wire: (a) surface, (b) cross section)

property of SiC ber. Thus, continuous (Al+Al2 O3 )coated SiC ber is desirable to prepare precursor wire
of SiC ber reinforced nickel matrix composite.
The surface and cross section morphology of precursor wire are shown in Fig. 2. In Fig. 2(a), the deposited 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 ) ber surface layer. Good combination
between (Al+Al2 O3 )-coated SiC ber and nickel matrix coating avoids abscission of matrix coating and
is benecial to prepare composite in SDB process. In
addition, the diameter of SiC ber is about 100 m
and the thickness of nickel coating is about 32 m.
Therefore, the volume ratio of SiC ber in precursor
wire was about 37% by calculation.
At room temperature the average tensile strength
of (Al+Al2 O3 )-coated SiC ber 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:
c = f Vf + m (1 Vf )

(1)

where, c is the tensile strength of precursor wire, Vf

is volume ratio of SiC ber in precursor wire, and m
is the tensile strength of nickel target (m =0.205 GPa
in our experiment).
Tensile testing results showed that the tensile
strength of the precursor wires prepared in the experiment was 1.18 GPa, about 85.5% of the theoretical value. After Ni coating of the precursor wire
was removed by corrosion, the tensile strength of
(Al+Al2 O3 )-coated SiC ber was 3.30 GPa, which
was near to the value before the deposition process.
Therefore, the process of depositing nickel matrix
has little negative inuence on tensile strength of
(Al+Al2 O3 )-coated SiC ber.
In sum, the MS process is a proper way to prepare
the precursor wires for (Al+Al2 O3 )-coated SiC ber
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 ber.
3.2 SiC ber reinforced nickel matrix composite
In SDB process, the important technology parameters are temperature, pressure and holding time.
The temperature should be between 0.5 and 0.7 of
melting point of pure nickel (in absolute temperature), which is 1453 K[16] . Thus the recommended
SDB temperature is in the range of 590935 C. On
one hand, high temperature helps to accelerate diffusion rate of nickel matrix and shorten the time of
preparation. On the other hand, if the selected temperature is too high, it will induce the undesirable
reaction at interface. With respect to the pressure,
higher pressure increases the plastic ow of nickel matrix and decreases the amount of voids, while too high
pressure will damage either the coating on the surface
of the bers or the bers themselves. In addition,
holding time should be appropriate to achieve the required 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 composites produced with dierent combinations of temperature, pressure and holding time, including
850 C30 MPa1 h in Fig. 3(a), 850 C
50 MPa2 h in Fig. 3(b), 870 C30 MPa2 h
in Fig. 3(c), 870 C50 MPa2 h in Fig. 3(d),
880 C50 MPa2 h in Fig. 3(e), and 870 C
70 MPa2 h in Fig. 3(f). Voids with dierent shapes
and sizes are observed at the interface between precursor wires in Fig. 3(a), Fig. 3(b) and Fig. 3(c), although
the bers keep intact. The occurrence of these voids
at the interface between precursor wires indicates that
precursor wires did not diuse adequately. Compared
with the quantity of voids in composite prepared at
850 C30 MPa1 h (Fig. 3(a)), the quantity of voids
in the composite prepared under higher pressure and

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237

Fig. 3 Morphology of composite prepared at: (a) 850 C30 MPa1 h, (b) 850 C50 MPa2 h, (c) 870 C
30 MPa2 h, d) 870 C50 MPa2 h, (e) 880 C50 MPa2 h, and f) 870 C70 MPa2 h

longer holding time, i.e. 850 C50 MPa2 h

(Fig. 3(b)), does not obviously decrease. However, most of the voids became smaller, and
their shape changes from polygonal to triangular.
In contrast, when the temperature improved, i.e.
870 C30 MPa2 h, only some quite small voids
are observed, as shown in Fig. 3(c). With both
improved temperature and improved pressure, i.e.
870 C50 MPa2 h, no void is observed (Fig. 3(d))
and furthermore bers are arranged in order, revealing that precursor wires diused completely under
this condition. With further increased temperature,
i.e. 880 C50 MPa2 h, Fig. 3(e) shows that the diffusion of precursor wires was adequate, but the margin of SiC bers was not as smooth as that before
SDB process. At 870 C70 MPa2 h (Fig. 3(f)), the
bers lost the original shape and (Al+Al2 O3 ) coating 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 eect of diusion barrier
would be weakened and lead to undesirable diusion
between SiC ber and nickel.
Fig. 4 shows the SEM line-scanning of the interface
between SiC ber and nickel matrix in the composite
prepared at 870 C50 MPa2 h. C-rich layer and
(Al+Al2 O3 ) coating were both as intact as that in
precursor wire, showing that Si did not diuse to the
matrix and Ni did not react with the ber. Calculated
by thermodynamics formula:

T S298
<0
G298 = H298

(2)

Al2 O3 , SiC and Ni can coexist under 1000 C.

Thus, this intact (Al+Al2 O3 ) coating could restrict

interdiusion of Ni and SiC, and protect SiC ber.
As analyzed above, the optimum SDB parameters
for the nickel matrix composite with 37% volume ratio of SiC ber is obtained as 870 C50 MPa2 h
in the present experiment, under which adequate diffusion of precursor wires is obtained and the eect of
the barrier layer (Al+Al2 O3 ) maintains.
Fig. 5 shows the XRD spectrum of nickel in precursor wire and in composite prepared at 850 C
50 MPa2 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 orientation (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 morphologies of tensile fracture surface in composite prepared
at 850 C50 MPa2 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 diused completely.
Therefore, adequate diusion of precursor wires during SDB process weakens the preferred orientation of
Ni coating that forms during the preparation of precursor wires and will favor the mechanical properties
of the composite.
3.3 Plastic ow mechanism of nickel matrix
Derby and Wallach[17,18] developed a model of

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

composite prepared at 850 C50 MPa2 h

Fig. 4 Line-scanning pattern of cross section of composite prepared at 870 C50 MPa2 h

diusion bonding and evaluated several mechanisms

which close the voids in the process. Based on
their model, Chen et al.[19] developed a model for
matrix-coated ber reinforced composite, in which the
matrix-coated bers are arranged in square hexagonal. This model shows a good agreement with the
experimental results of the consolidation process of
sapphire ber-reinforced NiAl composites. The mechanisms developed in these two models were: (i) surface diusion, (ii) volume diusion from surface, (iii)
evaporation-condensation, (iv) grain boundary diusion, (v) volume diusion from interfacial sources, (vi)
power-law creep, and (vii) plastic ow.
Fig. 7 shows the process of plastic ow mechanism
of nickel matrix in our experiment. At the rst stage
(Fig. 7(a)) before the pressure was applied, precursor wires rearranged in hexagonal symmetry and a
quadrangular void formed between the adjacent precursor wires. Surface diusion, volume diusion, and
evaporation-condensation were the main mechanisms

Fig. 6 Dierent morphologies of nickel matrix in tensile fracture surface of composite prepared at
850 50 MPa2 h: (a) columnar crystal of nickel; (b) columnar crystal of nickel disappeared

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239

Fig. 7 Plastic ow mechanism of nickel matrix

controlling this stage[20] . Among these mechanisms,

volume diusion 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 deformation controlled this stage and it ceased when the
contact area at the interface was sucient 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 nally disappeared
(Fig. 7(e)). This stage was a time-dependent process,
and most of the seven mechanisms contributed to
the diusion bonding, especially power-law creep and
grain boundary diusion. Power-law creep mechanism was developed from microcreep of asperities at
high temperature, and stress had much inuence on
it. Grain boundary diusion was aected by the grain
size.
During SDB process, all the mechanisms work together to inuence the diusion of precursor wires and
these mechanisms are aected by temperature, pressure and holding time. Although higher temperature,
higher pressure and longer time contribute to the diffusion of matrix, they are not of benet to protect
diusion barrier layer (Al+Al2 O3 ) or SiC ber. Thus,
these three parameters should be optimized and controlled under the limit values, as discussed in Section
3.2.
4. Conclusions
A method to prepare continuous (Al+Al2 O3 )-

coated SiC ber reinforced nickel matrix composite

was presented in this paper. This method is advantageous to prevent the diusion between SiC ber and
nickel matrix by using the MS in preparation of precursor 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 m on the surface of (Al+Al2 O3 )-coated
SiC ber; Ni coating combined well with (Al+Al2 O3 )
coating and it has little negative inuence on tensile
strength of (Al+Al2 O3 )-coated SiC ber.
(2) SDB process was optimized to prepare the
(Al+Al2 O3 )-coated SiC ber reinforced nickel matrix composite. The obtained optimum parameters
were 870 C50 MPa2 h when the volume ratio
of SiC ber in precursor wires was about 37%. Under this condition, precursor wires diused adequately
and (Al+Al2 O3 ) coating eectively restricted the reaction between SiC ber and nickel matrix.
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