Materials Chemistry and Physics 160 (2015) 352e358

Contents lists available at ScienceDirect

Materials Chemistry and Physics

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

Ni-AlxNiy coreeshell structured particle reinforced Al-based

composites fabricated by in-situ powder metallurgy technique
Wenqian Wu, Baisong Guo, Yang Xue, Rujuan Shen, Song Ni, Min Song*
State Key Laboratory of Powder Metallurgy, Central South University, Changsha 410083, China

h i g h l i g h t s

A new metal matrix composite (MMC) has been developed.

The developed MMC has a matrix/shell/core structure.

The developed MMC has both high strength and plasticity.

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

Article history: Ni-AlxNiy coreeshell structured particle reinforced aluminum based composites were fabricated using
Received 15 October 2014 in-situ powder metallurgy method. Scanning electron microscope, X-ray diffraction, density analysis,
Received in revised form hardness and compressive tests were used to investigate the effects of volume fraction of Ni particles and
13 March 2015
sintering atmosphere on the microstructures and mechanical properties of the composites. It has been
Accepted 29 April 2015
shown that compared to Ar sintering atmosphere, N2 atmosphere is active sintering atmosphere for
Available online 4 May 2015
fabricating the composites. The AlN formed during the sintering process, which can substantially in-
crease the density and hardness of the composites. The strength of the composites sintered under N2
Keywords:
Composite materials
atmosphere is higher than that of the composites sintered under Ar, while the ductility is slightly lower.
Sintering It can be confirmed that the Ni-AlxNiy coreeshell structures are of great benefit not only to increase the
Mechanical properties strength but also to remain the plasticity of the composites.
Microstructure © 2015 Elsevier B.V. All rights reserved.

1. Introduction
Due to the excellent mechanical properties including hardness,
strength and elastic modulus over the corresponding aluminum
alloys, particulate reinforced aluminum based composites (PRACs)
are widely used in aerospace, electronics and automobile
manufacturing industries [1e3]. Ceramic particles such as SiC,
Al2O3 and B4C are generally used as the reinforcements to fabricate
PRACs [4,5]. However, the great difference in thermal expansion
coefficient between the aluminum matrix and the ceramic re-
inforcements can easily result in weak interfacial bonding strength
[6,7]. In addition, cracks can be easily nucleated due to the brit-
tleness of the ceramics, thus to severely decrease the mechanical
properties of composites, particularly the plasticity. Furthermore,
the size ratio of the original ceramic reinforcements and matrix
* Corresponding author.
E-mail address: msong@csu.edu.cn (M. Song).
constrain the volume fraction of the reinforcements and their dis-
tribution [8]. Recently, intermetallic compounds such as Al3Ti, Al3Fe
and Al3Ni reinforced Al matrix composites fabricated by in-situ
powder metallurgy technique were regarded as possible alterna-
tives for ceramic reinforced composites to significantly improve the
interfacial bonding strength [9e11]. The composites prepared by
in-situ powder metallurgy technique offer advantage that the dis-
tribution of the reinforcements is more uniform, which can give
rise to better mechanical properties. It should be noted that
although the in-situ intermetallic compound reinforced Al-based
composites have high strength due to enhanced interfacial
bonding strength, their plasticity might also be low because of the
high brittleness of the intermetallic compounds [12]. The brittle
fracture occurs easily on the intermetallic compounds when the
applied stress is transferred from Al matrix to the intermetallics
during deformation, and the length of the cracks is similar to the
size of the intermetallic compounds.
Recently, we have successfully fabricated Fe-AlxFey coreeshell
structured particle reinforced Al-based composites by in-situ

http://dx.doi.org/10.1016/j.matchemphys.2015.04.051
0254-0584/© 2015 Elsevier B.V. All rights reserved.
 W. Wu et al. / Materials Chemistry and Physics 160 (2015) 352e358 353

powder metallurgy technique [13,14]. Mechanical testing results

showed that these composites have both high strength and plas-
ticity. The high strength results from the fact that the externally
applied stress can be transferred from Al matrix to hard AlxFey shell
during deformation, while the large plasticity is due to the fact that
the crack propagation can be effectively inhibited because the soft
Al matrix and Fe core can blunt two tips of each crack. Based on our
previous work, a new Ni-AlxNiy coreeshell structured particle
reinforced Al-based composite was fabricated by in-situ powder
metallurgy technique in this article. The reinforcements in the
composites also consist of a coreeshell structure with the hard
AlxNiy intermetallic compounds being the shell and soft pure Ni
being the core. The composites with this special coreeshell struc-
tured reinforcements can significantly increase the strength of the
composites and retain the plasticity simultaneously.

2. Experimental

The initial materials used in the experiments were gas atomized

Al powder with an average size of ~40 mm (99.8% in purity) and
commercially pure Ni powder with an average size of ~38 mm
(99.9% in purity). The Al and Ni powders were blended for 8 h using
a planetary powder mixer with a rotation speed of 300 rotation per Fig. 1. XRD patterns of (a) Al-1 vol.%Ni, (b) Al-3 vol.%Ni and (c) Al-5 vol.%Ni composites
minute (rpm) under argon atmosphere. The volume fraction of the after sintering under Ar atmosphere.

Ni powder is 1 vol.%, 3 vol.% and 5 vol.%, respectively, with the ball

to powder weight ratio being 3:1. The anhydrous ethanol was used
only on thermodynamics but also on diffusion Kinetics. The for-
as a liquid medium. After blending the powders were dried in a
mation of intermetallic compounds at the interface between Al and
vacuum oven at 85  C for 8 h. Then the powders was die-pressed
Ni is a nonequilibrium process during solid-state interfacial reac-
under a pressure of 400 MPa (double-action compaction) in a cy-
tion. Under Ar atmosphere, the reaction between Al and Ni is
lindrical steel die with a diameter of 10 mm at room temperature,
exothermic and thus the Al3Ni2 phase forms at the AleNi interface
using zinc stearate as the lubricant. The thickness of the green
as a shell.
compacts is 7 mm. Subsequently, the green compacts were sintered
Fig. 2 shows that the composites sintered under N2 atmosphere
at 530  C under argon (Ar) or N2 atmosphere (with a pressure of
mainly include five phases, Al, Ni, Al3Ni, Al3Ni2 and AlN phases. It
10 MPa), respectively, with a heating rate of 10  C per minute. At
can thus be concluded that N2 can react with Al to form AlN phase
530  C, all the compacts were sintered for 5 h.
during the sintering process, and N2 atmosphere can significantly
The bulk densities and the porosity of the composites were
affect the chemical reaction between Al and Ni. It has been estab-
measured via the standard Archimedes method. X-ray diffraction
lished that AlN forms when the deep of pore network becomes
(XRD) with Cu Ka (k ¼ 0.154 nm) radiation was utilized to identify
essentially oxygen-free through a self-gettering process of
the phases present in the sintered specimens. The microstructures
of the sintered specimens were analyzed by a FEI nano230 field
emission scanning electron microscope (SEM) equipped with an
energy dispersive X-ray spectroscope (EDX). The Brinell hardness
was tested by applying 62.5 Kg load for 30 s. Each datum was the
average value of 4 independent tests. The compressive properties of
cylindrical samples (diameter of 3 mm and height of 5 mm)
machined from the specimens at ambient temperature were tested
using an Instron 3369 universal testing machine at a cross head
speed of 1 mm per minute. The yield strength was determined as
the 0.2 pct offset.

3. Results and discussion

3.1. XRD patterns

Figs. 1 and 2 show the XRD patterns of the composites sintered

under Ar and N2 atmosphere, respectively. It can be seen from Fig. 1
that the composites sintered under Ar atmosphere mainly include
three phases, Al, Ni and Al3Ni2 phases. As the volume fraction of Ni
increases from 1 vol.% to 5 vol.%, the intensity of Al3Ni2 peaks also
increases, indicating that the content of Al3Ni2 increases with the Ni
volume fraction. According to AleNi binary phase diagram [15],
there are five stable intermetallic compounds, Al3Ni, Al3Ni2, AlNi,
Al3Ni5 and AlNi3 with increasing the Ni content. Al3Ni and Al3Ni2
have been detected by XRD in this work. Generally, the formation of Fig. 2. XRD patterns of (a) Al-1 vol.%Ni, (b) Al-3 vol.%Ni and (c) Al-5 vol.%Ni composites
the intermetallic compounds in AleNi binary system depends not after sintering under N2 atmosphere.
354 W. Wu et al. / Materials Chemistry and Physics 160 (2015) 352e358
aluminum [16]. In self-gettering process, the outside Al powders of
the compacts act as a getter for the inner Al powders, and finally the
oxygen concentration becomes low enough for the formation of
AlN [17]. The formation of AlN is strongly exothermic [18], which
may result in an increase in local temperature, thus promote the
interdiffusion between Al and Ni and affect the solid-state inter-
facial reaction. In that case, both Al3Ni and Al3Ni2 are likely to exist
in the composites sintered at 530  C under N2 atmosphere.
3.2. SEM microstructures
Fig. 3a and b shows the back scattered SEM images of the com-
posites with 1 vol.% Ni sintered under Ar atmosphere. It can be seen
from Fig. 3a that two types of the reinforcements including coree-
shell structured particles and complete intermetallic particles can be
clearly observed in the matrix. Fig. 3b shows a coreeshell structured
particle with a grey shell and a white core. Line scanning of the
particle shows that the core is pure Ni, while the shell includes both
Ni and Al. Combined with the XRD result shown in Fig. 1a it can thus
be concluded that the reinforcements consist of Al3Ni2 intermetallic
shell and Ni core. It should be noted that some pores exist along the
interface between the Al matrix and reinforcements, and also be-
tween the Al powders. The pores are resulted from three possible
reasons. First, oxide layer that formed on the surface of the Al or Ni
powders can inhibit the elements diffusion and thus substantially
degrade the solid-phase-sintering ability [13,14,19]. Second, the
unbalance diffusion between Al and Ni results in pore generation on
the Al side of AleAl3Ni2 interface during the solid-phase-sintering, a
phenomenon called Kirkendall's effect [13,14]. Third, pores will be
nucleated for the purpose of relaxing the internal stress that
Fig. 3. Back scattered SEM microstructures and EDS line scanning of Al-1 vol.%Ni composite sintered under (a, b) Ar and (c, d) N2 atmosphere, respectively.
generated by the volume change during the formation of Al3Ni2
phase.
Fig. 3c and d shows the back scattered SEM images of the
composites with 1 vol.% Ni sintered under N2 atmosphere. It can be
seen from Fig. 3c that the reinforcements consist of three types of
the reinforcements including complete intermetallic particles,
core-one-layer-shell structured particles and core-two-layer-shell
structured particles. The complete intermetallic particles are the
dominant reinforcements and the core-one-layer-shell structured
particles are NieAl3Ni2 reinforcements. Fig. 3d shows the line
scanning of a core-two-layer-shell structured particle. The shell
consists of a two-layered structure with different Al and Ni con-
tents. Combined with XRD result shown in Fig. 2a and EDX analysis
shown in Fig. 3d, it can be concluded that the shell has a Al3Ni-
eAl3Ni2 two-layer intermetallic structure. It can be seen from
Fig. 3b and d that the volume fraction of the pores at Al-
intermetallic interface in the composites sintered under N2 atmo-
sphere is much less than that in the composites sintered under Ar
atmosphere. This phenomenon indicates that N2 atmosphere has a
positive effect on the densification of the composites during sin-
tering process. Schaffer et al. [17] indicated that, under N2 atmo-
sphere, Al matrix will react with N2 in the pores by in-situ route and
generate AlN layer, thereby to reduce the pressure in the pores and
thus to improve density of the composites. EDS elemental maps of
Al, Ni and N for the sample with 1 vol.% Ni sintered under N2 are
shown in Fig. 4. Elemental map distribution demonstrates the
presence of Al, Ni and N in the sample, and most N atoms is
concentrated on the interfaces between different phases. From the
line scanning in Fig. 3d, it can be seen that most of the AlN dis-
tributes on the interface between Al phase and intermetallics. The
 W. Wu et al. / Materials Chemistry and Physics 160 (2015) 352e358 355

Fig. 4. (a) SEM microstructure and EDS elemental maps of (b) Al, (c) Ni, (d) N for Al-1 vol.%Ni composite sintered under N2 atmosphere.

reaction area of Al and N2 is mainly on the interfaces between Al
and intermetallics, in which kirkendall-pores form because of the
unbalance diffusion between Al and Ni. The volume fraction of
pores at the interfaces between Al and intermetallics increases with
increasing the Ni content from 1% to 5%, thereby to increase the
contact area between Al and N2. As a result, the content of AlN
generated by the reaction between Al and N2 increases with
increasing the Ni content from 1% to 5%, as shown in Fig. 2. The
formation of AlN can be described as:
highly exothermic reaction, it will promote the interdiffusion be-
tween Al and Ni and then enhance the sintering process. As a
consequence, the number of the coreeshell structured re-
inforcements in the composites after sintering under N2 atmo-
sphere is significantly lower than that under Ar atmosphere, and
the main reinforcements are complete intermetallic particles, as
shown in Fig. 3a and c.
3.3. Density and porosity evolutions

Fig. 5 shows that the density of the composites sintered under

1
Al þ N2 /AlN (1) both Ar and N2 atmosphere increases with the Ni content, due to
2 the fact that Ni has a larger density than Al. Fig. 6 shows the
The reaction is highly exothermic with the Df HAlN 0 porosity of the composites sintered under Ar and N2 as a function of
being 318 kJ mol1 [20]. If the temperature rises because of the the Ni content. Figs. 5 and 6 indicate that the density are higher and

Fig. 5. Density of the composites sintered under different atmosphere as a function of Fig. 6. Porosity of the composites sintered under different atmosphere as a function of
the Ni content. the Ni content.
356 W. Wu et al. / Materials Chemistry and Physics 160 (2015) 352e358
Fig. 7. Hardness of the composites sintered under different atmosphere as a function
of the Ni content.
the porosity are lower for the composites sintered under N2 at-
mosphere than those of the composites sintered under Ar atmo-
sphere, respectively. From Fig. 3b and d it is known that the volume
fraction of the pores at Al-intermetallic interface in the composites
sintered under N2 atmosphere is much less than that in the com-
posites sintered under Ar atmosphere. All the above mentioned
factors confirm that N2 atmosphere has advantageous to the
densification of the composites.
3.4. Mechanical properties
Fig. 7 depicts the hardness of the composites sintered under
Fig. 8. The compressive testing curves of (a) Al-1 vol.%Ni and (b) Al-5 vol.%Ni composites sintered under Ar, (c) Al-1 vol.%Ni and (d) Al-5 vol.%Ni composites sintered under N2,
respectively.
both Ar and N2. As the Ni content increases from 1 vol.% to 5 vol.%,
the hardness of the composites sintered under both Ar and N2 in-
creases because of the higher hardness of the formed intermetallics
than that of Al. The composites sintered under N2 have higher
density and a larger quantity of the intermetallics, resulting in the
higher hardness of composites. Besides, the formation of AlN with
high hardness is beneficial to the hardness of the composites sin-
tered under N2.
Fig. 8a and b shows the compressive strain-stress curves of
composites with 1 vol.% Ni and 5 vol.% Ni after sintering under Ar
atmosphere, respectively. It can be seen from Fig. 8a and b that
although the composites sintering under Ar have similar yield
strength of ~107 MPa, the ultimate compressive strength decreases
from ~240 MPa to ~218 MPa and the ductility decreases from 40.9 %
to 33.5 % with the Ni content increasing from 1 vol.% to 5 vol.%. The
decreases in the ultimate compressive strength and ductility are
due to three possible reasons. First, when the Ni content increases
form 1 vol.% to 5 vol.%, more intermetallic compounds will be
formed in the composites after sintering, accompanied by the in-
crease in the number of pores between Al matrix and intermetallic
compounds. It should be noted that the pores located in the
interface between the Al matrix and intermetallic compounds will
inhibit the stress being transferred from Al matrix to re-
inforcements since the stress will be released from the pores, and
thus severely decrease the mechanical properties. Second, pores
can act as crack sources during deformation. Once the externally
applied stress reaches a critical value, the crack will propagate, and
the critical stress for crack propagation depends on the pore size.
The larger the pore size, the smaller the critical stress. Third,
dislocation glide can be prevented by the pores at the interface
between Al matrix and intermetallic compounds, which results in
the decrease of ductility.
Fig. 8c and d shows the compressive strain-stress curves of the
 W. Wu et al. / Materials Chemistry and Physics 160 (2015) 352e358 357

Fig. 9. Macro-photos of the specimens before and after compression.

composites with 1 vol.% and 5 vol.% Ni after sintering under N2 cracks mainly nucleated along the intermetallic Al3Ni2 shell, with
atmosphere, respectively. It can be seen from Fig. 8c that the the length similar to the thickness of the shell. During deformation,
average yield strength, ultimate compressive strength and ductility the Al matrix will transform the stress to the reinforcements. Once
of the composites with 1 vol.% Ni are ~125 MPa, ~257 MPa and the stress concentration on the reinforcements reaches a critical
~34.7%, respectively. However, when the Ni volume fraction in- value, cracks will nucleate in the intermetallic Al3Ni2 shell. How-
creases to 5%, the ductility of the composites is only ~3% despite of ever, the cracks cannot propagate easily since the two tips will be
the high yield strength (~343 MPa) and ultimate compressive blunted due to the high toughness of the Al matrix and Ni core,
strength (~346 MPa). Two reasons might account for this phe- because the plastic deformation of Al matrix and Ni core can relieve
nomenon. First, the distribution of AlN with high hardness is the stress concentration and prevent the crack propagation. That
similar to net in the composites, and it is easy to result in brittle means the Ni-AlxNiy coreeshell structures are beneficial to the
fracture of composites. On the other hand, a large number of plasticity of the composites. Thus, the Ni-AlxNiy coreeshell struc-
intermetallic compounds with high brittleness and hardness can tures are of great benefits not only to increase the strength but also
significantly reduce the plasticity of the composites. to remain the plasticity of the composites.
Fig. 9 illustrates the macro-photo of the specimens, including
undeformed composite (diameter of 3 mm and height of 5 mm),
4. Conclusion
deformed composite with 1 vol.% Ni sintered under Ar and
deformed pure Al. It can be seen from Fig. 9 that both the composite
In this paper, Ni-AlxNiy coreeshell structured PRMMCs were
and Al were compressed from cylinder shape to drum shape,
fabricated by in-situ powder metallurgy. The Ni-AlxNiy coreeshell
indicating that both materials have good ductility due to the
structures are of great benefits not only to increase the strength but
continuously deformation without tearing. After sintered under Ar
also to remain the plasticity of the composites. The conclusions can
for 5 h, the pure Al fabricated using the same route has a yield
be summarized as follows:
strength of ~87 MPa and super high ductility since it doesn't frac-
ture during the whole test process. Compared to pure Al, the
(1) Under N2 sintering atmosphere, N2 can react with Al to form
composites sintered under Ar can increase the yield strength and
AlN phase during the sintering process. The formation of AlN
remain a good plasticity simultaneously, as is shown in Fig. 8a and
can enhance the sintering process and thus to reduce the
b. Compared to the mechanical properties (~81 MPa in yield
pressure in the pores and increase the interfacial bonding
strength, ~220 MPa in ultimate compressive strength and ~42.8% in
strength.
ductility) of the pure Al fabricated using the same route, the com-
(2) With increasing the Ni content, the density and hardness of
posites with 1 vol.% Ni after sintered under N2 for 5 h have a sig-
the composites increase. Compared to the composites
nificant increase in the strength, and without much expense of the
plasticity, as is shown in Fig. 8c. It is confirmed that both Ar and N2
have a positive effect on increasing the strength of composites.
Comparing Fig. 8a and c, the yield strength and ultimate
compressive strength of the composites after sintering under N2
atmosphere are obviously higher than those under Ar atmosphere,
due to the high density of the composites after sintering under N2
atmosphere. While the ductility of the composites after sintering
under N2 atmosphere decreases. The number of the coreeshell
structured reinforcements in the composites sintered under Ar
atmosphere is significantly higher than that in the composite sin-
tered under N2 atmosphere, resulting in a higher ductility of the
composites sintered under Ar. The high plasticity of the composites
with a large number of the coreeshell structured reinforcements is
due to the fact that the crack propagation can be effectively
inhibited because the soft Al matrix and Ni core can blunt two tips
of each crack. In addition, the formation of AlN phase with high
brittleness is harmful to the ductility of the composites sintered
under N2.
Fig. 10 shows the back scattered SEM image of the composite
(with 1 vol.% Ni and after sintering under Ar atmosphere) close to
Fig. 10. Back scattered SEM image of the Al-1 vol.%Ni composite sintered under Ar
the fractural surface after compression. It can be seen that the atmosphere after compression.
358 W. Wu et al. / Materials Chemistry and Physics 160 (2015) 352e358
sintered under Ar, the composites sintered under N2 have
higher density and hardness, due to the fact that the volume
fraction of the pores in the composites is much less and the
formed intermetallic shell has a higher hardness than Al.
(3) The strength of the composites sintered under N2 is higher
than that sintered under Ar because of the high density,
while the ductility is slightly lower due to the less number of
the NieAl3Ni2 coreeshell structured reinforcements in the
composites.
Acknowledgments
The financial supports from National Natural Science Founda-
tion of China (51301206), the China Postdoctoral Science Founda-
tion (2013M531806), and the China Postdoctoral International
Exchange Program are appreciated.
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