Metals and Materials International

https://doi.org/10.1007/s12540-019-00549-z

In‑Situ Synthesis of Aluminum Matrix Composite from Al–NiO System

by Mechanical Alloying
Samaneh Mamnooni1 · Ehsan Borhani1 · Davoud Bovand2

Received: 22 July 2019 / Accepted: 14 November 2019

© The Korean Institute of Metals and Materials 2019

Abstract
In this paper, Al-based composites reinforced by Alumina and Al–Ni intermetallic compounds have been successfully
fabricated by mechanical alloying technique. The intermetallic phase, i.e., NiAl, N­ iAl3, ­Ni2Al3, as well as Alumina, were
formed in the aluminum matrix by in situ solid-state reactions between pure Al and NiO powders. The effects of NiO content
(7–10–13 vol%) on the characteristics of the fabricated composites were examined, the hardness, wear properties, phase
constituent, and composite microstructure with different NiO content in particular. The results showed that the addition of
NiO to Al increases the formation of Al–Ni system intermetallic compounds and enhance the surface hardness. Further, it is
ascertained that Al–10 vol% NiO nanocomposite has better wear properties in comparison with samples with 7 and 13 vol%
NiO due to the better matrix integrity and reinforcement distribution in the Al matrix.

Keywords  Mechanical alloying · Al–NiO system · In situ nanocomposite · Wear test

1 Introduction and modulus [6, 11]. Hence, the superior interfacial bond-
ing strength may be achieved by an in situ synthesis through
Low-density aluminum-based metal matrix composites a chemical reaction, whether between the elements or
(MMCs), indeed, sound quite promising to be appropriate between elements and compound within the sintering pro-
for a wide variety of applications in aircraft and automotive cess or mechanical alloying. In situ production of aluminum
industries due to the importance of high specific strength, matrix composites was typically through one or more reac-
modules, strength-to-density ratio, and wear resistance tions between aluminum and ceramics such as S ­ iO2, ­TiO2,
[1–5]. and ­ZrO2 [12]. Few studies have still focused on Al–NiO
The mechanical properties of metal matrix composites systems, thus having inadequate information [6]. Several
are generally influenced by several parameters such as size, research papers have reported potential wear-critical appli-
shape, distribution of reinforcement particles, and the vol- cations for nickel aluminides [13, 14].
ume fraction, amongst which, the latter is the most signifi- The synthesis of ­AlxMey (Me = metal: Mg, Ni, Ti, etc.)
cant [6–8]. Nanostructures, with ultra-fine reinforcements intermetallic phases through a chemical reaction between
made through an in  situ fabrication, may be effectively metal oxide (MeO) particles and nearby aluminum matrix
retained by the solid-state techniques [2]. The good inter- led to the formation of such composites. These intermetal-
face of the matrix-reinforcement bonding is significantly lic grains begin to grow followed by the diffusion of corre-
contributed to achieving premier mechanical properties [9, sponding Me-atoms into the nearby matrix [1].
10]. Intermetallic compound-reinforced composites have In situ formation of aluminum matrix composites
shown considerable strength regarding their high strength (AMCs) takes place through numerous processing routes
that are classified based on the physical state of the reactant,
* Ehsan Borhani including solid–solid, liquid–solid, and liquid–liquid reac-
[email protected] tions. Typically, the solid–solid reaction has been the most
favorable process due to its reduced cost and influence on
1
Department of New Science and Technology, Nanomaterials the properties of the composite. In situ formation leads to a
Group, P.O. Box 35131‑19111, Semnan, Iran
much cleaner interface and stronger binding with the matrix
2
Department of Materials and Metallurgical Engineering,
Semnan University, P.O. Box 35131‑19111, Semnan, Iran

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as compared with reinforcements that are added externally where D is the average crystallite size, λ is the wave length
[2]. of incident rays, β is the full width (in radians) at half maxi-
Fine-grained metal matrix nanocomposites are success- mum intensity, and θ is the diffraction angle. The micro-
fully processed by mechanical alloying (MA) [7, 15–18]. structures of the milled powders and sintered specimens
The high-energy ball milling (HEBM) technique enhances were studied through scanning electron microscopy (SEM,
the reactivity of a powder mixture. Mechanosynthesis (MS), Leo.1455.vp.english). The densities of sintered samples
known as reactive milling, is an important HEBM-induced were determined via the Archimedes method. The Vickers
chemical reaction due to the availability of synthesizing microhardness of polished bulk samples was carried out via
nanocomposites with various compounds, such as metals, micro-Vickers hardness tester (BUEHLER Co, Germany)
oxides, and organic materials in different combinations [2, under a load of 200 g for 10 s. The microhardness measure-
19–22]. ment was performed five times for each sample to obtain a
The literature on the in  situ fabrication of Al matrix precise average value.
composite from mechanically alloyed Al–NiO system is yet To show the effect of NiO content on tribological
scarce. Accordingly, the present paper aimed to determine and wear behavior of the sintered samples wear test was
the impact of different NiO contents on the microstructure, employed using a pin-on-disk wear testing machine at an
phase formation, and wear properties of an aluminum matrix ambient atmosphere. A pin-on-disc, which permits rota-
reinforced by Alumina and nickel aluminide particle. tion of a flat specimen against a stationary pin or ball, was
used in the wear tests. All of the wear tests were carried out
under 20 N normal load using AISI 52100 steel pin (5 mm in
2 Experimental diameter) as the counter-face. The sliding speed and distance
were kept constant at 0.13 m/s and 500 m, respectively. The
Aluminum and NiO powder with an average particle size weight loss of the specimens was measured via a micro-
of ≤ 5 μm and ≤ 45 μm were purchased from Merck KGaA balance with a resolution of 0.1 mg. The following equation
(Darmstadt, Germany) and Sigma-Aldrich, respectively. was used to obtain the wear rate of specimens:
Mechanical alloying and powder metallurgy routes were
M
used to prepare Al matrix nanocomposite with 7, 10 and W= (2)
𝜌D
13 vol% of NiO. The initial Al and NiO powders were placed
in a planetary mill, and mechanical alloying was carried where W is the wear rate (­ mm3/m), M denotes mass loss
out using T4 steel vial (125 ml) containing stainless steel (g), and ρ (g/mm3) and D (m) are the density and sliding
balls with a diameter of 20 mm for 24 h. A ball-to-powder distance, respectively. The worn surface of the specimens
mass ratio of 10:1 and a rotation speed of 250 RPM was after the wear tests was also investigated via scanning elec-
employed. In order to minimize oxidation, the milling pro- tron microscopy.
cess was performed under a protective argon atmosphere.
Subsequently, the milled powders were  uniaxially pressed at
room temperature (250 MPa, 1 min hold time, Zinc Stearate 3 Results and Discussion
used as a die-wall lubricant) to form pellets with 20 and
10 mm diameter and height, respectively then the pellets 3.1 X‑Ray Diffraction
sintered at 600 °C for 1 h in a furnace under argon atmos-
phere and subsequently cooled down to room temperature Figure 1 shows the XRD pattern of Al–NiO powders after
in the furnace. The sintered compacts were mechanically 24 h milling. As can be observed, the sample with 7 vol%
polished using 1000 grit SiC papers in water and ultrasoni- NiO shows the presence of Al and NiO phases, indicating no
cally rinsed with distilled water to remove any probable reaction of primary powders by milling (Fig. 1a).
contamination. X-ray diffraction (XRD) with Cu ­Ka radia- The XRD pattern of Al–10 vol% NiO shows the existence
tion (k = 0.154 nm) was utilized to identify the phases in the of Al, ­Al2O3, and ­Al3Ni phases. Such oxide and intermetallic
mechanically alloyed powders and sintered specimens. The could have been formed as a result of thermite reaction in
Scherrer formula were used to calculate the mean crystal- the mill vial activated by high energy ball-mill according to
lite size of the milled and sintered sample according to the the following reactions:
following equation:
3NiO + 2Al → Al2 O3 + 3Ni + ΔH (3)
0.9𝜆
D= (1)
𝛽Cos𝜃
3Al + Ni → Al3 Ni (4)

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Fig. 2  XRD patterns of sintered nanocomposites. a Al–7 vol% NiO, b

Al–10 vol% NiO, c Al–13 vol% NiO

Fig. 1  XRD patterns of nanocomposites with different initial

NiO content after 24  h of milling process. a Al–7  vol% NiO, b
atoms produced from Eq. 3 could react with Al to form sev-
Al–10 vol% NiO, c Al–13 vol% NiO
eral kinds of intermetallic compounds such as A ­ l3Ni, ­Al3Ni2,
AlNi, and ­AlNi3. Based on the thermodynamic calculation
The XRD pattern of Al–13 vol% NiO shows the exist- [24], the intermetallic ­Al3Ni2 compound is more stable than
ence of Al, A­ l2O3, ­Al3Ni, and NiAl phases. By compar- the intermetallic ­Al3Ni one, and it most likely appears in the
ing the XRD pattern of Al–10 vol% NiO with Al–13 vol% sintered materials instead of ­Al3Ni [12].
NiO, it can be seen that the NiAl phase are formed only in
the sample with 13 vol% NiO. The structure of A ­ l3Ni2 may
Al3 Ni + Ni → Al3 Ni2 (5)
be considered as AlNi modification with every third diago-
nal plane of nickel atoms missing. In the case of increasing The average crystallite size of milled powders determined
nickel content (compared with stoichiometric A ­ l3Ni2), the by Scherrer’s formula is illustrated in Fig. 3. It can be seen
empty sites are filled gradually by nickel atoms, making the that the minimum Al crystallite size is associated with the
structure progressively more similar to AlNi [23]. sample with 13 vol% NiO powder. It seems that the increase
As shown by the XRD pattern in Fig. 1, it can be seen in ceramic-intermetallic with a higher content of NiO
that the powders peaks become broad, and their intensities enhances the milling process and results in finer crystallite
decrease as NiO content increases. Decreasing the peak size of powder due to changing the milling system from duc-
intensities as well as broadening, is due to the formation tile–brittle to brittle–brittle. In the milling of ductile–brittle
of higher ceramic–intermetallic content in the sample with components, the ductile metal particles get flattened by ball
higher NiO content. collisions and brittle particles fragmented and occluded by
Comparing the XRD pattern of Al–10 vol% NiO and
Al–13 vol% NiO, it can be evidently seen that in the sample
with 13 vol% NiO, the peak related to Al becomes weaker;
whereas the ­Al2O3, ­Al3Ni, and NiAl peaks become more
intense, which indicates the higher reaction of aluminum
due to the higher content of NiO.
Figure 2 shows the XRD patterns of sintered samples.
The result shows that the sample with 7 vol% NiO (Fig. 2a)
composed of Al, ­Al3Ni and ­Al2O3 phases, which such oxide
and aluminide phases are formed by the reaction of NiO
and Al during the sintering process according to Eqs. (3, 4).
In the case of the sintered Al–10 vol% NiO composite, the
XRD pattern shows the existence of ­Al2O3, ­Al3Ni, and Al
phases. The XRD pattern of the sintered Al–13 vol% NiO
Fig. 3  Crystallite size of nanocomposite powders as a function
sample (Fig. 2c) shows the presence of A­ l2O3, ­Al3Ni2, NiAl, of NiO volume fraction. a Al–7  vol% NiO, b Al–10  vol% NiO, c
­Al3Ni, and Al phases. It should be pointed out that active Ni Al–13 vol% NiO

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ductile metal, whereas in the brittle–brittle system, the brit- cold-welding, which leads to particle refinement instead of
tle components get fragmented during the milling and the particle coarsening.
absence of ductile component preventing any welding, and The SEM micrograph of the sintered sample is shown
their particle size get reduced continuously. In the case of in Fig. 5. According to Fig. 5a, it can be seen that the sam-
the sample with 13 vol% NiO, much of the Al content reacts ple with 7 vol% NiO displays a different morphology with
with NiO and forms an intermetallic phase together with homogeneous porosity distributed randomly and micro-
Alumina particle, and very little Al remains in the mixture, crack formed in the intermetallic region. During the sinter-
which changes the milling system from ductile–brittle to ing process, the reaction firstly occurs in the surface region
brittle–brittle [25]. of the compact. Thus, conventional heating in the furnace
induces the internal residual stress of the compact.
In Fig. 5a, a coarse block of Al can be seen, where inter-
3.2 SEM Microstructure metallic particles and Alumina are formed non-uniformly
on the surface of Al; with an increase in NiO content more
Figure 4 shows the SEM micrograph of Al–NiO powder intermetallic and Alumina phases are formed, and micro-
composites with different NiO content after 24 h milling. structure becomes finer and more uniform.
It can be clearly seen that with an increase in NiO content, According to Fig. 5a–c, it can be seen that the number of
the particle becomes smaller. The smaller particles related pores in the sample increase with increasing the intermetal-
to the formation of a higher content of ceramic/intermetallic lic particle volume fraction. Increasing NiO content means
phases in the sample with higher NiO content. more intermetallic particle formation that is accompanied by
In the case of Al–7 vol% NiO sample, cold welding and more cracks. It is known that the formation of intermetallic
deformation of the Al particles can be seen easily (Fig. 4a); accompanies a change in the volume fraction, leading to
in the case of Al–10 vol% NiO and Al–13 vol% NiO sam- induce the micro-crack in the brittle phase.
ples, the powders become smaller with less cold weld and
agglomeration. It should be emphasized that with an increase 3.3 Microhardness and Density Measurement
in NiO content, the milling system gradually changes from
ductile–ductile to ductile–brittle for Al/NiO and Al/Al–NiO The Vickers microhardness results of the sintered nano-
reaction products, respectively [25]. In the high content of composites, with different content of NiO, are shown in
NiO after reaction between Al and NiO, the brittle phases, Fig. 6. The results show that the hardness of the compos-
such as A ­ l2O3, ­Al3Ni, and AlNi are formed; these brittle ites increases with increasing the NiO content, leading to
particles can be placed in interfacial boundaries, and cold the formation of more Ni-rich nanometer-scale interme-
welding of ductile particles (Al) may become more diffi- tallic compounds that leads to increase in hardness of the
cult. Moreover, the fracture of powders predominates the nanocomposites [14] . Table 1 shows the density of sintered

Fig. 4  SEM images of nanocomposite powders after 24 h of milling process. a Al–7 vol% NiO, b Al–10 vol% NiO, c Al–13 vol% NiO

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Fig. 5  SEM images of the

polished surface of the samples
sintered at 600 °C. a Al–7 vol%
NiO, b Al–10 vol% NiO, c
Al–13 vol% NiO

Table 1  Density of investigated Sample Practical

composites after sintering in density (g/
600 °C cm3)

Al–7 vol% NiO 3.29

Al–10 vol% NiO 3.53
Al–13 vol% NiO 4.99

3.4 Wear Test

The dry sliding wear test results of the composites are shown

in Table 2. the results shows that the wear rate is too high
Fig. 6  Microhardness of nanocomposites as a function of NiO vol- for Al–7 vol% NiO composite, and it decreases significantly
ume fraction. a Al–7  vol% NiO, b Al–10  vol% NiO, c Al–13  vol%
with increasing the nickel oxide volume fraction, and inter-
NiO
metallic content for Al–10 vol% NiO composite. This can
be since the increase of hardness enhances the tribological
composite, it can be seen that with increase in NiO content properties of the composite materials. Wear rate then tends
the density increases, the highest density was related to sam- to increase slightly for Al–13 vol% NiO composite as com-
ple with 15 vol% NiO.  pared with Al–10 vol% NiO composite.

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Table 2  Wear rate of sintered nanocomposites. a Al–7  vol% NiO b leading to the deterioration of the wear properties. As can be
Al–10 vol% NiO c Al–13 vol% NiO seen in Fig. 7c, due to the presence of pores in the sample,
Sample Wear rate ­(mm3/m) the delamination wear occurs as a result of nucleation and
propagation of crack near the pores. The crack network will
Al–7 vol% NiO 0.11
be propagated to the surface, connected to each other, and
Al–10 vol% NiO 0.000014
product wear debris (Fig. 8c). It can be observed that wear
Al–13 vol% NiO 0.000038
debris of Al–13 vol% NiO with a mixture of plate lets and a
small number of powders (Fig. 8c), confirms that the major
wear mechanism related to the Al–13 vol% NiO sample is
The worn surface of the specimens was examined through delamination one.
the SEM technique to understand the wear characteristics Figure 7b shows the worn surface of the Al–10 vol% NiO
of the nanocomposites. Figure 7 illustrates the SEM micro- sample; as can be seen, the SEM micrograph shows less
graph of the worn surface after 500 meters of dry sliding. surface damage. The characteristics of the worn surface in
As can be seen, for the sample with 7 vol% NiO and 10 vol% the sample with 10 vol% NiO are clearly different compared
NiO, both abrasive and adhesive wear exist (Fig. 7a, b). As with the samples with 13 and 7 vol% NiO (Fig. 7a, c). In
can be observed in Fig. 7a, in the case of the Al–7 vol% the case of Al–10 vol% NiO (Fig. 8b), debris consists of
NiO sample, due to the presence of micro-crack and pores, mainly much smaller amount of large particle than those
the particle is easily polled out from the matrix that causes of the samples with 7 and 13 vol% NiO (Fig. 8a, c), which
the formation of rough wear track. Particle detachment indicates little particle fracture during wear process. The
is the main reason for the considerable weight loss of the worn surface becomes more homogenous and smoother for
Al–7 vol% NiO sample. The debris with the coarse detected the Al–10 vol% NiO composite.
particle is shown in Fig. 8a.
It can be clearly seen that the sample containing 13 vol%
NiO shows higher weight loss as compared to the sample
with 10 vol% NiO. In this case, similar to the Al–7 vol% 4 Conclusion
NiO sample, the presence of micro-crack, porosity between
intermetallic and oxide particles, as well as a meager amount In situ, Al-based nanocomposites with a different volume
of Al as a matrix, more importantly, lead to deterioration fraction of reinforcement are prepared from the Al–NiO
of wear properties. It should be pointed out that pores act system using mechanical alloying. The results show that
as stress concentration regions and crack generation origin, the milling of NiO and Al powders lead to the formation

Fig. 7  SEM images of worn

surfaces. a Al–7 vol% NiO, b
Al–10 vol% NiO, c Al–13 vol%
NiO

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Fig. 8  SEM images of wear

test debris. a Al–7 vol% NiO, b
Al–10 vol% NiO, c Al–13 vol%
NiO

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