Materials Today Communications: 2 2 Ji-Dong Zhang, Lan Zhang, Hui-Zhong Ma

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Materials Today Communications 37 (2023) 107437

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Materials Today Communications


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

Effect of ZrO2 additions on the microstructure, mechanical and wear


properties of ZrO2/7075 aluminium alloy composite
Ji-dong Zhang , Lan Zhang *, Hui-zhong Ma *
School of Mechanics and Engineering Science, Zhengzhou University, Zhengzhou 450000, China

A R T I C L E I N F O A B S T R A C T

Keywords: In this study, to improve the comprehensive performance of aluminium matrix composites, a 7075 aluminium
Aluminium composite alloy reinforced with ZrO2 particles was successfully fabricated via spark plasma sintering (SPS). Moreover, the
Microstructure effects of ZrO2 addition on the micromorphology, mechanical and wear properties of the composites were
Spark plasma sintering (SPS)
investigated. Microstructural analysis revealed that the pinning effect of the ZrO2 particles restrained grain
Mechanical properties
Wear properties
growth and induced a more significant grain size reduction. The addition of ZrO2 resulted in an initial increase
and subsequent decrease in density, hardness, ultimate tensile strength and elongation. The fracture surface of
the composites was characterised by homogeneous dimples, indicating that the fracture mode of materials is
ductile fracture mode. When 4 wt% ZrO2 was added, the density, hardness, tensile strength, elongation and wear
rate of the composites were higher than those of 7075Al aluminum alloy., reaching 97.23 %, 152.54 Hv, 376
MPa, 14 % and 0.9 × 10− 3 mm3/N⋅m, respectively. A significant increase in the dislocation density relative to the
aluminium alloy was obtained by adding ZrO2. With the addition of ZrO2, the wear resistance of ZrO2/7075Al
composites is superior to 7075 matrix alloy. The wear mechanism changed from adhesive to abrasive wear.

1. Introduction of the composite reached 399 MPa, 492 MPa, and 9.6 %, respectively.
Zou et al. [11] studied carbon nanotubes coated with TiO2-reinforced Al
The utilization of suitable lightweight materials to fabricate certain 7075 composites fabricated via ultrasonic assisted casting. They found
vehicle and airplane components and equipment can considerably that the composites achieved the highest hardness (171.1 Hv) after
reduce energy consumption and alleviate environmental constraints [1, aging time for 18 h. The hardness, yield strength, and ultimate tensile
2]. Owing to their low density, high strength and ease of manufacturing, strength of the composites reached 163.8 Hv, 262.4 MPa, and 338.1 MPa
aluminium alloys are used extensively in engineering materials, auto­ after aging time for 24 h, respectively. Vithal et al. [12] investigated the
mobiles, and aircraft that include transmissions, brake discs, wheels, effects of ZrB2 addition on the micromorphology and mechanical char­
wings, and fuselage skins [3,4]. However, with the advancement of acteristics of composites fabricated via stir casting. The micrographs
science and technology, the performance requirements have become displayed a significant accumulation of dislocations near the grain
more severely. Single aluminium alloys cannot meet all the standards for boundary. With a ZrB2 content of 10 %, the tensile strength reached
lightweight materials. In addition, the application of aluminum alloys in 360.42 MPa, resulting in significantly improved wear resistance. Ac­
tribological field is limited because of their relatively poor wear prop­ cording to Zhang et al. [13], the hardness and elastic modulus of Al 7075
erties [5–7]. As a result, aluminum matrix composites (AMCs) have composites reinforced with 0.3 % GNTs (carbon nanotubes) exceeded
attracted significant interest as they offer a good balance between those of Al 7075. The wear rate of Al 7075/GNTs composite was
weight reduction and other excellent properties [8,9]. 0.00273 mm3/ (N⋅m), while that of Al 7075 was 0.00342 mm3/ (N⋅m).
In recent years, researchers have employed various methods to Owing to their high specific strength and adaptability, AMCs have been
enhance the properties of aluminum alloys. Jiang et al. [10] developed a utilised for turbopump housings in liquid propulsion engines [14,15].
SiC/7075 aluminum composite by semi-solid processing (SSP). The The use of aluminium alloys as the primary material for automotive
microstructures displayed a presence of liquid phases and spheroidal suspension components can lead to weight reductions of up to 40 %.
solid grains. The yield strength, ultimate tensile strength, and elongation Recent research have demonstrated the potential of ZrO2 as a

* Corresponding authors.
E-mail addresses: [email protected] (L. Zhang), [email protected] (H.-z. Ma).

https://doi.org/10.1016/j.mtcomm.2023.107437
Received 4 September 2023; Received in revised form 14 October 2023; Accepted 26 October 2023
Available online 28 October 2023
2352-4928/© 2023 Elsevier Ltd. All rights reserved.
J.-d. Zhang et al. Materials Today Communications 37 (2023) 107437

reinforcing phase in metal matrix composites owing to its stable crystal Table 1
structure, high melting point, stable chemical properties, excellent Chemical composition of Al 7075 (wt%).
thermal insulation properties, and high room-temperature fracture Zn Si Mg Cu Cr Fe Mn Ti Others Al
toughness. Besides, the thermal expansion coefficient of ZrO2 is close to
5.6 0.4 3.2 1.7 0.2 0.8 0.2 0.2 0.3 Bal.
that of Al alloy, which enhances the adhesion between the two mate­
rials. In SPS sintering process, ZrO2 basically does not undergo phase
transformation [16,17]. Thus, researchers have investigated the appli­ shown in Fig. 1.
cation scope of ZrO2 toward the improvement in the performance of Using a planetary ball mill (XQM-2, Changsha Tianchuang Powder
metal matrix composites. M. Ghanbariha et al. [18] produced Technology Co., Ltd., China), 0, 2, 4, 6, and 8 wt% of ZrO2 particles were
ZrO2/AlCoCrFeNi composites using SPS methods and found that adding dispersed into the 7075Al matrix for 4 h at a speed of 300 rpm with a
5 wt% ZrO2 to AlCoCrFeNi improved slightly in wear rate. When the ball-to-power mass ratio of 5:1. Steel balls of four different sizes (di­
ZrO2 content was increased to 10 wt%, the hardness increases from 3.42 ameters of 6 mm, 8 mm, 10 mm, and 12 mm) with an equal weight ratio
to 4.48 GPa and the wear resistance was considerably enhanced. P Haja were used as the milling media. The selection of different sizes of
Syeddu Masooth et al. [19] studied that ZrO2 reinforced Ti6Al4V com­ grinding balls is to make the powder mix more uniform.
posites fabricated through powder metallurgy method. The strong
interfacial bonding resulted in composite with a hardness of 128 Hv and 2.2. Preparation of Al 7075 and Al 7075 /ZrO2
a compression strength of 270 MPa. Gunasekaran et al. [20] demon­
strated that Al 7075 alloy composites with varying ZrO2 content could Powder mixtures containing different mass fractions (0, 2, 4, 6, and
be successfully fabricated via the compo-casting process. The casting 8 wt%) of ZrO2 were sintered by employing the SPS process (SPS-10 T-5,
temperature was up to 800 ◦ C, and the maximum hardness and ultimate Shanghai Chenhua Electric Furnace Co., Ltd., China). The hot-pressing
tensile strength reached 70 BHN and 218 MPa, respectively. Although mould was made of graphite. During the sintering process, the sinter­
their method had a higher sintering temperature compared to other ing temperature, heating rate, pressure, and holding duration were
processes, the mechanical properties showed less improvement. Mean­ 540 ◦ C, 60 ◦ C/min, 50 MPa and 10 min, respectively. A thermocouple
while, the strengthening mechanism and microscopic interface were not was placed in the graphite mould to determine the temperature of the
analysed in depth. A few studies have been conducted on the manu­ sample. The sample was lowered to room temperature with flowing
facture of Al 7075/ZrO2 via the powder metallurgy route; nevertheless, cooling water. Three samples were prepared with identical settings to
the evolution behaviour and reinforcing mechanism of these composites guarantee the accuracy of the data.
have not been investigated [21].
Mechanical alloying (MA) is known for producing a more uniform 2.3. Characterisation
distribution of reinforcements in the metal matrix. It helps to enhance
the mechanical properties of the resulting materials. Spark plasma sin­ The surface of each sample was sequentially polished with abrasive
tering (SPS) is an innovative form of hot pressing, in which pulsed direct papers of 400#, 800#, and 1200# grit. The Archimedes drainage
current (DC) and pressure are applied to a graphite mould containing a method was used for density measurements. The hardness of the sin­
sample to accelerate the heating and cooling rates [22]. Compared to the tered compact was measured using a Vickers hardness tester (HXD-
compo-casting process, SPS offers advantages such as lower sintering 1000TMC, Shanghai Taiming Optical Instrument Co., Ltd., China) with a
temperatures and higher sample density. SPS technology has attracted load of 1.96 N and dwell time of 20 s. The values averaged from five
attention [23] due to its ability to restrict grain growth during the fast measurements for each material. The tensile strength was measured
sintering process. This technology has become indispensable in powder using an electronic universal testing machine (LITM2203) at a strain
metallurgy for the preparation of nano bulk materials, amorphous ma­ rate of 0.5 mm/min. Wire cutting (DK77130, Zhong Yuan, China) was
terials and multiscale composite structures [24,25]. The selection of SPS used to shape the sample into a dog-bone shape with a gauge length and
process to further improve the comprehensive performance of the ma­ diameter of 30 and 2 mm, respectively. Wear test were conducted using
terial, reducing its manufacturing cost and in-depth analysis of the a tribometer (Model MS-T3000; Lanzhou Institute of Chemical Physics,
strengthening mechanism is of great significance to the application of Al Chinese Academy of Sciences, China) under a load of 5 N for 30 min.
7075. Then, multifunction tester for material surface (MFT-4001, Lanzhou
Few studies are available in the literature on the production of the Al Huahui Instrument Technology Co. Ltd., China) was used to test the
7075/ZrO2 composite using MA and SPS. In this study, a ZrO2-reinforced cross-sectional area of the wear marks. The wear rate was calculated
7075-aluminium-alloy-based composite (Al 7075/ZrO2) was prepared according to the following formula:
via MA and SPS. We investigated the effects of ZrO2 on the structure,
volume
wear and mechanical properties of Al 7075/ZrO2. Furthermore, the ef­ wear rate = (1)
load × sliding distance
fect of ZrO2 on the pinning effect and dislocation density of the com­
posite was studied to further analyze the strengthening mechanism. The Wear scar depth and width were used to calculate the cross-sectional
aim of the study is to provide experimental guidance for improving the area of the wear track.
comprehensive performance of AMCs. By incorporating ZrO2 rein­ The values averaged from three measurements for each material. The
forcement, the composite exhibited enhanced performance, making it microstructures and ZrO2 distributions of the composites, appearance of
more suitable for various industrial applications. fracture were imaged via field emission scanning electron microscopy
(SEM, Helios G4CX). The specimens were observed by electron back­
2. Experimental methods scattering diffraction (EBSD) using scanning electron microscopy (SEM;
Helios G4CX FIB) at the voltage of 20 kV and the current of 11 nA. EBSD
2.1. Materials and methods analysis was conducted to characterise the grain sizes of 7075Al and the
composite samples. The crystal structures of the ZrO2 grains and their
The matrix material, 7075 aluminium alloy (purity ≥ 99.85 wt%), bonding interfaces with the Al matrix were also identified through high-
was used in this study. Powder with an average particle size of 10 µm resolution transmission electron microscopy (HRTEM FEI Tecnai G2
were purchased from Changsha Tianjiu Metal Material Co. Ltd., China. F20).
The chemical composition of the 7075 aluminium alloy samples is listed
in Table 1. Monoclinic ZrO2 with an average particle size of 200 nm was
used as the reinforcing phase. The morphologies of the materials are

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J.-d. Zhang et al. Materials Today Communications 37 (2023) 107437

Fig. 1. SEM images of (a) ZrO2 particles, (b) 7075Al particles before ball milling, and (c, d) the addition of ZrO2 is 4 wt% composite powder after ball milling.

Fig. 2. Microstructure of the composites at ZrO2 contents of (a, b) 0 wt%, (c) 2 wt%, (d) 4 wt%, (e) 6 wt%, and (f) 8 wt%.

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J.-d. Zhang et al. Materials Today Communications 37 (2023) 107437

3. Results aluminium alloy. Jiang Yue et al. [27] reported that the precipitate
phase of 7075 Al mainly contained MgZn2 in rod shape and Al2CuMg in
3.1. Microstructure analysis capsule shape. It can be seen that the surface of 7075Al mainly contains
rod and capsule shape in Fig. 2(b). Furthermore, the energy dispersive
As shown in Fig. 1(b), the surface of 7075Al particles before ball spectroscopy (EDS) shown in Fig. 3(a) revealed that the precipitate was
milling was smooth and composed of particles of different sizes. The primarily composed of Al, Mg, Zn and Cu. The predominant constituent
morphology of the powders that were milled for 4 h (Fig. 1(c)) exhibited of this precipitate are (MgZn2) phase and S-phase (Al2CuMg). When the
an irregular shape because of the shearing effect of the balls. The addition content of ZrO2 is 4 wt%, it can be seen that in addition to the
irregular shape was also due to the adhesion of ZrO2 to the surface of the precipitate phase, there are some white particles distributed at the grain
7075 Al alloy particles, as small particles and layers of ZrO2 were clearly boundaries. Fig. 3(c) reveals that ZrO2 was consistently distributed at
visible on their surface (Fig. 1(d)). The particle size of the composite the grain boundaries.
powder decreased significantly after ball milling, and ZrO2 evenly An increase in the ZrO2 content resulted in a decrease in the number
adhered to the surface of 7075Al. The Nano measurement software was of flaws. However, with excessive zirconia content, ZrO2 aggregates and
used for the statistical analysis of the 7075Al and composite material surface defects emerge, as shown in Fig. 2(e). Fig. 2(f) displays a more
powders. The average particle size of 7075Al prior to milling is 9.75 µm, pronounced growth of ZrO2 reassembly, which increases the number of
while the mean size of the composite particles reached 6.7 µm after flaws. Therefore, the addition of zirconia is 4 wt%, where zirconia can
milling for 4 h, indicating that ball milling can effectively refine the be relatively evenly distributed within the composite material.
particles size of powder [26].
3.3. EBSD and TEM
3.2. Microstructural evolution of the composites
The misorientation patterns of Al 7075 and Al 7075 /ZrO2 compos­
As shown in Fig. 2, the microstructure of composites is affected ites obtained through EBSD mapping are depicted in Fig. 4(a, b). The
differently at various ZrO2 contents. Fig. 2(b) depicts the precipitation of increase in content of ZrO2 resulted in the formation of fine grains with a
white particles with rod and capsule shapes on the surface of 7075 homogeneous distribution along the coarse grain borders. According to

Fig. 3. EDS profiles of the composites at ZrO2 contents of (a) 0% and (b) 4 wt%.

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J.-d. Zhang et al. Materials Today Communications 37 (2023) 107437

Fig. 4. EBSD maps of the composites at ZrO2 contents of (a) 0 wt% and (b) 4 wt%, (a, b) Inverse pole figure maps of Al 7075 and 4 wt% Al 7075 /ZrO2 composite,
respectively. (c, d) The grain size distribution of (c) Al 7075 and (d) 4 wt% Al 7075 /ZrO2 composite.

Fig. 4(c), the average grain size of the Al 7075 base alloy was determined 7075 and Al 7075 /ZrO2 samples, respectively. The thermal expansion
to be 3.9 µm based on EBSD statistical data. However, the Al 7075 /ZrO2 coefficients of ZrO2 and Al 7075 differed significantly, resulting in
composite was composed of more grains with an average grain size of mismatches among the composites. During the sintering process, the
2.8 µm in Fig. 4(d). specimens experienced varying pressure and temperature levels, leading
Fig. 5(a) and (b) depict recrystallization organisation analysis dia­ to the generation of unavoidable stress and numerous dislocations.
grams. The blue, yellow and red areas represent completely recrystal­ Dislocations effectively hinder the grain boundary sliding process.
lized grains, recovered grains, and deformed grains, respectively. After Moreover, increased dislocation density impedes dislocation motion,
sintering, most of the grains underwent recrystallization. The addition of thereby increasing the material’s resistance to plastic deformation and
ZrO2 led to significant small-scale deformation within the composite strengthening of the composite. This highlights the significant impact of
material [19]. Recrystallization refinement is mostly induced by the dislocation strengthening on the material properties of composites [31].
nano-ZrO2 pinning effect that occurs during the sintering process. In Fig. 6(a) illustrates that the ZrO2 particles are distributed at the grain
Fig. 5(b), it can be observed that ZrO2 at the grain boundary inhibits the boundaries where the pinning effect of ZrO2 hinders the sliding and
growth of recrystallized grains and promotes the growth of some refined migration of the grain boundaries. The bonding strength of interface
deformed, recrystallized grains during the grain recrystallization pro­ between the reinforcing ZrO2 particles and the matrix phase of Al 7075
cess. Grain refinement in the deformed and recrystallization structures alloy plays a crucial role in the comprehensive performance of com­
became more significant as the nano-ZrO2 content increased [28,29]. posites [14]. Therefore, a detailed investigation of the interfacial
Fig. 5(c) and (d) display the KAM maps for the Al 7075 and Al 7075 structure of Al 7075 and ZrO2 was conducted. Fig. 6(b) shows a
/ZrO2 samples. The distribution of local microstructure strain can be high-resolution transmission electron microscopy (HRTEM) image of the
determined by KAM. KAM values were assigned to each point based on interfacial structure. It is clearly seen that the interface is clean, smooth
the grain it belongs to, effectively representing the extent of local and free from additional interfacial reaction products and exhibits a
misorientation. By visualizing the KAM values in a map, the color var­ good bonding status, which is conducive to effective load transfer in the
iations highlight the non-uniform distribution of local strain within the composite material.
microstructure [30]. The green-coloured line represents dislocations.
The step size and Burgers vector were 0.2489 µm and 0.268 nm,
respectively. The Channel 5 software was used to calculate the average 3.4. Mechanical property
dislocation density (ρ) of 2.5 × 1014 m2 and 6.8 × 1014 m2 for the Al
Fig. 7(a) presents a bar chart illustrating the variation of hardness

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J.-d. Zhang et al. Materials Today Communications 37 (2023) 107437

Fig. 5. EBSD maps of Al 7075 and composite samples (a, b) Recrystallised fraction illustrations, (c, d) KAM maps of Al 7075 and 4 wt% Al 7075 /ZrO2 composites.

Fig. 6. (a) Nano-sized ZrO2 microstructures at the grain boundary. (b) HRTEM image of the interfacial structure.

and density with the addition of ZrO2 in the composite material, the compared with the results published in open literature, as listed in
results show that that hardness first increased and then decreased as the Table 2. It is evident that the Al 7075 /ZrO2 composite prepared using
ZrO2 content increased. However, the density of the composite the SPS technique exhibits significantly higher hardness and tensile
decreased with the ZrO2 content increased. When the addition content strength compared to composite casting. Furthermore, when compared
of ZrO2 is 4 wt%, the relative density and hardness were 97.23 % and to 7075 Al/GNPs composites fabricated through the SPS process, the Al
152.54 Hv, respectively. Fig. 7(b) depicts the tensile characteristics of Al 7075 /ZrO2composites show a slight increase in density and a significant
7075 and Al 7075 /ZrO2 composites at different content of the ZrO2. The 22 % increase in hardness. Additionally, it can be observed that the use
tensile strengths initially increased and then decreased as the ZrO2 of ZrO2 as a reinforcement particle yields superior mechanical proper­
content increased, reaching a maximum of 365 MPa at a doping level of ties compared to other strengthening phases. This indicates that
4 wt% ZrO2. However, when the content of ZrO2 was further increased employing ZrO2 as a reinforcement phase can effectively enhance the
to 6 wt%, the ZrO2 particles agglomerate severely which leading to a mechanical performance of Al 7075, thereby expanding the application
decrease in the tensile strength of the composite material. range of this material.
The mechanical properties of the investigated composites have been

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J.-d. Zhang et al. Materials Today Communications 37 (2023) 107437

Fig. 7. (a) Density and hardness values of the composites at various ZrO2 contents. (b) Tensile strength and elongation of composites with different ZrO2.

Table 2
Mechanical properties of 7075 aluminium alloy composites with different reinforcement phases.
Materials Process Density (%) Hardness(Hv) Tensile strength (MPa) Elong-ation Refs.
(%)

Al 7075 /ZrO2 SPS 97.23 152.5 376 12 This work


7075Al /ZrB2 Stir casting – – 360.4 – [12]
Al 7075 /ZrO2 Compo-casting – 70 218 – [20]
Al 7075/B4C Casting – 160 260 – [32]
Al7075/Al2O3 /C Liquid Metallurgy – 134 236 – [33]
Al 7075GNPs SPS 95.31 124.9 – [34]
7075Al/CNTs-TiO2 Casting – 163.8 338.1 [11]
7075Al /TiB2 Stir casting – 128 286 8 [35]

3.5. Wear properties decrease in the coefficient of friction. This is primarily due to the added
hard particles act as a main load bearing unit and their addition leads to
Fig. 8(a) shows the coefficients of friction of the specimens with a reduction in the coefficient of friction. The average coefficient of
varying ZrO2 contents. It is observed that the coefficient of friction in­ friction reached 0.25 upon the addition 4 wt% ZrO2, and the overall
creases steeply, followed by a subsequent decrease, and finally stabil­ trend of coefficient of friction is relatively smooth without significant
ises. This can be attributed to the large amount of heat generated fluctuation. However, the coefficient of friction starts to increase with
between the friction substrate and sample surface during the friction the continual addition of ZrO2 till up to 6 wt%, which may be due to the
process. The heat generated during the friction process causes the agglomeration of ZrO2 particles and low sample density. In addition, the
oxidation of the friction surface, resulting in the formation of a dense ball milling process will remove some ZrO2 particles and scattering them
oxide film that plays a lubricating role and causes the coefficient of on the surface of the sample. These hard particles create deep grooves on
friction to decrease [36]. the surface, retaining a large volume of dispersoids and bring more as­
The addition of ZrO2 in the composite material results in a visible perities in direct contact with each other [37], which leads to an increase

Fig. 8. (a) COF and (b) wear rate of composites at different ZrO2 contents.

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J.-d. Zhang et al. Materials Today Communications 37 (2023) 107437

in the coefficient of friction. The wear rate exhibits a decreasing trend


initially and then increases with increasing ZrO2 contents. Compared to
7075Al alloy, when the ZrO2 content is 4 wt%, the wear rate decreases
from 2.6 × 10− 3 mm3/N⋅m to 0.9 × 10− 3 mm3/N⋅m. However, the wear
rate further increases to 1.4 × 10− 3 mm3/N⋅m when 6 wt% ZrO2 is
added. Fig. 9 shows the friction micromorphology at different ZrO2
contents, revealing significant changes in the wear surface with the
addition of ZrO2 particles. The wear width in the 7075Al sample is
approximately 1011 µm, while in the sample with 4 wt% ZrO2, it mea­
sures approximate 628.7 µm. This confirms the better performance of
composites of 4 wt% ZrO2 addition.

4. Discussion

4.1. Densification behavior during SPS

The displacement measurements provide a way to observe changes


in the thickness of the sintered powder within the mold over time.
Fig. 10. The punch displacement profiles in the study of spark plasma sintering
Hence, the displacement can effectively reflect the densification of sin­
of sample.
tered samples. Fig. 10 shows the punch displacement profiles during the
study of spark plasma sintering of sample. These changes of displace­
ment over time (Fig. 10) can be divided into three distinct stages which rearrangement leading to a decrease in densification [38]. Similar re­
correspond to (I) rapid densification stage, (II) densification stabiliza­ sults that the density decrease with the addition of ceramic reinforce­
tion stage and (III) final densification stage. ment have been reported. Samuel Ranti Oke et al. [40] fabricated
In the rapid densification stage, it can be seen that the displacement ZrO2/Ti6Al4V-Ni composites by using SPS and observed a decrease in
of the sample significant change with the heating and compression sintered density from 99.56 % to 98.06 % with the addition of ZrO2
process [38]. It is mainly due to the rapidly decrease in the height of the increasing. Mohsen Hajizamani et al. [41] used nanoparticles of
powder layer under pressure. Under the action of sintering temperature Al2O3-10 % ZrO2 as reinforcement to fabricate Al 356/ZrO2 composites.
discharge plasma activates the powder surface and the powder particles They found that an increase in nanoscale reinforcements resulted in
undergo a transition from solid phase to liquid phase resulting in a higher porosity content and decreased densification. When an excessive
significant change in displacement. Variation of displacement in stage II amount of ZrO2 was added, the agglomeration of ZrO2 particles
which can be attributed to plastic flow [39]. The displacement continues occurred, preventing complete sintering at lower temperatures and
to decrease under the later sustained pressure and cooling conditions in leading to decreased density. When the ZrO2 content was increased to
stage III. In this stage, the temperature drops rapidly resulting in the 6 wt% (Fig. 2(d)), the agglomeration of ZrO2 causes defects to form on
rapid transformation of the sample from liquid phase to solid phase and the surface of the composite material.
the gas in the sample can still escape from the grain boundaries before
the sample is completely solidified under the action of pressure. The 4.2. Reinforcing mechanism
densification of composite powders is primarily controlled by two
mechanisms: particle rearrangement and plastic deformation of a soft According to the mixing law [42], the addition of ZrO2 particles to
matrix. Reinforcements with lubricating properties benefit particle the Al 7075 alloy matrix increases the hardness of the composite ma­
rearrangement, while hard reinforcements hinder particle terial. This is because ZrO2 has a higher hardness compared to the Al

Fig. 9. Worn surface morphology of the composites with ZrO2 contents of (a)0 wt%, (b)2 wt%, (c)4 wt%, (d)6 wt% and (e)8 wt%.

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J.-d. Zhang et al. Materials Today Communications 37 (2023) 107437

7075 alloy. The hardness values of the 7075Al matrix and four com­ resist tensile stresses, with the matrix efficiently transmitting stress to
posites are shown in Fig. 7. The results reveal that the hardness of the the reinforcement particle [46]. In addition, ZrO2 particles act as a
composite increases first and then decreases with the addition of ZrO2. barrier, impeding development and sliding of the grain boundaries
Firstly, the mismatch of thermal expansion coefficient between ZrO2 and during addition and stretching. The addition of ZrO2 enhance the
the Al 7075 matrix, leads to the formation of dislocations with high dislocation density and strength, resulting in an increase in the
density and complexity in the composites. When the composite material load-bearing capability of the composite [21]. The elongation is mainly
undergoes deformation, the ZrO2 particles impede dislocation move­ influenced by the combined effect of grain refinement and particle
ment, enhancing the material’s resistance to deformation and ultimately strengthening. When ZrO2 is added at 4 wt%, the increased number of
increase its hardness [43]. Secondly, the strong bonding strength be­ grains in the composite allow for more grains to withstand the external
tween the ZrO2 particles and Al 7075 surfaces can improve the capacity tensile force and undergo deformation. Consequently, the uniformity of
of the material to withstand and transfer loads. The utilisation of hard deformation is improved. The smaller the grain size, result in greater
ZrO2 particles as the principal carrier enable efficiently load transfer bending of grain boundaries, effectively inhibiting crack propagation
from the soft matrix to the hard particles [44]. Thirdly, the uniform and enhancing the ability to withstand deformation before fracture.
dispersion of 4 wt% ZrO2 particles in the AMCs lead to grain refinement When cracked by external tensile stresses, ZrO2 alters the crack exten­
of the composites, which hinders dislocation slip at the grain bound­ sion path, leading to crack bridging and flexing, which consumes more
aries. This further improves the hardness of composites [45]. An energy and leads to the increase of crack propagation resistance, thus
excessive addition of ZrO2 at 6 wt% (Fig. 2(e)) causes agglomeration to improving the fracture toughness. In addition, the presence of ZrO2
occur, resulting in a weak interface between the ZrO2 particles and the particles will hinder the dislocation migration and reduce the elonga­
matrix. When the composite material is deformed, the effect of ZrO2 on tion. However, the decrease in elongation caused by this effect is out­
dislocation movement is reduced, leading to a decrease in the hardness. weighed by the overall increase in elongation resulting from ZrO2
Fig. 11(a) illustrates that the 7075 Al and 7075 Al/ZrO2 composites addition. Therefore, the elongation of the composite increases after the
have prominent ductile fracture characteristics with visible tear lines introduction of ZrO2 particles [47].
and deep dimples. Increasing in the ZrO2 content in the composites led At 8 wt% ZrO2 content (as shown in Fig. 11(e)), significant
to a decrease in dimple size and a more uniform distribution. The ZrO2 agglomeration occurred resulting in a brittle fracture surface
particles were uniformly dispersed within the matrix and had excellent morphology. Poor sintering due to ZrO2 aggregation led to a deterio­
contact with the matrix material. Under tensile stress, the ZrO2 particle ration in the tensile strength of the composite. The weakened particle
strength in Al 7075 /ZrO2 is significantly higher than that of the Al 7075 interfaces resulted in premature fracture under tensile loading. As a
alloy. This strong interfacial binding strength allow the composite to result, the plasticity of the composite decreased, making it more

Fig. 11. Tensile fracture microstructure of the composites at ZrO2 contents of (a) 0 wt%, (b) 2 wt%, (c) 4 wt%, (d) 6 wt%, and (e) 8 wt%.

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J.-d. Zhang et al. Materials Today Communications 37 (2023) 107437

susceptible to fracture during the tensile process. However, the rein­ observed on the wear surface of the composites with 4 wt% ZrO2
forcing effect is dependent on the distribution of reinforcing particles in compared to that 7075 aluminium alloy. When the ZrO2 content is 8 wt
the matrix. The addition of excessive ZrO2 particles leads to agglomer­ %, the abrasion depth increases.
ation within the matrix, which results in early interface debonding and
the formation of holes in the ductile matrix. This can trigger crack 5. Conclusion
initiation in the particle aggregation regions, leading to a decline in
elongation [48]. In this study, a ZrO2-reinforced 7075-aluminium-alloy-based com­
posite (7075 Al/ZrO2) was prepared via MA and SPS, and the effects of
4.3. Wear mechanism ZrO2 addition was investigated. The following main outcomes were
noted:
Fig. 12 displays the worn surface morphology of the composites with
varying ZrO2 contents. The base alloy without the addition of ZrO2 (1) Grain refinement was observed during the SPS process upon ZrO2
exhibited wider and deeper abrasion marks with flake peeling, a few addition. The pinning effect of the ZrO2 particles slowed grain
pits, and partial plastic deformation of the laminae [49]. During the growth, following recrystallization in the SPS process, leading to
friction process, the aluminium alloy with relatively low hardness and a reduction in the grain size.
elastic–plastic modulus was the main unit bearing the normal load easily (2) A significant increase in the dislocation density of the composite
occurred plastic deformation due to shear force. The friction process relative to that of the aluminium alloy was obtained when ZrO2
generated significant between the friction pairs, which leads to the particles were added. The dislocation density of 7075 Al/ZrO2 is
oxidation of the sample surface. Some soft and strongly adherent oxides notably higher than that of Al 7075 alloy; their average disloca­
were repeatedly extruded and stretched, and finally laid on the wear tion densities (ρ) were 2.5 × 1014 and 6.8 × 1014 m2,
surface of the specimen to form a dense friction layer during the wear respectively.
process. This indicates that the aluminium alloy experienced worn (3) The fracture surfaces of the composites were characterised by
through both adhesive and oxidation wear mechanisms. After the homogeneous dimples. The strong interfacial bonding between
addition of ZrO2, the wear surface shows obvious grooves and abrasive ZrO2 and the Al 7075 alloy matrix is responsible for the balance of
chips, indicating that the composite wear mechanism is mainly domi­ moderate elongation and high strength of the ZrO2/7075Al
nated by abrasive particle wear [17]. The wear particles are fragments composites.
and chips resulting from by micro-cutting of the friction ball in the (4) The ZrO2 particles dispersed on the outer surface of the friction
friction test. The composites with 4 wt% ZrO2 exhibited the highest wear substrate take the main load, leading to improved wear resistance
resistance. This is attributed to the uniform distribution of ZrO2 within of the composite. At considerably high ZrO2 contents, agglom­
the composite with high hardness,elastic–plastic modulus. During the eration occurs, causing a decrease wear rate.
friction test, when the friction pair is in contact with the composite
surface, the ZrO2 particles dispersed on the outer surface of the friction 7075 aluminium-based composites are commonly used in ship
substrate bear the main load. This further reduces the coefficient of structures, masts, and components due to their high strength and
friction of the composite. In addition, wear resistance is generally pro­ lightweight properties, which significantly reduce fuel consumption.
portional to the material’s hardness [50]. The presence of ZrO2 in the However, the aluminium alloy matrix has relatively poor corrosion
composite material exerts a pinning effect, inhibiting grain growth, resistance, so improving its corrosion resistance to increase its service
refining the grains, and increasing the hardness and wear resistance. life is of great research significance. Future studies will involve accel­
When the ZrO2 content is excessively high, incomplete sintering and erated aging tests, exposure to corrosive environments, or cyclic loading
weak bonding strength between the Al 7075 matrix and ZrO2 interface simulations to evaluate the performance of the composite over time.
can occur, making composites easy to stripping. Fig. 13 shows the 3D Further optimization in composite material design and selection will
profile of the wear track at different contents. Slight worn can be also be pursued.

Fig. 12. Worn surface morphology of the composites with ZrO2 contents of (a)0 wt%, (b)2 wt%, (c)4 wt%, (d)6 wt% and (e)8 wt%.

10
J.-d. Zhang et al. Materials Today Communications 37 (2023) 107437

Fig. 13. 3D wear track images of (a).0%, (b).4% and (c). 8% wear track.

Ethical approval 7075 tubing by Shear Assisted Processing and Extrusion (ShAPE), J. Manuf.
Process. 71 (2021) 699–710, https://doi.org/10.1016/j.jmapro.2021.10.003.
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[7] A. Baradeswaran, A. Elaya, Perumal, Study on mechanical and wear properties of
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Declaration of Competing Interest https://doi.org/10.1016/j.compositesb.2013.08.013.
[8] P.A. Bajakke, V.R. Malik, A.S. Deshpande, Particulate metal matrix composites and
their fabrication via friction stir processing–a review, Mater. Manuf. Process. 34 (8)
The authors declare the following financial interests/personal re­
(2019) 833–881, https://doi.org/10.1080/10426914.2019.1605181.
lationships which may be considered as potential competing interests: [9] D.Y. Kim, H.J. Choi, Recent developments towards commercialization of metal
Lan Zhang reports financial support was provided the Program for New matrix composites, Materials 13 (12) (2020) 12–35, https://doi.org/10.3390/
Century Excellent Talents in University from the Ministry of Education ma13122828.
[10] J. Jiang, Y. Wang, Microstructure and mechanical properties of the rheoformed
of China NCET-11-0951. cylindrical part of 7075 aluminum matrix composite reinforced with nanosized SiC
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fabricated by stir casting, Mater. Today Commun. 25 (2020), 101289, https://doi.
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