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Composites Part B 157 (2019) 131–139

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Composites Part B
journal homepage: www.elsevier.com/locate/compositesb

Gas-atomized copper-based particles encapsulated in graphene oxide for T


high wear-resistant composites
Wenzheng Zhaia, Wenlong Lua,∗, Youming Chenb, Xiaojun Liua, Liping Zhoua, Dong Linc
a
The State Key Laboratory of Digital Manufacturing Equipment and Technology, School of Mechanical Science and Engineering, Huazhong University of Science and
Technology (HUST), Wuhan, 430074, PR China
b
Engineering Research Center of Advanced Equipment, Ministry of Education, Hunan University of Science and Technology, Xiangtan, 411201, PR China
c
Department of Industrial and Manufacturing Systems Engineering, Kansas State University, Manhattan, KS, 66506, United States

A R T I C LE I N FO A B S T R A C T

Keywords: A novel architecture of graphene oxide wrapped copper spheres (Cu/GO) is proposed for fabricating high wear-
Metal-matrix composites (MMCs) resistant Cu-based composites. Tribological results indicate that GO shell layers present an exceptional
Wear strengthening efficiency surpassing conventional nanoparticle, fiber and nanosheet reinforcements for Cu-based
Surface analysis materials reported to date. The friction torque of the composites shows a load-insensitive behavior stabilized at
Powder processing
0.26–0.41 Nm. Such good tribological performance is ascribed to integrated effects including strong metal/GO
interfacial coupling, uniform distributed GO, and the GO-assisted tribofilm formed on ridges and asperities of
wear tracks. The fabrication strategy is convenient, low cost, easily scalable, and can be expanded to the pre-
paration of other metal/GO materials.

1. Introduction Herein, we made an effort on the synthesis of gas-atomized (GA) Cu-


based particles encapsulated in GO for the fabrication of Cu/GO com-
A good control of wear and friction is crucial for improving the posites with enhanced tribological properties. The gas atomization
energy efficiency not only in macro-scaled moving assemblies including process offers many advantages including a high sophericity that is
pumps, compressors and turbines [1], but also in micro/nano-scaled beneficial for the Cu/GO interface bonding, control of contamination,
technologies such as micro/nano-electromechanical systems [2–4]. In grain refinement and avoidance of composition segregation [15]. It has
these devices, mechanical stability is also a fundamental requirement to been demonstrated that nano-precipitation could present in GA pow-
enhance the lifetime of parts, and to maintain their functionalities [5]. ders, and remain in the materials after subsequent fabrication processes
Copper and copper-based alloys have commonly been used in these [16,17], thus providing extra wear resistance and mechanical strength.
devices [6–8], which often suffer from substantial tribological problems In addition, the gas atomization technique enables the large-scale
and subsequent mechanical durability owning to the wear damage. production of powders (2 kg/min) with a uniform microstructure due to
Nanostructure engineering and hybridization of particles with gra- rapid solidification [18,19], which is favorable for engineering appli-
phene oxide (GO) shell layers might show the potential to address these cations of our Cu/GO composites. Anti-wear properties of samples from
problems [9,10]. The flexibility and the high surface area of the two- blank GA powders without GO were also tested to highlight the benefit
dimensional (2D) nanostructured functional derivative from graphene of the Cu/GO hybridization routing. As demonstrated in fretting wear
enable a good bonding of its hybrid materials, allowing it to attach well measurements, the as-prepared GO wrapped spherical Cu-particle
with the dispersed particles while avoiding agglomeration during hy- composite exhibited exceptional anti-wear performance and distinct
bridization [11]. GO systems with excellent electrical, thermal con- stable friction torque. The GO shell layers showed remarkably higher
ductivity and considerable mechanical strength, have inspired the de- strengthening efficiency than those of conventional nanoparticle, fiber
velopment of hybrid materials for various applications, such as and nanosheet reinforcements for the Cu matrix, and also considerably
optoelectronics [11,12] and electrodes [10,13,14]. Nevertheless, to the higher than their hybrid structured reinforcements reported so far.
authors' best knowledge, thus far in the literature no study has been
reported to evaluate the anti-wear performance of parts fabricated from
the hybrid nanostructures of Cu-based particles encapsulated in GO.


Corresponding author.
E-mail address: hustwenlong@mail.hust.edu.cn (W. Lu).

https://doi.org/10.1016/j.compositesb.2018.08.125
Received 14 July 2018; Received in revised form 23 August 2018; Accepted 27 August 2018
Available online 28 August 2018
1359-8368/ © 2018 Elsevier Ltd. All rights reserved.
W. Zhai et al. Composites Part B 157 (2019) 131–139

Fig. 1. (a) Schematic illustration of fabrication of GO wrapped Cu spherical particles; (b) SEM image of GA Cu spherical particles; (c) SEM and TEM images of Cu/GO
composites showing good Cu/GO interface bonding; (d) The digital photograph of the consolidated Cu/GO composite.

Table 1 7 ± 6 μm (Fig. 1b) supplied by Metal Products Trade Co. Ltd. China,
Typical composition of GA Cu-based powders in this work. were used as initial particles for the encapsulation. The chemical
Element Cu Al Ni Fe Mn Impurity composition of the powder is shown in Table 1. In a typical preparation
process, the Cu/GO powders were obtained from GO wrapping mod-
Content (wt.%) Balance 9.5 4.2 4.0 1.2 < 0.5 ified-GA powders by the electrostatic adsorption method. Fig. 1c clearly
displayed that GA powders were well encapsulated inside thin GO na-
nosheets. After the hybridization process, a cylindrical graphite mold
2. Materials and methods loaded with Cu/GO powders was put into an spark plasma sintering
apparatus (LABOX-1575, SINTER LAND, Japan) and then heated up to
2.1. Synthesis of Cu/GO samples 800 °C at a rate of 100 °C/min and a pressure of 40 MPa for 10 min
under an argon gas flow. After the apparatus was completely cooled,
Fig. 1a schematically depicts the synthesis strategy of Cu/GO sam- the product was taken out and the Cu/GO powders were consolidated
ples. Spherical GA powders with an average particle diameter of

Fig. 2. (a) XRD patterns and (b) Raman spectra of blank Cu matrix and Cu/GO powders; (c and d) FESEM images of the cross-section of the consolidated Cu/GO
composite showing good interfacial bonding between the Cu particles and GO after the SPS consolidation process.

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Fig. 3. (a) FESEM image of the surface microstructure of the consolidated Cu/GO composite; (b–g) C, Al, Mn, Fe, Ni and Cu maps of areas in (a).

into a tablet with a diameter of 26 mm and a height of 4 mm (Fig. 1d). diffraction (XRD) on the XRD-7000 S X-ray diffractometer with Cu Kα
To study the influence of the GO shell layers on anti-friction and anti- radiation. Raman spectra were recorded using the inVia Raman mi-
wear performance of Cu materials, the same consolidation process was croscope (RENISHAW). The morphology and microstructure of the
carried out for blank GA powders. After the SPS process, the as-pre- products were carried out on the JSM-7600 F field emission scanning
pared specimens were ground to remove the surface layer to eliminate electron microscope (FESEM) and the JEOL JEM 2100 transmission
carbon atmosphere effects induced by the graphite mold, followed by electron microscope (TEM).
mechanical polishing with emery papers down to 2000 grit.

2.3. Wear and mechanical tests


2.2. Characterization
The anti-wear behaviors of the consolidated samples were examined
The phase purity of prepared products was determined by X-ray by a fretting test system with a flat-on-flat configuration at contact

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Fig. 4. (a) Dynamic friction torques (T) of the Cu/GO composite and the blank Cu matrix as a function of fretting cycles under varied loads of 43, 86 and 106 N. The
inset shows the static mean value of T; (b) Typical wear volumes of Cu and Cu/GO samples after fretting tests; (c) 3D morphologies with the depth profile of wear
tracks of the Cu/GO composite demonstrating the slight wear at different loads; (d) A summary of the friction coefficient versus the strengthening efficiency of
various reinforcements for Cu matrix composites, including GO shell layers in this work, and conventional nanoparticle, fiber and nanosheet reinforcements, as well
as their hybrid structured reinforcements for Cu matrix composites. The GO shell layers in this work present a superior strengthening efficiency which exceeds other
reinforcements in Cu matrix composites reported so far.

Table 2 3. Results and discussion


Detailed experimental data under certain wear test conditions.
Reinforcement Load Friction Wear rate Ref.
3.1. Composition and morphology
condition (N) coefficient 10−3 mm3/
Nm Fig. 2a presents XRD patterns of pure Cu and Cu/GO powders,
where all of diffraction peaks can be indexed to Cu (JCPDS No.
TiB2 + Pb 10 0.71–0.75 1.5–3.0 [31]
Carbon fiber + reduced 20 0.32 0.064 [32]
50–1246). Some weak peaks marked by black rhombus and square
GO belong to NiAl and AlCu3, respectively. The complicated phases con-
Cr + graphite 40 0.4–0.6 0.25–1.25 [33] sisting of Cu matrix, NiAl and AlCu3 rather than a pure phase could be
Cr + SiC 10–40 0.4–0.8 0.15–0.48 [34] attributed to the precipitation during the gas atomization process [17].
WC 10 0.3 0.14 [35]
Nevertheless, no diffraction peaks from graphite or impurities are ob-
SiC + carbon nanotubes 10–50 0.45–0.85 0.025 [36]
(CNTs) served, suggesting a desired encapsulation of GO wrapped Cu without
detrimental chemical reactions. The graphene structure in the Cu/GO
composite was also investigated by the Raman spectrum, in which two
loads of 43, 86 and 106 N and a frequency of 2 Hz for 20000 cycles. The broad peaks located at 1348 and 1597 cm−1 could be assigned to ty-
relative displacement stroke was set to 180 μm. The configuration of the pical D- and G-bands of carbon, respectively (Fig. 2b). The G band of
test device can be found in our previous studies [17,20,21]. The angular Cu/GO displays a shift to a higher frequency (1597 cm−1) than that of
displacement amplitude (θ) of tests was 1.5°. These experimental graphite (1580), which indicates that the carbon in the composite was
parameters were set on the basis of the engineering operating condi- indeed partially amorphous carbon. Specifically, the calculated peak
tions [22]. The counterpart material was 42CrMo4 steel with a hardness intensity ratio of the D- and G-bands (ID/IG) was ≈1, implying in-
of 25 HRC and a roughness of Ra = 0.2 μm. Each test was carried out creased sp3 bonded carbon atoms in GO as a result of the disruption of
three times to make sure the repeatability of experimental results at sp2 bonds by oxidative functional groups. This is beneficial to achieve a
same conditions, and average results were reported. better metal-graphene interface interaction strength [23].
A typical FESEM image of the cross-section of consolidated Cu/GO
composite indicates that they retained well the pristine spherical

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Fig. 5. Typical FESEM images of wear tracks on Cu/GO samples after fretting under contact loads of (a) 43 and (b) 106 N; (c) The high magnification FESEM image
with corresponding line scanning of elements for the ridge area indicating the C-element accumulation in ridges after the fretting wear process; (d–k) The high
magnification FESEM image with element maps for an asperity of wear tracks demonstrating the accumulation of the C element.

morphology of the as-prepared GO wrapped Cu even after the high- spectroscopy (EDS) maps of elements in the composite are shown in
temperature sintering process (Fig. 2c). The magnified FESEM images Fig. 3b–g. It is clearly seen from EDS results that the GO is uniformly
of the Cu/GO composite show good interfaces between the Cu particles distributed in the composite without aggregation.
and GO layers after the SPS consolidation process (Fig. 2d). Such well
interfaces would effectively hinder crack propagation and improve the 3.2. Tribological behaviors
wear resistance during fretting. The surface microstructure of con-
solidated Cu/GO composite is shown in Fig. 3a. Energy-dispersive X-ray Fretting wear tests were performed on surfaces of the consolidated

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conventional nanoparticle, fiber and nanosheet reinforcements, and


also considerably higher than that of their hybrid structured re-
inforcements in other Cu matrix composites reported so far [31–36].
Detailed experimental data under the wear test conditions are shown in
Table 2.

3.3. Strengthening mechanisms

To clarify the underlying strengthening mechanism, the morphology


and composition of wear tracks were thoroughly investigated. Fig. 5a
and b shows the typical FESEM images of wear tracks on Cu/GO sam-
ples after fretting under contact loads of 43 and 106 N (corresponding
to the low and high loading conditions, respectively). Under the two
different loads, the wear tracks show the slight plastic deformation with
ridges and asperities (identified by arrows). Specifically, the phase
Fig. 6. Raman spectra of wear tacks of the Cu/GO composite after wear tests enrichment is observed on the ridge and asperity areas on the wear
under different contact loads. The insets are the optical photographs of wear tracks (marked by curves and circles). The high magnification FESEM
tracks. image with corresponding line scanning of elements for the ridge area
indicate that the C element accumulates in this region after the fretting
Cu/GO composite and the blank Cu matrix at contact loads of 43, 86 wear process, as illustrated in Fig. 5c. As depicted in the elemental
and 106 N. Fig. 4a presents their variations of the friction torque (T) as distribution images of an asperity on the wear track after 2 × 104 cy-
a function of fretting cycles. Friction torques of all samples stabilize at cles, a similar accumulation of the C element is also observed on a as-
0.1 Nm with the first 100 fretting cycles because of the adsorption film perity (Fig. 5d–k), indicating that the C-rich tribofilm could be formed
on the fretting surface [24], and eventually arrive at relatively stable on the ridges and asperities of wear tracks after the fretting wear pro-
values. For the Cu matrix, the friction torque is largely sensitive to loads cess. The formation of tribolayer in these areas plays a significant role
and has values between 0.14 and 0.40 Nm; these values matched well in maintaining the stable friction and enhancing the wear resistance
with literature studies for casting Cu materials against steel (0.20 [37–40]. This represents a huge advantage for expanding this strategy
Nm ≤ T ≤ 0.57 Nm) [25]. It can be calculated that the friction coeffi- of GO wrapped spherical metallic powders for advanced tribological
cient (friction force/normal force) increases with the raise of normal applications including pumps, valves, fittings, bearing, winches and
loads, which is very different compared with metal-polymer contacts their gears, as well as ship propellers [41–43], because remarkable
that usually have a decreasing trend of friction coefficient when load friction and wear properties can be obtained with a minimum addition
increases [26,27]. However, for Cu/GO composite samples, the friction of GO shell layers of 0.3 wt.%. Indeed, recent works have shown that
torque shows a load-insensitive behavior, and steadily maintains at GO nanoparticles as additives for lubrication are able to efficiently re-
0.26–0.41 Nm with an improved wear resistance. Owing to the out- duce the friction and wear of metal surfaces [44,45].
standing mechanical strength, the anti-friction behavior of GO is high The GO nanosheet has been demonstrated to possess a strong tri-
insensitive to the change in the load. When stresses are applied on the bofilm-forming ability due to its strong adsorption on the metal surface
surface of the Cu/GO composite, its surface deformation energy would [46]. The adsorption ability is attributed to oxygen functional groups
be significantly released by the out-of-plane wrinkles of GO. Similar and the π bond in the basal plane of the GO nanosheet. Raman spec-
load transfer mechanisms have been also demonstrated by others re- troscopy was conducted to further examine the structural features of
searchers [28]. In addition, this mechanism could enhance the wear the Cu/GO composite after wear tests under different contact loads, as
resistance of the Cu/GO composite. shown in Fig. 6. The G band at ∼1580 cm−1 and the D band at
Fig. 4b presents the typical wear volume of Cu and Cu/GO samples ∼1350 cm−1 of GO can be found in Raman spectra from these three
fretting under varied loads of 43, 86 and 106 N, demonstrating an un- wear tracks. It is noteworthy that intensities of the D and G bands for
expected anti-wear performance of the GO wrapped Cu composite. the wear track at 106 N are distinctly increased due to the adsorption of
After fretting wear tests, the Cu/GO shows an extremely low wear vo- Cu nanoparticles during the fretting wear process, which is considered
lume of 0.12–0.18 mm3 that is 28–37% lower than that of the SPS- as the surface enhanced Raman scattering caused by the chemical en-
consolidated Cu matrix. Moreover, the wear volume of Cu/GO is sig- hancement effect [47]. Also, Raman spectra (Fig. 6) obtained from wear
nificantly reduced by one order of magnitude compared with that of the tracks show slightly decreased intensity ratios (ID/IG) when compared
common wrought counterparts at this composition (see data in Fig. 4b). to the initial Cu/GO composite (Fig. 2b), suggesting that the GO
Interestingly, the Cu/GO composite shows nearly the constant wear structure has been retained during the fretting process. The ID/IG ratios
volume tested under loads from 43 to 106 N (Fig. 4b and c), indicating a for the wear tracks obtained from 43, 86 and 106 N are 0.97, 0.96 and
load-independent volume loss compared with wrought Cu materials. 0.97, respectively, indicating that no more defects are induced even
These results clearly demonstrate that the encapsulation of spherical Cu after fretting under 106 N. In addition, during the fretting process, the
particles in GO is an effective way to improve the tribological perfor- layers of GO nanosheets decreased by the shear stress. Therefore, the
mance. The high strengthening capability can be better presented by 2D band (at ∼2650 cm−1) of the wear track under 106 N is down-
comparing its anti-wear strengthening efficiency with that of bare Cu shifted and become narrower as compared to that of the wear track
materials or Cu-based composites enhanced by other reinforcements under 43 N. Peaks below 1000 cm−1 is observed, which suggests that
[29–31]. The strengthening efficiency of the reinforcement in compo- the formation of metallic oxides on wear tracks. The content of oxides
sites can be defined as the wear resistance (Rw) increment per unit increases significantly for the wear track under 106 N, as demonstrated
weight fraction of the reinforcement, i.e., (Rw(c) - Rw(m))/WfRw(m), where by the intense Raman peaks (Fig. 6).
Rw(c) and Rw(m) are the wear resistance of the composite and the matrix, The detailed valence states of typical elements on wear tracks of the
respectively; and Wf is the weight fraction of the reinforcement. The Cu/GO composite were further characterized by XPS measurements.
wear resistance is calculated as Rw = (Load × No. of cycles × Stroke Fig. 7a shows that the major composition on the wear tracks is Cu with
length)/Wear volume. As shown in Fig. 4d, the strengthening efficiency minor oxidation. Fig. 7b–d indicate that after the wear test, iron and
of GO shell layers in terms of the wear resistance is superior to that of aluminum oxides were formed due to the tribochemical reaction. From
Fig. 7e, it can be seen that after the wear test, the C element on the wear

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Fig. 7. XPS spectra of typical elements on the wear tracks of the Cu/GO composite.

tracks mainly existed in the form of C-C and C]O which could be fretting process, these small GO nanosheets could be easily transferred
oxygen-containing groups in GO, further confirms the structural in- and accumulated into the ridges and asperities existing on wear tracks
tegrity of GO during the friction process [48,49]. (Fig. 5c and d). Consequently, the friction mainly occurs between the
Fig. 8 illustrates the schematic diagram of the anti-friction me- steel counterface and the GO nanosheet film, preventing the direct
chanism of GO shell layers before and after the fretting process. During contact between the Cu matrix and steel counterface. Since the van der
the fretting wear, slight plastic deformation was observed on the sur- waals force of GO nanosheets is relatively weak, which should play a
face of the Cu/GO composite (Fig. 5a and b), leading to the formation of significant role in reducing the friction between the contact surfaces.
wear-induced ridges and quasi-flat graphene-like nanosheets containing Thus, these GO nanosheets could act as anti-friction and anti-wear films
different carbon rings between friction interfaces. With the cyclic to reduce the wear volume and to promote the stable friction torque

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Fig. 8. Schematic diagram of the anti-friction mechanism of GO nanosheet films before and after the fretting process.

(Fig. 8). polytrifluorochloroethylene (PCTFE) micro-particles and application on treating


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