Engineering Science and Technology, an International Journal xxx (xxxx) xxx

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Engineering Science and Technology,

an International Journal
journal homepage: www.elsevier.com/locate/jestch

Full Length Article

Powder metallurgical fabrication of graphene reinforced near-eutectic

Al-Si matrix composites: Microstructural, mechanical and
electrochemical characterization
Nazlı Akçamlı a,⇑, Berk Sß enyurt a, Hasan Gökçe b, Duygu Ağaoğulları b
a
Bursa Technical University, Department of Metallurgical and Materials Engineering, Faculty of Engineering and Natural Science, Yıldırım, Bursa, Turkey
b
Istanbul Technical University, Department of Metallurgical and Materials Engineering, Faculty of Chemical and Metallurgical Engineering, 34469 Maslak, Istanbul, Turkey

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

Article history: Al-10 wt% Si matrix composites reinforced with a few-layered graphene (FLG) were fabricated via a pow-
Received 29 March 2021 der metallurgical route. FLG in varying amounts (0.25, 0.5, 1, 2, and 5 wt%) was incorporated into the Al-
Revised 22 July 2021 10Si matrix via mechanical alloying (MA) for different durations in a high-energy ball mill. The mechan-
Accepted 24 August 2021
ically alloyed (MAed) powders were consolidated by uniaxial pressing and pressureless sintering pro-
Available online xxxx
cesses. The as-blended (non-MAed) and MAed powders and bulk composites were investigated
comparatively in terms of microstructural, thermal, mechanical, tribological and corrosion properties.
Keywords:
The MAed powders demonstrated refined and semi-equiaxed particle morphology with reduced crystal-
Al-Si alloy composites
Few-layered graphene (FLG)
lite size values. Additionally, the FLG/Al10Si composites exhibited advanced microstructural and
Mechanical/microstructural properties mechanical properties by the contribution of MA and reinforcing particles compared to those of the
Corrosion resistance as-blended and unreinforced matrix. The highest hardness and lowest wear rate values were obtained
for the 4 h-MAed Al10Si-2FLG (138 HV and 6.485x10-4 mm3/N.m) and Al10Si-5FLG (178 HV and
7.456x10-4 mm3/N.m) composites. Moreover, the compressive strength of the Al-10Si matrix improved
approximately by 50 and 20% via 0.5 and 2 wt% FLG addition, respectively. Also, lower corrosion resis-
tance properties were observed for the FLG reinforced composites compared to the Al10Si matrix.
Ó 2021 Karabuk University. Publishing services by Elsevier B.V. This is an open access article under the CC
BY-NC-ND license (http://creativecommons.org/licenses/by-nc-nd/4.0/).

1. Introduction corrosion resistance and abrasion, high strength-to-weight ratio

and low coefficient of thermal expansion properties [4,7–9].
Aluminum matrix composites (AMCs) have been used as high- Generally, ceramic-based particles (Al2O3, SiC, TiB2, etc.) were
performance components for the automotive, aerospace, defense incorporated into the Al matrix to improve mechanical properties
and electronic industries instead of conventional materials [1–5]. for demanding applications [6,10–15]. Recently, graphene has
Al-Si alloys are potential materials for replacing heavier materials emerged as a high performance reinforcement candidate for the
in transport sector due to their unique combination of lightness discontinuously reinforced AMCs [16–33]. It is utilized because of
and good mechanical, wear and corrosion properties [4–8]. The its superior mechanical and physical properties such as high sur-
hard Si phase distributed into the Al matrix provides these face area (2630 m2.g
1), excellent thermal conductivity
advanced physical and mechanical properties [5,6]. The combina- (5000 W.m
1.K
1), high Young’s Modulus (~1 TPa) and intrinsic
tion of lightweight and sufficient strength of Al-Si alloys enables strength (130 GPa) [34–36]. Therefore, better properties are exhib-
this alloy family to find usage in automobile parts such as piston ited by the graphene compared to those of the ceramic materials, C
rings, cylinder liners, diesel engine pistons, drive shafts, connecting fibers and carbon nanotubes [37–41]. In this study, mechanical and
rods, etc. The near eutectic Al-10Si alloys are broadly preferred in tribological properties of the Al-10Si alloys are aimed to improve
automotive parts, especially in piston components, because of high by taking the advantages of these superior properties of graphene.
Powder metallurgy (PM) including mechanical alloying (MA)
and subsequent sintering process is an efficient solid-state produc-
tion method, which provides near net-shape formability, low man-
⇑ Corresponding author. ufacturing temperature, high efficiency as well as high
E-mail addresses: [email protected] (N. Akçamlı), [email protected] densification rate and low cost. MA is one of the most effective
ß enyurt), [email protected] (H. Gökçe), [email protected] (D. Ağaoğulları).
(B. S
powder processing method which enables to disperse secondary
Peer review under responsibility of Karabuk University.

https://doi.org/10.1016/j.jestch.2021.08.009
2215-0986/Ó 2021 Karabuk University. Publishing services by Elsevier B.V.
This is an open access article under the CC BY-NC-ND license (http://creativecommons.org/licenses/by-nc-nd/4.0/).

Please cite this article as: Nazlı Akçamlı, B. Sß enyurt, H. Gökçe et al., Powder metallurgical fabrication of graphene reinforced near-eutectic Al-Si matrix
composites: Microstructural, mechanical and electrochemical characterization, Engineering Science and Technology, an International Journal, https://
doi.org/10.1016/j.jestch.2021.08.009
Nazlı Akçamlı, B. Sßenyurt, H. Gökçe et al. Engineering Science and Technology, an International Journal xxx (xxxx) xxx

reinforcing particles more homogeneously in a metallic matrix (C18H36O2, ZAG, 99.5% pure) was added as a process control agent
[10,13–15,17,21,22,42–47]. Also, it allows to extend the solid solu- (PCA) for preventing the welding of ductile Al particles during the
bility limits and produce non-equilibrium (metastable) state alloys milling. Starting powders (8 g in total) were initially mixed in a
or compounds that cannot be obtained at room temperature with dry powder blender for 2 h, and they were named as non-MAed
conventional methods and hinders the undesired reactions (or as-blended) powders. The as-blended powder mixtures were
between the reinforcement phase and matrix because of being a loaded to the milling vials in a glove box under Ar atmosphere to
room temperature technique [45–47]. provide a protective atmosphere against oxidation. Then, they were
In the literature, there are only few studies on the graphene mechanically alloyed (MAed) in a high-energy vibratory ball mill.
reinforced near-eutectic and hyper-eutectic Al-Si matrix compos- The parameters of MA are explained in Table 1. Brief names were
ites, and liquid-state fabrication techniques were employed in given to the powders according to their FLG amount and MA dura-
these studies [48,49]. Graphene nanoflakes reinforced Al-20Si tions: for example, 2 h of MAed Al-10 wt% Si-1.0 wt% FLG powders
composites were produced via the pressure infiltration method, were briefly named as Al10Si-1G-2 h.
and it was reported that the hardness and the elastic modulus of The as-blended and MAed powders were pre-compacted as
the composites were improved gradually with the increasing gra- cylindrical samples (/ 12 mm) under 650 MPa uniaxial pressure
fen amount [48]. In another study, Cu nanoparticles-coated gra- in a MSE MP-0710 uniaxial hydraulic cold press. Prior to the sinter-
phene nanoplatelets reinforced Al-10Si composites were ing process, the stearic acid was removed by debinding procedure
produced by using stir casting technique. A Cu coating on the gra- carried out at 425 °C for 2 h under flowing Ar atmosphere in a MSE
phene was applied to adjust the density difference between the tube furnace. Subsequently, they were subjected to pressureless
metal matrix and graphene, and thereby to prevent the float of gra- sintering at 565 °C for 2 h under flowing Ar gas with a 5 °C/min
phene during the stirring. Improved tensile strength properties heating and cooling rate in a Protherm tube furnace.
were reported by the addition of 0.5 wt% graphene [49]. Addition- A Bruker D8 Advanced Series X-ray diffractometer (XRD) was uti-
ally, 4043 Al alloy (Si: 5.9; Fe: 0.8 in wt.%) matrix composites rein- lized for the phase analyses of the MAed powders and sintered com-
forced with carbon nanosheets were produced by hot extrusion posites. The analysis conditions were CuKa radiation (k = 1.5406 Å) at
and gas tungsten arc (GTA) welding processes [23]. However, any 40 kV and 35 mA with 2h range of 10-90°, step size of 0.02° and scan
study on the powder metallurgy of the graphene reinforced Al-Si rate of 2°/min. Morphological and microstructural characterization
matrix composites was not reported in the open literature yet. of the powder and bulk samples were performed via Zeiss/Gemini
Likewise, the tribological and corrosion properties of the Al-Si- 300 scanning electron microscope (SEM) and JEOL 2100 JEM high-
graphene composites have not been reported up to now. resolution transmission electron microscope (HRTEM) with respec-
In the present study, graphene reinforced near-eutectic Al-Si tive accelerating voltages of 15 kV and 200 kV. Additionally, during
alloy matrix composites were produced with the aim of improving the SEM and TEM analyses, the compositions of the obtained phases
the mechanical and wear properties of these alloys for applications were probed by an energy dispersive spectrometer (EDS). Thermal
like automotive parts such as engines, piston parts, cylinder blocks properties of the as-blended and MAed powders were investigated
and etc. Few-layered graphene (FLG) reinforced Al-10 wt% Si in a Linseis PT1600 differential scanning calorimeter (DSC) by heating
matrix composites were produced via mechanical alloying fol- approximately 10 g of sample up to 700 °C under Ar atmosphere with
lowed by pressureless sintering. The high-energy mechanical a heating rate of 5 °C/min. Archimedes’ density values of the sintered
milling process was utilized for different durations up to 8 h to samples were measured in an ethanol medium by repeating mea-
obtain a homogeneous alloy of starting powders with varying surements three times for each sample.
FLG (0.25, 0.5, 1, 2 and 5 wt%) amounts. The effects of different Microhardness values of the bulk samples were determined
FLG quantities and milling durations on the properties of the com- using a Qness microhardness tester by indenting a load of 100 g
posites were examined in details via thermal, structural, mechan- for 10 s. The results were obtained by taking at least fifteen mea-
ical, tribological and corrosion characterizations. It is also surements on a sample. Reciprocating wear tests were applied to
believed that this study will give contribution to the literature with the bulk samples in a Bruker UMT2 Tribometer under these condi-
its findings on the powder metallurgical fabrication of the Al-10Si- tions: 3 N force, 5 mm.s
1 speed, 25000 mm total distance and
graphene composites. chrome steel balls (Ø: 5 mm, ASTM E52100). Wear volume loss
amounts of the samples were observed using a Veeco Dektak
6 M Stylus profilometer. The average wear volume loss amounts
2. Materials and method and corresponding wear rates (mm3/N.m) were determined by tak-
ing three measurements. The evolving wear tracks were investi-
Al-10 wt% Si matrix (Al10Si) composites reinforced with gated using the SEM to investigate the wear mechanism. The
few-layered graphene (FLG) were prepared from the Al wear rate values are calculated based on the profilometer results
(Alfa Aesar,
325 mesh, 99.5%), Si (Alfa Aesar,
325 mesh, 99.5%) according to the equation given below:
and FLG starting powders. The FLG was produced in an originally
½Area loss  Wear track length ð5 mmÞ
designed reactor via direct current arc discharge method in our lab- Wear Rate ¼ ð1Þ
½Test load ð3 NÞ  Total wear distance ð25 mÞ
oratories. The production and properties of FLG were explained in
details in our previous study [20]. According to the particle size mea-
surements which were conducted via Malvern Mastersizer 3001, Al
Table 1
and Si powders have 10.9 and 4.12 lm mean particle sizes, respec- The employed process parameters for MA process.
tively. Additionally, average particle size and BET surface area of
Parameters Descriptions
the FLG were determined as 10.42 nm and 153.52 ± 2.36 m2/g,
respectively via a Nano-flex particle size analyzer (PSA) and a Mill type Spex Type Mixer/Mill
Micromeritics Tristar II surface area analyzer. The near-eutectic Rotation speed 1200 rpm
Vial/Ball material Hardened Steel
Al-Si powder system was aimed to produce by utilizing the Si Vial volume 55 ml
amount as 10 wt%. FLG in amounts of 0.25, 0.5, 1.0, 2.0 and 5.0 wt Ball diameter 6 mm
% were added to Al10Si matrix as reinforcement agent. MA process Ball-to-powder weight ratio 8:1,
was applied starting powder mixtures to achieve well-dispersed Milling atmosphere Ar
Milling time 0, 2, 4, 8 h
graphene nanoparticles in the Al-10Si matrix. Stearic acid
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Nazlı Akçamlı, B. Sßenyurt, H. Gökçe et al. Engineering Science and Technology, an International Journal xxx (xxxx) xxx

Compression tests were conducted in a Shimadzu AG-X Plus

universal test instrument on 8 mm  18 mm cylindrical specimens
with a loading rate of 0.18 mm/min. From the results of compres-
sion tests, yield and compressive strength and compressive strain
values were determined. The yield strength is calculated by draw-
ing a straight line parallel to the elastic portion of the stress–strain
curve at strain offset of 0.002. The stress value obtained from the
intersection of the stress–strain curve is taken as the yield strength
(rys).
Electrochemical properties were examined at 25 °C by a CH
instruments Electrochemical Analyzer/Workstation (CHI608E) in
a three-electrode cell. The Ag/AgCl electrode, platinum plate and
studied sample electrode were functioned as the reference, coun-
ter, and working electrodes, respectively. The working electrode
was dipped in a 3.5 wt% NaCl solution until a steady free open cir-
cuit potential (OCP) was reached before the measurement were
executed [50]. The polarization curves were obtained at
260
to +260 mV intervals with OCP obtained at a 1 mV.s
1 scan rate.

3. Results and discussion

3.1. Microstructural and thermal properties of the as-blended and

MAed powders

X-ray diffraction patterns of some non-MAed and MAed Al10Si-

xG (x= 0 – 5 wt%) powders are shown in Fig. 1a-b, respectively.
Al10Si-2G and Al10Si-5G powders were selected as representative
samples. In the XRD patterns of the non-MAed and MAed powders,
Al (ICDD Card #: 04–0787, Bravais lattice: face-centered cubic, a =
b = c = 0.405 nm) and Si (ICDD Card #:27–1402, Bravais lattice:
face-centered cubic, a = b = c = 0.543 nm) phases were detected.
However, the graphene phase cannot be determined in the XRD
patterns of the as-blended and MAed powders that even have
5 wt% of graphene due to its comparatively low crystallinity. By
comparing the XRD patterns of non-MAed and MAed powders, it
is seen that the intensity of MAed powders’ XRD peaks reduce,
and they broaden by the effect of mechanical deformation. Also,
this deformation effect becomes more evident in case of longer
MA durations, and the crystallinity of 8 h-MAed powders reduces
Fig. 1. XRD patterns of (a) non-MAed and (b) MAed Al10Si-xG (x= 2 and 5 wt%)
compared to that of the 4 h-MAed ones. These changes in the powders.
XRD patterns indicate the reduced crystallite size and increased
lattice strain of the powders. In addition, any carbide phase
evolved by the reaction between the graphene and matrix ele- spherical particle morphology, as observed in the SEM images
ments (Al and Si) is not detected in the structure of the MAed pow- (Fig. 2d-e) [20]. Also, according to the EDS analyses in Table 2,
ders. During the milling, the average lattice strain rises as a result points 3 and 4 in Fig. 2e are the separate Si and Al particles, respec-
of climbing dislocation density in the severely deformed regions. tively. On the other hand, as seen in Fig. 2b, in the microstructure
The mechanically alloyed materials are subjected to particle size of 4 h-MAed powders, entwined particles including different
refinement as a function of milling duration. In addition, refine- phases form a more homogenous powder mixture. By observing
ment effect increases by the utilization of hard particles during the clustered 4 h-MAed Al10Si-2G powders at a higher magnifica-
the milling due to the interaction of dislocations with tough rein- tion in Fig. 2f, much smaller Si particles embedded into the ductile
forcing particles and thereby formation of dislocations as a result Al particles can be seen. However, it is hard to observe the gra-
of mismatch between the thermal expansion coefficients of metal phene particles due to their few-layered structures. The brittle Si
matrix and these particles [47]. particles are fragmented during the high-energy ball milling and
The secondary electron SEM micrographs of the non-MAed, 4 embedded into the flattened Al particles together with graphene,
and 8 h-MAed Al10Si-2G powders are illustrated in Fig. 2a-g at dif- thus a composite powder structure develops. By MA for 8 h, the
ferent magnifications. Table 2 shows the compositions of the Al10Si-2G powders gain a finer structure as seen in Fig. 2c. Thus,
marked regions in Fig. 2a-g according to the EDS analyses. In the composite Al-Si-graphene powders with submicron-sized Si and
SEM image of the non-MAed Al10Si-2G powders, discrete particles graphene particles are obtained, according to Fig. 2f and g.
consisting of Al, Si and graphene phases are observed, and they The bright-field TEM (BF-TEM) and high-resolution TEM images
have fairly different particle sizes ranging between 1 and 20 lm. (HR-TEM) of the Al-10Si-5G-4h powders are shown in Fig. 3a-f.
Additionally, graphene particles (in red-squared areas) located Fig. 3a, b, d and e illustrate the submicron-size particles including
between Al and Si particles are observed as rounded shaped parti- Si and graphene phases introduced into the ductile Al matrix. Thus,
cles with roughly 1.5 lm radius (Fig. 2d-e). The graphene utilized BF images indicate composite structures of the particles. The HR-
in this study was produced by arc discharge method as few-layered TEM micrograph in Fig. 3c acquired from the red-squared area in
graphene nano particles under N2 + He gas flow with semi- Fig. 3b belongs to the Al phase ({1 1 1} family of plane and

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Nazlı Akçamlı, B. Sßenyurt, H. Gökçe et al. Engineering Science and Technology, an International Journal xxx (xxxx) xxx

Fig. 2. SEM images of the (a, d, e) non-MAed, (b, f) 4 h-MAed and (c, g) 8 h-MAed Al10Si-2G powders.

are demonstrated in Fig. 5a-e. In the BF-TEM image (Fig. 5a), a rect-
Table 2
angular shaped particle is observed. According to the EDS mapping
EDS results of marked regions in Fig. 2.
results in Fig. 4b-d, this rectangular particle is a submicron-sized
Regions in Fig. 2d, e, f and g Amounts of elements (wt.%) and Si-based particle, which is also covered by ductile Al phase
Al Si C and a low amount of graphene phase. The line-EDS analysis con-
001 5.23 5.23 89.54 ducted on this particle through the line marked on Fig. 4e reveals
002 26.75 16.50 56.75 the particle’s composition as 8.4 wt% Al, 86.7 wt% Si and 4.9 wt% C.
003 2.63 95.68 1.69 Fig. 5 illustrates the DSC curves of the Al10Si-0 h, A110Si-8 h
004 100.0 – – and A10Si-2G-8h powders up to 700 °C. In the DSC curves,
005 99.29 – 0.71
endothermic peaks at around 640, 576 and 572 °C are observed
006 16.63 81.68 1.69
007 55.42 43.32 1.26 for the non-MAed Al10Si and 8 h-MAed Al10Si and Al10Si-2G pow-
008 36.61 62.52 0.87 ders, respectively. Therefore, the MAed powders show a melting
point that corresponds well with the eutectic point of the Al-Si bin-
ary system which is at around 577 ± 1 °C [51]. Whereas, the melt-
0.233 nm interplanar spacing). Fig. 3e includes the nano-sized Si ing of non-MAed powders does not conform to this alloy behavior,
flakes (dark regions, about 10–50 nm size) inserted into the Al and hence they melt above the eutectic temperature which is
crystallites. Furthermore, Fig. 3f (acquired from the Fig. 3e) proves rather near to the pure aluminum’s melting point. Therefore, the
the presence of nano-scaled Si particles ({2 2 0} family of plane and effect of MA process can be clearly observed by comparing the
0.192 nm interplanar spacing) embedded into the Al phase with thermal behaviors of the as-blended and MAed powders. In addi-
flake morphology. tion, any peak that arises from a chemical reaction between the
The BF-TEM image, TEM-EDS mapping results for Al, Si and C carbon and Al or Si is not detected in the DSC curves of the
elements and line-EDS spectrum of the Al-10Si-5G-4h powders inspected powders.

Fig. 3. (a, b, d, e) Bright-field TEM images of the Al10Si-5G-4 h powders and (c, f) High-resolution TEM images of the regions respectively marked on (b) and (e).

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Nazlı Akçamlı, B. Sßenyurt, H. Gökçe et al. Engineering Science and Technology, an International Journal xxx (xxxx) xxx

Fig. 4. (a) TEM image, EDX mapping results of (b) Al, (c) Si and (d) C elements, and (e) line-EDS spectrum for the Al10Si-5G-4 h powders.

3.2. Physical, microstructural and mechanical properties of the density values are obtained for the composites originated from
sintered composites the as-blended powders compared to those of produced from the
MAed powders. Also, graphene addition does not have an unfavor-
X-ray diffraction patterns of the Al10Si-xG (x= 0 – 5 wt%) com- able effect on the densification rates. Moreover, the composites
posites sintered from the 4 and 8 h-MAed powders are shown in fabricated from the 8 h-MAed powders generally have lower Archi-
Fig. 6. XRD analyses were conducted on the composites including medes’ and relative density values.
2 and 5 wt% of FLG, due to they represent the higher interaction The change of microhardness values of the Al10Si-xG (x= 0, 0.5,
between the metallic matrix and graphene phase. In the XRD pat- 1, 2 and 5 wt%) composites according to the FLG amount and MA
terns, Al and Si phases were detected similar to the XRD patterns of duration is illustrated in Fig. 7. As seen from the Fig. 7, the FLG
the MAed Al10Si-xG (x= 2 and 5 wt%) powders. After the sintering amount plays a significant role on the hardness of sintered com-
treatment which was posites, and the hardness values gradually increase as the gra-
conducted at 565 °C for 2 h under Ar flow, Al and Si phases are phene amount increases. The steady increase in the 4 h-MAed
detected in the bulk structures. The intensities of the 8 h-MAed Al10Si-xG (x= 0 to 0.25, 0.5, 1, 2 and 5 wt%) composites’ hardness
composites’ XRD peaks decrease compared to the 4 h-MAed com- values by the increasing FLG amount is determined as 102, 106,
posites due to the growth of mechanical energy induced into the 109, 113, 138 and 178 HV, respectively. Additionally, utilization
powders during the extended milling durations. In addition, low and duration of the MA process have a major effect on the eleva-
amount of aluminum carbide phase (Al4C3) resulted from the tion of the hardness. The hardness values of the non-MAed samples
chemical reaction between graphene and Al phases occurred dur- are very low compared to those of their MAed counterparts, and
ing the sintering process is detected in the XRD patterns. Addition- any increment by the increasing FLG amount is not determined
ally, oxides or any other impurity phase are not detected in the for the as-blended samples. Generally, the highest hardness values
XRD investigations of the sintered composites. are illustrated by the 4 h-MAed composites, and commonly hard-
The theoretical, Archimedes and relative density values of the ness values reduce or do not show a significant increase after this
sintered Al10Si-xG (x= 0.25, 0.5, 1.0, 2.0 and 5.0 wt%) composites duration. Therefore, the optimum or sufficient MA duration can be
are given in Table 3. The theoretical density values were calculated accepted as 4 h in terms of the hardness properties.
according to the rule of mixture by taking the theoretical values of Secondary electron SEM micrographs of the 4 and 8 h-MAed
Al, Si and graphene as 2.70, 2.33 and 1.77 g/cm3, respectively. Al10Si-1G composites are illustrated in Fig. 8a-d. In the SEM
Accordingly, the theoretical density values of Al10Si-xG compos- images of the composites, highly densified structures are observed.
ites are ranging between 2.677 and 2.609 g/cm3. Highly densified The chemical compositions of the marked phases in Fig. 8b and d
bulk structures are obtained according to the densification rates which were determined with SEM-EDS analyses are given in
which reach to between 89.1 and 98.9%. Generally, lower relative Table 4. According to the SEM-EDS results, mainly three different
phases are detected in the microstructure of the Al10Si-1G com-

Fig. 5. DSC curves of the (a) Al-10Si-0 h, (b) Al-10Si-8 h and (c) Al-10Si-2G-8 h
powders. Fig. 6. XRD patterns of the 4 and 8 h-MAed Al10Si-2G and Al10Si-5G composites.

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Nazlı Akçamlı, B. Sßenyurt, H. Gökçe et al. Engineering Science and Technology, an International Journal xxx (xxxx) xxx

Table 3
Theoretical, Archimedes and relative density values of the sintered composites.

Sample Theoretical Archimedes Relative

Density (g/cm3) Density (g/cm3) Density (%)
Al10Si-0 h 2.677 2.514 93.9
Al10Si-2 h 2.516 94.0
Al10Si-4 h 2.530 94.5
Al10Si-6 h 2.515 94.0
Al10Si-8 h 2.471 92.3
Al10Si-0.25G-0 h 2.673 2.390 89.4
Al10Si-0.25G-2 h 2.523 94.4
Al10Si-0.25G-4 h 2.546 95.2
Al10Si-0.25G-6 h 2.581 96.5
Al10Si-0.25G-8 h 2.511 93.9
Al10Si-0.5G-0 h 2.700 2.424 90.8
Al10Si-0.5G-0–2 h 2.490 93.3
Al10Si-0.5G-4 h 2.484 93.0
Al10Si-0.5G-6 h 2.484 93.0
Al10Si-0.5G-8 h 2.478 92.8
Al10Si-1G-0 h 2.663 2.439 91.6
Al10Si-1G-2 h 2.471 92.8
Al10Si-1G-4 h 2.483 93.3
Al10Si-1G-6 h 2.498 93.8
Al10Si-1G-8 h 2.478 93.1
Fig. 7. Hardness values of the sintered Al10Si-xG (x= 0, 0.5, 1, 2 and 5 wt%) samples
Al10Si-2G-0 h 2.649 2.360 89.1
according to the graphene amount and MA duration.
Al10Si-2G-2 h 2.598 98.1
Al10Si-2G-4 h 2.470 93.2
Al10Si-2G-6 h 2.472 93.3
Al10Si-2G-8 h 2.459 92.8 0.00065 mm3/N.m, while those prepared from the 8 h-MAed pow-
Al10Si-5G-0 h 2.609 2.449 93.9 ders illustrate the wear rate amounts between 0.0025 and
Al10Si-5G-2 h 2.507 96.1 0.00075 mm3/N.m. The wear rate amounts of the 4 h-MAed com-
Al10Si-5G-4 h 2.580 98.9
posites are lower than that of the 8 h-MAed ones in general. More-
Al10Si-5G-6 h 2.457 94.2
Al10Si-5G-8 h 2.539 97.3 over, the lowest wear rate and highest wear resistance are
demonstrated by the composites reinforced by 2 wt% FLG, whereas
the lowest wear resistance values belong to the Al-10Si matrix
samples. The increase in the wear resistance and hardness values
posites. Accordingly, the a-Al and eutectic b-Si phases are evolved of the 4 h-MAed composites with the increasing FLG amount show
after the sintering process. The point EDS results for 001 and 006 generally a parallel tendency. During the reciprocating wear test,
(in Fig. 8b and d) in the Table 4 shows the presence of eutectic the wearing force operating on the sample is countered by the
b-Si phases. This is also shown by the EDS analyses (points 002 reinforcing phase network, and thereby FLG reinforced composites
and 004) that the matrix consists of a-Al phase and an amount can demonstrate a higher wear resistance compared to the matrix
of carbon. Additionally, a needle-like phase is observed in the structure [22,42]. In addition, it was reported in the previous stud-
SEM images in Fig. 8a-d. Fig. 8e shows the EDS spectrum of the ies that graphene addition could reduce the wear rates of the Al
point 003 in the Fig. 8b. According to the point EDS analyses taken matrix composite by means of its lubricant effect [22,31,32]. The
on the points marked as 003 and 005 (in Fig. 8b and d), these change of mean friction coefficient values of Al10Si-xG composites
needle-like phases include 11.05 wt% Si - 6.44 wt% Fe and according to the FLG amount and MA duration is shown in Fig. 10b.
9.74 wt% Si - 5.72 wt% Fe, respectively. Thus, these needles are The mean friction values are ranging between 0.474 and 0.704 lm,
thought to be an intermetallic compound formed between Al, Si and they illustrate a descending trend with the increasing gra-
and Fe. Fe can stem from worn off the steel milling medium. These phene amount. Therefore, it can be said that the wear coefficient
intermetallic compounds could not be determined in the XRD anal- values demonstrate a downward tendency with the reducing wear
yses of sintered composites (Fig. 6), probably due to their relatively rate.
low amount. Secondary electron SEM images of the Al10Si-0.25G-4h, Al10Si-
Fig. 9a shows SEM image of the 4 h-MAed Al10Si-2G composite, 2G-4h and Al10Si-2G-8h samples’ worn surfaces are illustrated in
and Fig. 9b-c illustrate the results of elemental EDX mapping anal- Fig. 10c-h at different magnifications. In the general SEM images,
yses for Si and C taken on Fig. 9a. EDX mapping analyses were con- it is seen that a more severe wear is developed on the Al10Si-
ducted for observing the distribution of Si and graphene phases in 0.25G-4h sample and its volume loss is larger than those of the 4
the and 8 h-MAed Al10Si-2G samples. In higher magnifications
microstructure. Fig. 9a shows a highly densified composite (Fig. 10f), deeper wear grooves are observed on the Al10Si-
structure including a-Al and b-Si phases. According to the EDX 0.25G-4h composite. According to the EDS analyses, the white par-
analysis for Si in the Fig. 9b, the b-Si phase is homogeneously ticles marked in red squares on Fig. 10f are oxidized matrix parti-
and finely distributed throughout the microstructure. In addition, cles. Harsh wear conditions can give rise to the evaluation of
C mapping analysis given in Fig. 8c proves the even dispersion of frictional heat and local oxidations on the wear surface during
C in the composite structure. Therefore, it can be said that by the wear test [10,42]. However, wear tracks observed on the
means of high-energy MA process, uniform dispersion of secondary Al10Si-2G-4h and Al10Si-2G-8h composites include shallower
Si phase and reinforcing graphene particles is obtained. tracks and grooves, which are compatible with the determined
Wear rate values of 4 and 8 h-MAed Al10Si-xG (x= 0, 0.25, 0.5,1, wear rates in Fig. 10a. Al10Si-2G composites illustrate a higher
2 and 5 wt%) composites relative to the FLG amounts are illustrated resistance to the wear forces by means of higher hardness values
in Fig. 10a. According to the reciprocating wear tests, the wear rate and a more dense network of reinforcing particles. The non-
amounts of the Al10Si-xG composites fabricated from the 4 h- existence of adhesive wear track on the worn surfaces indicates a
MAed powders are determined between 0.0022 and good interface binding between graphene nanoparticles and Al-Si

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Nazlı Akçamlı, B. Sßenyurt, H. Gökçe et al. Engineering Science and Technology, an International Journal xxx (xxxx) xxx

Fig. 8. SEM images of the (a, b) AlSi-2G-4 h, (c, d) AlSi-2G-8 h composites, and (e) EDS spectrum of point 003 marked on (b).

Table 4
EDS results of marked regions in Fig. 8.

Regions in Fig. 8b and d. Amounts of elements (wt.%)

Al Si C Fe
1 39.04 59.73 1.23 –
2 96.11 1.64 2.25 –
3 82.51 11.05 – 6.44
4 97.48 0.78 1.74 –
5 84.54 9.74 – 5.72
6 32.53 66.58 0.89 –

matrix. Moreover, due to the worn surfaces include predominantly 371 and 316 MPa, respectively. Therefore, the rys and rucs values
grooves, it is found out that the main wear mechanism applied on of Al10Si-xG samples gradually decrease by addition of graphene
the composites is abrasive type wear. above 0.5 wt%. Moreover, the failure strain values of the Al10Si-
Compressive strain–stress curves of the Al10Si-xG (x= 0, 0.5, 1, xG composites are determined as between 1.5 and 2.9%. The ef
2 and 5 wt%) composites sintered from the 4 h-MAed powders are value of the Al-10Si alloy is measured as 2.9% and it reduces
shown in Fig. 11. The yield strength (rys), ultimate compression slightly by the increase of reinforcement amount. The graphene
strength (rucs) and failure strain (ef) values obtained from the addition in amounts of 0.5, 1 and 2 wt% does not cause a dramatic
compressive strain–stress curves are shown in Fig. 12a, b and c, effect on the compressive strain values, which are determined as
respectively. The Al-10Si alloy’s rucs and rys values are determined between 2.4 and 2.7%. However, by the increase of FLG amount
respectively as 260 and 295 MPa. Reinforced samples including up to 5 wt%, the ef value decreases to 1.5%. In addition, as observed
to 5 wt% graphene illustrate higher rucs values than Al-10Si alloy from Figs. 11 and 12, an evident decrease is seen in the rys and
matrix. As seen in Fig. 12a and b, the highest rucs and rys values rucs values by the utilization of 5 wt% graphene.
are represented by the Al10Si-0.5G sample as 395 and 442 MPa, The enhancement in the mechanical properties of the graphene
respectively. Thus, by the addition of 0.5 wt% graphene, both rucs reinforced Al matrix composites is ensured by the high hardness,
and rys values are improved approximately by 50%. The rucs val- modulus and strength properties of nano-sized graphene phase
ues of the Al10Si-1G and Al10Si-2G composites are determined [34–38]. The possible strengthening mechanisms acting on the

Fig. 9. (a) SEM image and EDX elemental mapping results for (b) Si and (c) C for the Al10Si-2G-4 h composite.

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Nazlı Akçamlı, B. Sßenyurt, H. Gökçe et al. Engineering Science and Technology, an International Journal xxx (xxxx) xxx

Fig. 10. (a) Wear rates and (b) Mean friction coefficient values of the composites originated from the 4 and 8 h-MAed powders according to graphene amounts, and SEM
images of the wear tracks: (c,f) AlSi-0.25G-4 h, (d, g) AlSi-2G-4 h and (e, h) AlSi-2G-8 h composites.

powder metallurgy processed graphene-Al composites are grain mechanisms are activated due to mechanical energy introduced
refinement (grain size strengthening), strain hardening, Orowan into the particles, which provides crystallite size refinement and
strengthening (dispersion strengthening), load transfer from lattice strain increase [47,52,53]. One of the most prominent
matrix to graphene and thermal mismatch [51–60]. By the MA pro- strengthening mechanisms for the graphene reinforced MMCs is
cess, grain refinement (Hall-Petch principle) and strain hardening the Orowan mechanism [54–58]. In order to enhance the strength

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Nazlı Akçamlı, B. Sßenyurt, H. Gökçe et al. Engineering Science and Technology, an International Journal xxx (xxxx) xxx

matrix’s Icorr value is lower compared to those of the Al10Si-xG

composites and a gradual increase is seen by the increasing FLG
amount. These findings indicate the lower electrochemical corro-
sion resistance of the Al10Si-FLG composites. This may be arisen
from the high electrical conductivity of few-layered graphene
which can constitute a galvanic couple between the matrix and
reinforcement phase. The corrosion rate of Al-10Si matrix is accel-
erated by the incorporation of graphene. The corrosion rate of Al-
10Si alloy increases from 1.98 to 3.75 mpy.year
1 by the addition
of 0.5 wt% graphene, and it increases further by the increasing rein-
forcement amount. The corrosion mechanism of Al is needed to
clarify to understand the electrochemical behavior of composite.
Aluminum hydroxide is formed as corrosion product by means of
the reaction of Al with water through the following reactions:

AlðsÞ ! AlðaqÞ 3þ + 3 e
(anodic reaction) ð2Þ

3H2 O + 3e
! 3/2H2ðgÞ + 3OHðaqÞ
(cathodic reaction) ð3Þ

Fig. 11. Compressive stress–strain curves of the Al10Si-xG (x= 0, 0.5, 1, 2 and
5 wt%) composites sintered from the 4 h-MAed powders. Al3þ + 3OH— ! Al(OH)3 (corrosion product) ð4Þ
A protective oxide film is formed on the Al surface when it is
exposed to the air and the stability and continuity of this oxide
efficiently and activate the Orowan mechanism, the graphene layer is strongly affected by the microstructure and presence of
phase should be homogeneously dispersed in the matrix. The the reinforcement phases. During the exposure of water, Al or
evenly and densely dispersed graphene particles hinder the dislo- Al2O3 reacts with water by forming H2 gas and Al(OH)3 which acts
cation motion in the grain interior [54–58]. In addition, thermal as a barrier layer providing a partial protection in the chloride ions
mismatch strengthening generated due to mismatch of the ther- medium. The interrupted sites form weak points for corrosion. The
mal expansions coefficients of graphene and Al matrix improves causes that weaken the corrosion resistance of the particulate rein-
the strength by the restricted dislocation motion [59–61]. forced MMCs can be proposed as: (1) formation of galvanic couple
between the alloy matrix and reinforcing phase, (2) interfacial
3.3. Electrochemical properties of the sintered composites phase formation between the matrix and reinforcement additive,
(3) impurity phases and contaminants stemmed from the produc-
Fig. 13 displays the polarization curves for the 4 h-MAed Al10Si- tion process and microstructural modifications [37,38]. In our pre-
xG (x= 0, 0.5, 1 and 2 wt%) composites obtained in a three- vious study, it was determined that graphene nanoplatelets (GNP)
electrode cell. Regarding the hardness values, 4 h of milling is eval- addition worsened the corrosion resistance of pure aluminum and
uated as the optimum MA duration. Thus, the effect of increasing powder metallurgically processed Al and Al-0.5GNP composites’
FLG amount on the corrosion behaviors of the 4 h-MAed Al-10Si corrosion rates were determined respectively as 3.79 and 7.03
matrix composites were investigated and compared to the Al- mpy.year
1 under similar conditions [22]. Additionally, the effect
10Si alloy. The determined corrosion potential (Ecorr), corrosion of graphene addition on the corrosion rate of Al alloy matrix was
current density (Icorr), and corrosion rate values are given in Table 5. investigated in some previous studies. In these studies, it was
According to Fig. 13 and Table 5, Al-10Si matrix shows a higher shown that graphene had a deteriorative effect on the corrosion
Ecorr value than those of the graphene reinforced composites. The resistance of the Al matrix due to the fact that it works as an effec-
Ecorr values reduce further by the increasing reinforcement amount tive cathode against the surrounding matrix to accelerate corrosion
up to 2 wt% graphene and polarization curves of the Al10Si-G com- [22,33,37,38,40]. Moreover, in the powder metallurgy processed
posites pull away to negative side as a whole compared to the composites, porosities (due to the comparatively low densification
Al10Si matrix. This phenomenon can be explain by the migration rates) at the interface between the metal matrix and reinforcing
speed of electrons in the graphene including structure. During particle act as preferred corrosion sites [26,38]. Furthermore, the
the anodic reaction, the transfer of metal ions to the solution oxide film evolved on the Al matrix creates a protection layer
increases by the graphene addition and this rate exceeds the rate against corrosion. However, by the addition of a reinforcing agent
of electron flow from the cathode to external circuit. Thus, the to the matrix, this oxide layer is interrupted and these unprotected
cathode is polarized to more negative side due to the excessive sites form weak points which can be attacked by the corrosive
charge accumulated on its surface [62]. In addition, Al-10Si environment and hence composite is corroded faster [22,38,41].

Fig. 12. Changes of (a) rys, (b) rucs and (c) ef values of the composites with the varying FLG amount.

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Nazlı Akçamlı, B. Sßenyurt, H. Gökçe et al. Engineering Science and Technology, an International Journal xxx (xxxx) xxx

 The Al10Si-xG composites illustrated improved wear resistance

compared to the Al-10Si matrix. The wear rate amounts of the
4 h-MAed Al10Si and Al10Si-2G samples were determined as
0.0022 and 0.00065 mm3/N.m, respectively.
 The corrosion resistance of the Al-10Si alloy gradually
decreased by the increasing FLG amount due to graphene parti-
cles behaved as active cathodes to accelerate the rate of
corrosion.

Declaration of Competing Interest

The authors declare that they have no known competing finan-

cial interests or personal relationships that could have appeared
Fig. 13. Polarization curves of the Al10Si-xG-4 h composites: (a) x= 0, (b) x= 0.25, to influence the work reported in this paper.
(c) x= 0.5, (d) x= 1 and (e) x= 2.

Acknowledgment
Table 5
Corrosion test results for the Al10Si-xG-4 h (x= 0, 0.25, 0.5, 1 and 2 wt%) composites. This study was financially supported by ‘‘The Scientific and
_
Technological Research Council of Turkey (TÜBITAK)” with the pro-

1
Sample Ecorr (V) Icorr (A) Corrosion Rate (mpy.year )
ject number of 118M185.
Al10Si
0.907 9.160x10-6 1.98
Al10Si-0.25G
0.992 16.57x10-6 3.60
Al10Si-0.5G
1.015 17.24x10-6 3.75 References
Al10Si-1G
1.094 82.84x10-6 18.04
Al10Si-2G
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