Nano Research

https://doi.org/10.1007/s12274-017-1779-9

A novel method for preparing and characterizing

graphene nanoplatelets/aluminum nanocomposites
Duosheng Li1 (), Yin Ye1, Xiaojun Liao1, and Qing H. Qin2

1
School of Materials Science and Engineering, Nanchang Hangkong University, Nanchang 330063, China
2
Research School of Engineering, Australian National University, Acton ACT 2601, Australia

Received: 4 April 2017 ABSTRACT

Revised: 25 July 2017
Accepted: 28 July 2017
© Tsinghua University Press
and Springer-Verlag GmbH
Germany 2017
KEYWORDS
graphene nanoplatelets,
nanocomposites,
mechanical properties,
two-step method
Graphene nanoplatelets/aluminum (GNPs/Al) nanocomposites were fabricated
using a novel two-step method. High resolution transmission electron microscope
(HRTEM), Raman, field emission scanning electron microscopy (FESEM), X-ray
diffraction (XRD), energy dispersive X-ray spectroscopy (EDS), EDS mapping,
and mechanical testing system (MTS) were applied to characterize the
microstructure and mechanical properties of the GNPs/Al nanocomposites. The
GNPs were homogeneously dispersed in GNPs/Al nanocomposites, and presented
a fine interface behavior and microstructure characteristics. A harmful phase,
aluminum carbide (Al4C3), was not observed in significant quantities in the
nanocomposite. Compared with pure aluminum, the mechanical properties of the
GNPs/Al nanocomposites containing a low volume fraction of GNPs were sharply
improved. When 0.5 vol.%, 1.0 vol.%, and 2.0 vol.% GNPs were added to the
aluminum matrix, the average compressive strength of GNPs/Al nanocomposites
was 297, 345, and 527 MPa, respectively, which remarkably increased the strength
over the original aluminum by 330% to 586%.

1 Introduction 1,100 GPa, respectively. It has a large specific surface

Graphene, a monolayer of carbon atoms arranged
in a hexagonal lattice, is a promising material for
high-strength structure and electronic packing appli-
cations. This is due to its unique atomic microstructure,
high conductivity, high elastic modulus, low thermal
expansion coefficient, and high resistance to thermal
fatigue and creep [1–7]. For example, its thermal
conductivity is 5,000 W·m−1·K−1, 3 times that of diamond.
The strength and Young’s modulus are 125 GPa and
area of about 2,630 m2·g−1. It is also considered to be
an excellent nano-filler in composites for a wide range
of potential applications. Therefore, graphene is an
ideal reinforcement material for some composites.
To date, many studies have investigated polymer-
graphene composites [8–10], with only a few reports
on metal-graphene composites found in the literature
[11–12].
When graphene was added into an aluminum
matrix, it can significantly improve the mechanical

Address correspondence to ldsnuaa@nuaa.edu.cn

2 Nano Res.
and thermal properties of the resulting composites.
Graphene/Al nanocomposites possess outstanding
properties, including high specific strength, light
weight, low density, high thermal conductivity, and
high corrosion resistance. They have been widely
applied in the aerospace, automotive and other
engineering industries, and have been used as electronic
heat sinks. Recent studies have begun to focus on the
fabrication process of graphene/Al composites [13–17].
Bastwros et al. investigated semi-solid sintering
processing techniques to synthesize an aluminum
alloy composite reinforced by graphene [18]. Rashad
et al. applied graphene nanoplatelets to pure aluminum
using a semi-powder method and characterized the
resulting mechanical properties of the fabricated
material [19]. Yield strength and ultimate tensile
strength of Al/graphene composites, with an addition
of only 1.0 wt.% GNPs, increased by 17.7% over the
pure aluminum sample [20]. It was also observed
that higher hardness values of GNPs/aluminum
nanocomposites could be obtained with milling for
5 h, compared to the pure aluminum sample, with an
increase of about 138% [21].
However, problems including non-uniform density
distribution, agglomeration, interfacial reaction, and
complicated preparation processes have significantly
restricted the development of GNPs/Al nanocomposites.
In this paper, a two-step method for the preparation
of GNPs/Al nanocomposites was developed. In brief,
GNPs/Al composite powder was magnetically stirred
in an ethanol solution with ultrasonic dispersion, then
cryomilling was performed with the goal of obtaining
a uniform mixture of GNPs/Al composite powder.
Finally, GNPs/Al nanocomposites were fabricated
by both cold and vacuum hot pressing sintering.
The morphology and mechanical properties of the
nanocomposites were also characterized.
2 Experimental
Commercial 1060 pure spherical Al powder with
a purity of 99.96% and nominal diameter of 3 μm
(Shanghai Crystal Pure Biochemical Technologies Co.,
Ltd.), and GNPs (Nanjing Xian Feng Nano Material
Technology Co., Ltd.) were used as raw materials.
The average thickness of the GNPs was about 5 nm.
The GNPs were dispersed in anhydrous ethanol, and
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then ultrasonicated by a KQ32OOE apparatus for
60–90 min. Al powder and graphene with volume
fractions of 0.5%, 1.0%, and 2.0% were mixed in the
ethanol solution and subjected to ultrasonic oscillation
for 90–120 min, and then the mixed composite powder
was magnetically stirred for 30 min at 25 °C. After,
the mixture was placed in a vacuum drying oven at
100 °C for 180 min. The mixed composite powder was
continuously milled by a QM-BP type planetary ball
mill at 350 rev·min−1 for 150 min. The mass ratio of
the milling ball to mixed composite powder was 40:1.
The diameter of the balls were 6, 8, and 10 mm, with
a weight ratio of 1:1:1, and were applied to mill the
mixed composite powder with the goal of preparing
more uniformly distributed GNPs/Al nanocomposites.
The composite powder was prepared via cryomilling
at −5 °C under an argon atmosphere to eliminate the
agglomeration of GNPs. It was also able to prevent
oxidation and the segregation of the GNPs and
aluminum powder.
The composite powder was extruded into rod in a
graphite mold by a hydraulic press at 25 °C and 50 MPa.
A ZRYS-2000 vacuum hot pressing sintering furnace
was used to fabricate the GNPs/Al nanocomposites.
The sintering temperature was 580 °C for 4 h, with a
hot-pressing load of 0.77 t, and a vacuum of 10−2 Pa.
With subsequent cooling in the furnace, the GNPs/Al
nanocomposites were successfully fabricated.
The microstructure morphology, interface behavior,
phase, and mechanical properties of the aluminum
powder, GNPs, GNPs/Al composite powder, and the
final GNPs/Al nanocomposites were characterized by
field emission scanning electron microscopy (FESEM,
NOVA NANOSEM 450), high resolution transmission
electron microscopy (HRTEM, Tecnai G2-20), Raman
(LabRAM HR), X-ray diffraction (XRD, D8ADVANCE-
A25), and a CMT5105 microcomputer controlled
electronic universal testing machine (MTS).
3 Results and discussion
FESEM images of pristine spherical Al powder, GNPs,
and GNPs/Al nanocomposites powder are shown
in Fig. 1.
Figure 1(a) shows that the aluminum powder
presents an approximately spherical morphology, with
a particle size of 1–4 μm. The GNPs and GNPs/Al
Nano Res. 3

Figure 1 FESEM images (a) Al powder, (b) GNPs, (c) GNPs/Al nanocomposites powder.

composite powder are shown in Figs. 1(b) and 1(c),
respectively. Fig. 1(b) shows the two-dimensional
layered GNP microstructure with a 3–5 nm thickness
and a large specific surface area. It was found that
after magnetic stirring, ultrasonic dispersion, and
cryomilling, the GNPs possessed fewer layers and
were uniformly dispersed in the aluminum powder
matrix. The GNPs did not agglomerate, as can be seen
in Fig. 1(c), which is an important prerequisite to
fabricate high quality GNPs/Al nanocomposites.
Figure 2 shows the FESEM image and energy
dispersive X-ray spectroscopy (EDS) of the polished
and etched 0.5 vol.% and 1.0 vol.% GNPs/Al nano-
composites. Figure 2(a) shows that some GNPs were
present as flakes and were embedded in the 0.5 vol.%
GNPs/Al nanocomposite. It is clear that the GNPs
contour in GNPs/Al composite. The GNP flakes com-
bined well with the aluminum matrix, which indicated
good surface and interface behavior characteristics.
The EDS is shown in Fig. 2(b) and indicates the
presence of a carbonaceous component of the GNPs/Al
nanocomposites. It also confirmed the presence of
the GNPs on the Al. An FESEM images and EDS
of the 1.0 vol.% GNPs/Al nanocomposite are shown
in Figs. 2(c)–2(e). It can be seen in Fig. 2(c) that the
interface between Al and GNPs is compact with no

Figure 2 FESEM images and EDS of GNPs/Al nanocomposites. (a) FESEM of 0.5 vol.% GNPs/Al nanocomposite. (b) Point EDS point
of 0.5 vol.% GNPs/Al nanocomposite. (c) FESEM of 1.0 vol.% GNPs/Al, (d) and (e) Line EDS of 1.0 vol.% GNPs/Al nanocomposite.

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4 Nano Res.
detachment and clear microporous structure. Line EDS
of the 1.0 vol.% GNPs/Al nanocomposite is shown
in Figs. 2(d) and 2(e). A clear interface transition zone
from GNPs to Al matrix can be seen in Figs. 2(d)
and 2(e), according to the distribution of carbon
aluminum elements. This suggests that the GNPs/Al
nanocomposite exhibits good interface behavior. Deng
et al. found that nano-additives can inhibit grain
growth through grain boundary pinning [22], and
lead to a finer grain microstructure. Finer interface
behavior can produce greater strength and hardness.
It was also found that the two nanocomposites had a
fine microstructure, as shown in Fig. 2. The micro-
structure likely contributes to the excellent properties
of nanocomposites such as high hardness values.
Figure 3 shows the SEM image and EDS map of
the tensile fracture surfaces of the 2.0 vol.% GNPs/Al
nanocomposite. The tensile fracture morphology of
the GNPs/Al nanocomposites is shown in Fig. 3(a). It
was found that the fossa and tear ridges were regular
and uniform. The 2.0 vol.% GNPs/Al nanocomposite
presented ductile fracture distinguishing features,
which also showed a good combination between the
Al matrix and GNPs. It is uncertain whether GNPs
were pulled out from the aluminum matrix. The GNPs
were more easily observed in the marked rectangular
region of the GNPs/Al nanocomposites, as shown in
Fig. 3(a). Figures 3(b) and 3(c) show EDS maps of the
GNPs/Al nanocomposite. Figure 3(b) shows the GNP
distribution in the GNPs/Al composite. Figure 3(c)
shows the aluminum distribution in composite.
Figures 3(b) and 3(c) show that, in the same marked
Figure 3 SEM image and EDS map of tensile fracture surfaces of GNPs/Al nanocomposite, (a) tensile fracture SEM of GNPs/Al
nanocomposites, (b) carbon map, (c) Al map.
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region as in Fig. 3(a), the composite contains carbon,
whereas the other areas are mostly composed of
aluminum. The GNPs were uniformly dispersed in the
aluminum matrix. In GNPs/Al nanocomposite powder,
the process of cold pressing and vacuum hot pressing
sintering did not destroy or oxidize the GNPs. The
lamellar morphology of the GNPs randomly distributes
in the aluminum matrix. This distribution indicates
fine microstructure in the GNPs/Al nanocomposite
and excellent mechanical properties.
The Raman spectra of the GNPs, composite powders
and the 0.5 vol.% GNPs/Al nanocomposites are shown
in Fig. 4. Raman spectroscopy is a noninvasive and
effective technology to study the defects, crystallization,
and microstructure of carbon containing materials.
It is widely applied to characterize carbonaceous
materials such as diamond, graphite, graphene,
carbon nanotubes, and amorphous carbon. In Fig. 4(a)
characteristic D peak at 1,345 cm−1, G peak at 1,586 cm−1,
and 2D peak at 2,680 cm−1 can be observed. The ID/IG
and I2D/IG of the composite powders were found to be
0.61 and 0.52, respectively, and the ID/IG and I2D/IG of
the GNPs/Al composites were 0.66 and 0.48, respectively,
indicating that most of the GNPs in the composite
powder and the composite material consist of a few
layers. They did not change evidently as the ratios for
both materials were similar. The degree of disorder of
the GNPs after sintering was slightly increased. The
two materials had similar heights of the G peak at
1,586 cm−1. However, Fig. 4 also indicated that minor
differences in the 2D peak remained. It is well known
that a bilayer gives a much broader and up-shifted
Nano Res.
Figure 4 Raman spectrum of GNPs, composite powders and
GNPs/Al nanocomposite.
2D band with respect to graphene [23]. The G peak
arises from the doubly degenerate zone center E2g
mode [24]. The GNPs were sufficiently uniformly
dispersed and formed bilayers or monolayers. However,
the G-band was also quite different from bulk graphite.
The characteristic peaks of graphene oxide and
graphitized carbon were not found in Raman spectra.
This provides further evidence showing that the GNPs
were not oxidized, graphitized or agglomerated with
the novel two-step synthetic method. The GNPs were
successfully and homogeneously dispersed in the
aluminum matrix with the novel fabrication process
presented herein.
HRTEM images of the 0.5 vol.% and 2.0 vol.%
GNPs/Al nanocomposite are shown in Fig. 5. In the
0.5 vol.% GNP composite, some multi-layer GNPs were
embedded within the aluminum matrix, as shown in
Fig. 5(a). The interface between the graphene and the
aluminum matrix is dense. To further understand
the interface behavior between the graphene and
aluminum matrix, a section of Fig. 5(a) was amplified
and displayed in Fig. 5(b). It is clear from Fig. 5(b)
that the interface between the GNPs and aluminum
has no obvious impurities, voids, or other defects.
The GNPs and aluminum matrix nearly achieve
atomic-scale metallurgical combination, forming a
pure and high-strength interface. In addition, the
deleterious phase (Al4C3), which is generally prone to
chemical reaction, was not observed in the HRTEM.
Only good interface behavior was observed between
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5
the graphene and aluminum matrix. This indicates that
the composites form a pure interface for metallurgical
bonding through the novel two-step method, which
is crucial to fully exploit the excellent properties
of the GNPs/Al nanocomposites. Figure 5(b) also
indicated that the thickness of the GNPs between the
two aluminum grains is about 3–4 nm, the thickness
of 10 carbon atoms which would correspond to a
few layers of GNPs. HRTEM images of the 2.0 vol.%
GNPs/Al nanocomposite are shown in Fig. 5(c),
showing the uniform distribution of the GNPs and
their combination with aluminum in the GNPs/Al
nanocomposite. In the further magnified image shown
in Fig. 5(d), the microstructure of the GNPs/Al nano-
composites can be more clearly seen. Graphene nano-
platelets were also well dispersed in the aluminum
matrix. The uniform dispersion suggests the formation
of a favorable interfacial interaction between the
GNPs and the aluminum matrix. The microstructure
of the GNPs/Al nanocomposite is compact and dense,
and defects such as interface separation, microcracks,
voids, impurities, and graphene agglomeration were
not observed, as shown in Fig. 5(d). The GNPs/Al
nanocomposite presents a strong combination of
advantageous microstructural characteristics. These
results are in agreement with the interfacial behavior
observed in Fig. 2. The observed properties indicate
that the GNPs/Al nanocomposites will possess potential
advantageous mechanical and thermal properties.
XRD was used to analyze the microstructural
characteristics of the GNPs, aluminum, and 1.0 vol.%
and 2.0 vol.% GNPs/Al nanocomposites over a range
of 2θ of 5°–65°, as shown in Fig. 6. The characteristic
peaks of graphene at 2θ = 12° can be seen, while the
characteristic peaks of graphite did not appear at 2θ =
26.7°. This indicates that the graphene was hardly
graphitized, which is significant in the fabrication of
the GNPs/Al nanocomposites. The XRD patterns of
pure aluminum matrix and different volume fractions
of GNPs/Al nanocomposites have the same clear
and consistent 2θ peaks at 38°, 46°, and 65°, without
contribution from any other diffraction peaks. This
indicates that between the aluminum matrix and
reinforcement of the GNPs, the interfaces are clearly
identified and are free of impurities, which is similar
to metallurgical bonding at the atomic scale. The
Research
6 Nano Res.

Figure 5 HRTEM images of 0.5 vol.% and 2.0 vol.% GNPs/ Al nanocomposite. (a) Low magnification of 0.5 vol.% GNPs
nanocomposite. (b) High magnification of 0.5 vol.% GNPs nanocomposite. (c) Low magnification of 2.0 vol.% GNPs nanocomposite,
(d) high magnification of 2.0 vol.% GNPs/ nanocomposite.

the GNPs/Al nanocomposites. In addition, no oxide

Figure 6 XRD Patterns of GNPs, aluminum and GNPs/Al
nanocomposites.
XRD results also show that there is no obvious
characteristic peak of Al4C3 or Al2O3 in the prepared
composites. It should be emphasized that the harmful
intermediate phase, Al4C3, was not detected in any of
phase (Al2O3) was found in the GNPs/Al nanocom-
posites, which indicates that there was no chemical
reaction between the GNPs and the aluminum alloys.
This suggests that high quality GNPs/Al nanocomposites
were fabricated by the novel two-step method. The
two undesirable phases can become points of brittle
weakness, which lead to sharply decreased mechanical
and thermal properties. The GNPs likely adhere to
the surface and interface of the aluminum particles
during milling, and form a strong interface combination.
During consolidation, and subsequent heating and
extrusion, the GNPs did not react with the aluminum
on the grain boundaries, and the GNPs were not
oxidized.
The compressive stress-strain curves of the GNPs/Al
nanocomposites with different volume fractions of
GNPs are shown in Fig. 7. It can be seen that the
compressive strength of the GNPs/Al nanocomposites

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Nano Res.
Figure 7 Compression stress-strain curves of nanocomposites
with different volume fraction GNPs/Al.
increased with increasing graphene volume fraction.
Figure 7 shows that, compared with pure aluminum,
the compressive strength of the composites is greatly
improved. When 0.5 vol.%, 1.0 vol.% or 2.0 vol.% of
GNPs were added to the composite, the average
compressive strengths were 297, 345, and 527 MPa,
respectively, which is 330% to 586% higher than
the pure aluminum. The compressive strength of
the GNPs/Al composites is far greater than that of
the unreinforced Al matrix. Only a small amount
of GNPs (0.5 vol.%, 1.0 vol.%, 2.0 vol.%) were added
to the composites, but the enhancement ratio was
exceptional, higher than any other reinforcements
[25]. The compressive strength of the GNPs/Al com-
posites was significantly increased, which indicates
that incorporation of GNPs can be used a potential
reinforcement strategy. In addition, the GNPs/Al
nanocomposites also exhibited excellent tensile
mechanical properties [14]. Thus, GNPs have great
potential for the reinforcement of metal matrix
composites. However, it was also found that when
excess graphene was added to the composites, the
mechanical properties of the GNPs/Al nanocomposites
sharply dropped due to clustering of the GNPs [20].
The results of this study indicated that adding a
low volume fraction of GNPs significantly increased
the compressive strength of the composite. The
GNPs exhibit unique behavior that differs from the
enhancement of conventional particle reinforcement.
On the one hand, the GNPs and aluminum matrix
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7
formed a strong aluminum-GNPs bonding interface,
and, with increasing of GNPs volume fraction, more
graphene nanoplatelets were evenly distributed and
randomly embedded in the aluminum matrix. Under
external loads, dislocations in the composite bypassed
the large surface area two-dimensional structure GNPs,
which can be approximated as distinct dislocation
walls that require more energy to disturb. It is more
difficult to bypass the GNPs than to cut them, as they
act as particulate reinforcements. The slipping of
dislocations was hampered, effectively inhibiting
the plastic deformation of the matrix, which greatly
increased the compressive strength of the GNPs/Al
nanocomposite. The high strength properties of
graphene, such as tensile strength (125 GPa) and elastic
modulus (1,100 GPa), are much greater than the
aluminum matrix. Therefore, it plays a strengthening
role in the GNPs/Al nanocomposites. When the
GNPs/Al nanocomposites are compressed, the synergistic
interface behavior allows more load transfer from
the matrix to the GNP reinforcement. It also can
effectively reduce the facture deformation rate and
improve the mechanical properties of the GNPs/Al
composites. In addition, high thermal mismatch between
the aluminum matrix and graphene produced a
large number of dislocations, and it also indirectly
strengthened the performance of the composite material.
The GNPs/Al nanocomposites were prepared by a
simple two-step method and exhibited excellent
mechanical properties.
4 Conclusions
GNPs/Al nanocomposites containing 0.5 vol.%, 1.0 vol.%,
and 2.0 vol.% GNPs were successfully fabricated by
a novel two-step method. It was found that a low
volume fraction GNPs in the composite resulted in
better mechanical properties and microstructural
characteristics than pure aluminum. When 0.5 vol.%,
1.0 vol.%, and 2.0 vol.% GNPs were added to
the GNPs/Al nanocomposites, compared with the
unreinforced Al matrix, the average compressive
strength of the GNPs/Al nanocomposites surprisingly
increased 330% to 586% over the untreated matrix.
Efficient load transfer in the composites occurred
from the soft Al matrix to the high strength GNP
Research
8 Nano Res.
reinforcement due to the uniform GNP embedding
and buckling nature at the interfaces of the composite.
This indicated a compatible surface and interface
behavior between the Al and GNPs. Furthermore, the
deleterious phase, Al4C3, which is known to worsen
the mechanical properties of composites, was not
detected in the GNPs/Al nanocomposites. The results
presented above indicated that the GNPs/Al nano-
composites, being fabricated using two-step method,
possess fine microstructural characteristics and high-
performance mechanical properties.
Acknowledgements
This project was supported by the National Natural
Science Foundation of China (NSFC) (Nos. 51562027
and 11372100), and Jiangsu Key Laboratory of Precision
and Micro-Manufacturing Technology.
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