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Materials Today: Proceedings 5 (2018) 27928–27935 www.materialstoday.com/proceedings

ICCMMEMS_2018

Dispersion of Graphene in Aluminum Powder to Aid Synthesis

of Homogenous Nano-Composites
Yoganand C.R.a, and Parvati Ramaswamyb*
a
MTech Scholar(Machine Design), b Professor
Department of Mechanical & Automobile Engineering, Faculty of Engineering, Christ (Deemed to be University) Bangalore-566074, India

Abstract

A fairly simple methodology to homogeneously disperse graphene in aluminum powder with potential for further use as
composites with superior performances is described. Graphene is indisputably the most superior additive in today’s engineering
materials world to perform as reinforcement to different metal matrices to form nano-composites with unusual properties.
Challenges arise from the need for uniform dispersion of graphene into metals without which the synthesis of high-performance
graphene-reinforced metal matrix composites are not possible. The processing steps involved dispersion of graphene in Ethanol
solution via ultrasonication, magnetic stirring, and addition of pure Aluminum powder (99%), followed by controlled
grinding/ball milling in methanol or by grinding in pestle and mortar to achieve the desired characteristics. The crystal structure
and microstructure of synthesized composite powders were examined via X-ray Diffracatrometry (XRD) and Energy Dispersive
X-ray Spectroscopy (EDS) associated with Scanning Electron Microscope (SEM). Results pertaining to homogenous dispersions
of graphene with varying concentrations of 0.5, 1 and 1.5% in aluminium powder, with potential to lead towards sintering via
powder metallurgy route has been studied and presented in this paper.

© 2018 Elsevier Ltd. All rights reserved.

Selection and Peer-review under responsibility of International Conference on Composite Materials: Manufacturing,
Experimental Techniques, Modeling and Simulation (ICCMMEMS-2018).

Keywords: Al-graphene composite; dispersion; ultrasonication; magnetic stirring, synthesis

* Corresponding author E-mail address: parvati.ramaswamy@christuniversity.in

2214-7853 © 2018 Elsevier Ltd. All rights reserved.

Selection and Peer-review under responsibility of International Conference on Composite Materials: Manufacturing, Experimental Techniques,
Modeling and Simulation (ICCMMEMS-2018).
 Yoganand C. R. / Materials Today: Proceedings 5 (2018) 27928–27935 27929

1.0 Introduction
Carbon is considered as a sensible prima for life and the source of all organic chemistry and the most versatile
chemical element in nature to support materials engineering. Since the discovery of carbon allotrope, ‘graphene’ by
Novoselov et al in 2004 [1], due to its sp2 - hybridized 2-D honeycomb structure, light weightiness, highly
favourable thermal, electrical and mechanical properties, it has fascinated researchers throughout the world. Truly,
graphene has a number of exceptional properties: strongest and stiffest material ever measured; the most stretchable
crystal and most thermally conductive material ever predictable to humans and this makes graphene extremely
suitable for highly sophisticated futuristic applications in the form of reinforcements to matrices to form composites.
The exact history of graphene and its appearance in technical prospect is attractive and being a main part of various
three– dimensional materials, graphene has been studied since the 1940s [2, 3]. Its outstanding properties are
discussed by several researchers: few recent ones being the efforts of Novoselov et al. [1, 4] and Zhang et al. etc. [5,
6].
1.1. Basics of Graphene
Graphene is only a monolayer of graphite. It is an allotrope of carbon consisting of strongly bound carbon atoms
structured in a two-dimensional hexagonal lattice. Sp2 hybridization and extremely thin atomic thickness (0.345 nm)
makes graphene a special material. It has a honeycomb arrangement with a carbon-carbon atomic length of 0.142
nm. These characteristics allow graphene to break up too many records in terms of strength, electricity, heat /
electric conduction, Also, graphene is widely known as "super carbon" due to its impressive properties within
smaller dimensions: one atomic thickness made of honeycomb lattice and revolutionary future material thus
considered Three-dimensional sheet of atoms. The single layer graphene has a Young's modulus of 1.0 TPa and a
tensile strength of 130 GPa. Graphene may absorb ten times the amount of energy of steel before failure [2].

With conductivity 1,000,000 times superior to copper, graphene conducts heat more than conducting silicon. Its
thermal conductivity being 3000-5000 W/mK in normal ambient, graphene is an inimitable character equated with
the thermal conductivity of pyrolytic graphite of around 2000 W·m-1·K-1 at room temperature. Due to the strong
nature of its 0.142 Nm-long carbon bonds, graphene is robust (≈ 2600 m2 g -1) and has a low density (2.2 g cm-3),
which makes it suitable for a reinforcement for nano-composites. The material ever exposed, with a vital tensile
strength of 130 gigapascals, matched to 4X108 for A36 organizational steel, or nearly 4X108 for Aramid (Kevlar).
while graphene astonishingly strong, it is also very light at 0.77 milligrams per square meter (for comparison
purposes, 1 sq meter of paper is approximately 103 times heavier). Trials have shown that graphene sheets (with
width between 2 and 8 Nm) have spring constants in the region of 1-5 N/m and a Young's modulus (different to that
of three-dimensional graphite) of 0.5 TPa [4].

As a word of caution: “Graphene” is frequently known as a clan containing (a) perfect graphene (G), (b) graphene
oxide (GO), and (c) reduced graphene oxide (RGO) and still there is no formal terminology for graphene and its
byproducts which is being practiced universally. Among the possible applications of graphene thermal management,
possibilities are in electronics, because graphene has the great ability to disperse heat and enhance its electronic
function. In micro and nano-electronics, heat is often a restrictive factor for tiny and more effective components.
Thus graphene/like materials with extraordinary thermal conductivity may have huge potential for such applications.
The superiority of thermal conductivity of graphene can be used in a number of ways, including thermal grease of
thermal material interface (TIM), heat spreader (E.g. thin layer between microprocessor and normal heat source as
heat sink), Nano-composite Graphene series, and many more. The advantage of using graphene as a reinforcing
material for metals and other matrices is very large [3]

1.2. The Challenges

Utilizing the excellent physical properties of the graphene is not without problems, often requires dispersion in an
aqueous or organic medium [6]. Dispersion must be attained with concentration and constancy suitable for intended
end use. Good interaction between graphene sheets is indicative of insufficient dispersion. From a manufacturing
standpoint, it is important to use a range of the dispersion media that contain less volatile and toxic solvents, e.g.
27930 Yoganand C.R./ Materials Today: Proceedings 5 (2018) 27928–27935

alcohol and water, promoting distribution firmness as a function of time, temperature and improved dispersion
stability as a function of ionic strength as well. In addition to these, there are issues such as accurate
characterization, safe handling, post-processing, and finally cost-effectiveness.

1.3 The Metal-Matrix composite

Aluminium is well known for its highly favourable characteristics as the matrix material in synthesis of metal-matrix
composites. This is due to the following characteristics of aluminium: light weight, corrosion resistance, high
electrical and thermal conductivity, ability for strengthening either via precipitation or by forming into composites,
highly recyclable metal and therefore environmental friendly. Hence, aluminum and its alloys find huge application
in research and highly specialized engineering industry applications which include electrical power lines, sporting
and marine goods, aero-space and household items. When used as matrix to form metal-matrix composites,
Aluminum Matrix Composites (AMCs) are usually reinforced with ceramics like Al2O3, SiC, SiO2 etc. and
significant amount of research information and published reports are available. Research and information on
composites by using graphene in aluminum is at its infancy and any information leading to improved understanding
on the use of graphene as reinforcement is welcome to the world of research involving Al and graphene composites.
1.4 Scope of the Present Investigation

This paper makes an attempt to address the issue of dispersing commercially available graphene flakes into
individual platelets before introduction to the commercially available aluminum powder prior to synthesis of nano-
composites.

2.0 Experimental Procedures

2.1 Materials and Processing Methodology

Commercially Aluminum powder (SD Fine Chem Ltd) and graphene (United NanoTech Innovations Pvt Ltd,
grade) were used as the starting materials. Prior to beginning the dispersion, the morphology of the as received
graphene flakes were analysed. The experimental details are given in the flow chart shown in Fig 1.

Characterization of Graphene and Aluminium powders (SEM and XRD)

Ultrasonication of graphene for homogeneous dispersion in Ethanol for 1 hour

Drying of Aluminum Graphene slurry

Addition of Aluminum powder to the ‘graphene in alcohol’ slurry: Magnetic stirring for 2 hours

Grinding / ball milling of dried Aluminum Graphene powder in methanol solution

Fig 1: (Al-graphene dispersed powder Synthesis: Flow Chart)

3.0 Results and Discussion

3.1 Graphene characteristics: The characteristics of the graphene used in this work (as provided by the
manufacturer) are given in Table 1.
 Yoganand C. R. / Materials Today: Proceedings 5 (2018) 27928–27935 27931

Table 1: Properties of Graphene (as provided by manufacturer)

Technical Grade
Sl.No. Properties
Graphene
United Nanotech
1 Manufacturer
Innovations Pvt Ltd
2 Bulk Density 0.35 g/cc
3 Oxygen <0.5%
4 Diameter X & Y dimensions <10 microns
5 Thickness average Z dimensions 5 – 10 nm
6 Product Purity >98%
7 Ash content <0.001%
8 Metallic Impurity <0.010%
9 Pore Size >0.15nm
10 PH <7
11 Number of Layers 10 – 15

3.2: Aluminium-Graphene composite Powder characteristics:

SEM Analysis: Figure 2 (a and b) shows the SEM micrograph of the aluminum powder (as-received) and Fig 3 (a
and b) of graphene powder (as-received), used in this study.

(a) (b)
Fig 2: SEM micrograph of aluminum Powder (as –received) : a @ 500X and (b) @ 1000X

(a) (b)
Fig 3: SEM micrograph of graphene Powder (as-received): a @ 10,000X and (b) @ 70,000X
27932 Yoganand C.R./ Materials Today: Proceedings 5 (2018) 27928–27935

Aluminum powder morphology comprised of elongated particles with large variation in length measuring between
2 and 100 µm and about 10 to 15 µm wide (Fig 2 a and b). The particle surfaces were featureless and exhibited a
fairly smooth non-faceted exterior.
In contrast, the graphene flakes were comprised of varying morphological manifestations. The individual graphene
flakes (most likely) were embedded over each other and likely measured between 3 and 10 microns (Fig 3 (a and b).
It was not possible to measure the thickness of the flakes accurately, although from the magnified image (Fig 3b) the
thickness appeared to be lower than 25nm.
Figure 4 shows the XRD pattern of the graphene (as received) powder.

Fig. 4: XRD pattern of Graphene (as received)

Well defined peaks of carbon, with out any additional peaks were the characteritics of graphene. In a similar manner
XRD pattern of aluminium powder (pattern not shown here) exhibited characteristic peaks pertaining to pure
aluminium powder.

After the dispersion process of graphene was completed in alcohol, SEM images of the dried powder (mounted on
conducting tape) revealed well separated graphene flakes as seen in Fig 5: a@33,000X and b @68,500 X)

a b
Fig 5: SEM micrograph of well dispered graphene Powder (as-received): a @ 33,000X and (b) @ 68,500X
 Yoganand C. R. / Materials Today: Proceedings 5 (2018) 27928–27935 27933

Dispersed graphene was mixed with aluminium powder during processing in alcohol, followed by grinding / ball
milling of dried Aluminum Graphene powder in methanol solution. The post processed and dried mixture was
analysed in the SEM. Detailed analysis revealed well dispersed graphene in aluminium powder. The compositions
that were processed and studied were 0.5, 1.0 and 1.5% graphene (weight percent) in aluminium powder.

Fig 6 shows the SEM micrographs of Al-graphene dispersed powder. The dispersion of graphene flakes was
possible to be inferred via microscopy at high (>50,000X) coupled with chemical analysis via EDS analysis.

The EDS pattern pertaining to the Al-graphene composite powder (Al-0.5%graphene) shown in Fig 7 revealed only
Al, C and O peaks: presence of O was most likely attributable to oxidation of aluminium powder on the surface.

a b
Fig 6: SEM micrograph of well dispered graphene (0.5 wt.%) in Aluminium powder: a @ 1,000X and (b) @ 33,000X

Fig 7: EDS pattern of Al-0.5% Graphene composite powder.

Fig 8 (a & b) shows the SEM image of Al -1.0% graphene composite powder and Al-1.5% graphene composite
powder (Fig 9) synthesized in the manner described in the previous section.
Yet again detailed EDS analysis revealed not just the presence of graphene (carbon) and aluminum, but well
distributed graphene flakes over aluminum particles. Closer study of the surface of Aluminium particles under SEM
revealed the presence of uniformly embedded carbon phase, most naturally graphene, because graphene was the
27934 Yoganand C.R./ Materials Today: Proceedings 5 (2018) 27928–27935

additive used to make the composite. Finer investigation was not possible with the limitations of the SEM
capabilities.

In the present work graphene compositions above 2% in Al powder has been studied because it is well published in
literature that attaining the positive collaboration between the mass fraction and positive effects of graphene is
substantial to the resulting performances [11]. Generally a maximum graphene content that is acceptable in
composites varies between 1 and 5%. Uniform distribution of graphene in aluminium powder was achieved as
observed via SEM-EDS studies.

(a) (b)
Fig 8: SEmicrograph of well dispered graphene (1.0 wt%) in Aluminium powder: a @ 1,000X and (b) @ 33,000X

Fig 9: SEM micrograph of well dispered graphene (1.5 wt%) in Aluminium powder: @50,000X
 Yoganand C. R. / Materials Today: Proceedings 5 (2018) 27928–27935 27935

4.0 Conclusions:

Well distributed Alumium - graphene powders were synthesized by simple laboratory technique comrpised of
carefully controlled processing conditions by employing ultrasonification, magnetic stirring, ball milling in alcohol
medium. Further work is required to undertsand the mechanism of adhesion of the graphene on aluminium powders
and the size of flakes that have become wedged or embedded onto the alumium powder surface. These powders are
now ready for further processing by following the powder metallurgical routes of compaction and sintering and
electrical and mechanical characterization. Work in this direction is in progress and will be reported in the future.

5.0 Acknowledgements

The authors gratefully acknowledge the Christ University Management headed by Vice Chancellor, Dr. (Fr.)
Thomas C Mathew, Engineering Director Dr. Fr. Benny Thomas, Associate Dean, Faculty of Engineering Dr. Iven
Jose and Mechanical Department HOD Dr. Gurumoorthy Hebbar, Associate Professor, for encouraging this R&D
work. Dr. Vijayasankar A V, Assistant Professor, Dr. Mothi Krishna Mohan, Assistant Professor and Prof. Nobi K
Daniel are specially thanked for providing the facilities to carry out the experiments.

6.0 References

[1] Novoselov KS, Geim AK, Morozov SV, Jiang D, Zhang Y, Dubonos SV, I.V. Grigorieva & A.A.Firsov et al.
Electric Field Effect in atomically Thin carbon films. Science 306, 666(2004).
[2] A. K. Geim and K. S. Novoselov, et al.” The rise of Graphene Nature Materials” 6, 183 – 191 (2007)
[3] P. R. Wallace,et al. “The Band Theory of Graphite” Physical Review, vol.71, No.9,1947,pp.622 – 634.
[4] K. S. Novoselov, D. Jiang, F. Schedin, T. J. Booth, V. V. Khotkevich, S. V. Morozov and A. K. Geim, et al.
“Two – dimensional atomic crystals”. 2005 Proc. Natl. Acad. Sci. U. S. A., 2005, 102(30) 10451 – 10453.
[5] Y. Zhang, Y.-W. Tan, H. L. Stormer and P. Kim et al.“Experimental observation of the quantum Hall effect and
Berry’s phase in Graphene” Nature, Vol. 438 no. 7065, pp. 201-204, 2005.
[6] B M Paramashivaiah and C R Rajashekhar et al.” Studies on effect of Various surfactants on stable dispersion of
Graphene Nano particles in simarouba biodiesel”. IOP conference series: Materials Science and Engineering
Volume 149, Issue 1, pp. 012083(2016).
[7] Nathan O Weiss, Hailong Zhou, Lei Liao, Yuan Liu, Shan Jiang, Yu Huang and Xiangfeng Duan et al.
“Graphene : An Emerging Electronic Material “Adv. Mater. 43/2012 page 5776.
[8] Patents - Processes for sintering Aluminum and Aluminum alloy components US 7517492 B2
[9] Patents - Method for reinforcing metal material by means of graphene, US 20170014908 A1
[10] Yuchi Fan, Lianjun Wang, Jianlin Li, Jiaqi Li , Shikuan Sun , Feng Chen , Lidong Chen , Wan Ji et al.
“Preparation and electrical properties of graphene nanosheet/Al2O3 composites “ CARBON 48 ( 2010 ) 1743 –1749
[11] Bo Tang, Haiqun Chen, Haoping Peng, Zhengwei Wang and Weiqiu Huang, Graphene Modified TiO2
Composite Photo catalysts: Mechanism, Progress and Perspective, Nanomaterials 2018, 8, 105; doi:10.3390/
nano8020105.