A Novel Route towards Sustainable Synthesis of Graphene
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Article
Volume 10, Issue 4, 2021, 2760 - 2765
https://doi.org/10.33263/LIANBS104.27602765
A Novel Route towards Sustainable Synthesis of Graphene
Rajib Biswas 1,* , Nishant Bharali 1 , Ashamoni Neog 1
1 Applied Optics and Photonics Laboratory, Department of Physics, Tezpur University, India
* Correspondence: rajib@tezu.ernet.in (R.B.);
Scopus Author ID 57202591766
Received: 10.02.2021; Revised: 12.04.2021; Accepted: 16.04.2021; Published: 8.05.2021
Abstract: Graphene is a wonder material having diverse, unique properties. It is used in many
applications spanning from optoelectronics to tailored semiconductor electronics. There exist many
routes of synthesis for this material. Amid them, exfoliation is generally preferred. In this report, an
unconventional route of exfoliation is executed. Here, graphene is exfoliated from the used mosquito
repellent rods, and correspondingly, its properties are studied. Accordingly, the attained yields are
characterized through Raman Spectroscopy and FTIR. It is observed a good match of the as-exfoliated
graphene with that of the pure sample. The reported synthesis results in a higher yield with immense
potential to be implemented in mass production by better controlling surfactants.
Keywords: graphene; exfoliation; repellant rods; FTIR.
© 2021 by the authors. This article is an open-access article distributed under the terms and conditions of the Creative
Commons Attribution (CC BY) license (https://creativecommons.org/licenses/by/4.0/).
1. Introduction
Graphene is considered a wonder material that has so far revolutionized the field of
material science. On the same note, graphene oxide is considered a prominent graphene
derivative that enables researchers to devise useful implementations. Thanks to their unique
chemical and physical properties. As catapulted by the immense use in several applications,
the growing demand for graphene forces researchers to explore innovative synthesis procedures
for graphene and its derivatives [1-8]. In general, graphene being a 2D crystalline allotrope of
carbon, possesses atoms having four bonds, namely, one σ (sigma) bond with each of the three
neighbors and one π (pi)bond, which is oriented out of the plane. As it contains only carbon
atoms, it shows less chemical activity. Nonetheless, it exhibits remarkable physical properties
[9-13]. The carbon atoms are bonded together in a hexagonal shape and are joined to another
hexagon. Such layers are joined to other layers above and below, giving us graphite, but these
layers are joined by weak Van der Waal forces and thus are easily exfoliated. The single layer
is so thin that it would take almost three million layers to make a 1mm thick layer of graphene.
There are many ways for the production of graphene, but not all are efficient.
Chemical vapor deposition is regarded as one of the potential methods of attaining high-
quality graphene. However, this turns out to be very expensive with the requirement of
controlled precursors. Alternately, the chemical method is one of the best appropriate methods
for the synthesis of graphene [14-19]. The colloidal suspension is produced in the chemical
method, which modifies graphene from graphite and graphite intercalation compound.
Likewise, chemical exfoliation is a two-step process. Initially, the interlayer van der Waals
forces are diminished to increase the interlayer spacing resulting in graphene intercalated
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compounds (GICs). It is then followed by exfoliation of graphene with a single to few layers
by rapid heating or sonication.
So far, the synthesis of graphene is concerned, abundant works of literature are dealing
with the various processes of synthesis [16-25]. It is noteworthy to mention that these proven
synthesis processes are not fully efficient. For instance, we can cite low yield as well as longer
execution time as some of the lacunae of these proven techniques. To address these issues, the
current work reports a novel route towards the synthesis of graphene. We adopt electrochemical
synthesis via a modified basic electrolyte medium through the utilization of used mosquito
repellent rods. The ECE technique [10-14] has been used in the present work as it is more
efficient than the chemical method and it entails less chemical consumption with high yield.
2. Materials and Methods
Sodium dodecylbenzene sulphonate, sodium dodecyl sulphonate, sodium chloride,
lithium chloride were purchased from Sigma Aldrich (USA). Used mosquito repellent rods
have been gathered from users. All glassware has been cleaned with aqua regia, followed by
thorough use of Millipore Water distill water.
2.1. Exfoliation of graphene.
First, the used mosquito repellent rods were cleaned by keeping them in 10% HCl
solution for 20 minutes and then boiled in distilled water at a temperature of 80°C for 20
minutes (Figure 1a); followed by exfoliation using Sodium Dodecyl Beneze
Sulphonate(SDBS) with a molarity of 0.02M. In the exfoliation process, the rod was immersed
in the SDBS solution and was connected to the power supply (Figure 1b). The whole setup was
then placed under sonication with the input voltage of 4V. The exfoliation was done for 4 hours.
The precipitate that was formed at the bottom was separated and extracted for characterization.
The problem with this batch was that the yield was very low. Thus exfoliation was next carried
in Sodium Dodecyl Sulphonate (SDS) by the same process. Here also, the same difficulty was
faced in the yield. Next, Sodium Chloride was used as the surfactant, and the process was
carried again but with a voltage of 9V. This gave us some amount of precipitate but was not
satisfactory. Thus, the surfactant was switched to Lithium Chloride, and the rods were placed
in the solution. The voltage was increased to 12V and was turned on for 6 hours. The molarity
was also increased to 0.04M. 10ml of buffer solution of ph 10 was added to the solution. The
final precipitate is shown in Figure 1c.
2.2. Extraction of the sample.
The extraction is one of the crucial factors for better characterization as well as purity
of the sample. As such, careful measures had to be taken. After the precipitate was formed, the
solution was put under centrifuge for 15minutes at 4000 RPM. As a result, the precipitate
settled at the bottom of the tube. The finer particles were afloat in the solution, so the solution
was further separated into smaller tubes leaving behind the precipitate in the bigger tubes. The
solution in the smaller tubes was again put to a centrifuge for another 15mintues at 4000 RPM.
The precipitate in the bigger tubes was again washed with distilled water to remove any
impurities present and again put under centrifuge at the same parameters. The same process
was done for the solutions in the smaller tubes also. The obtained precipitates from both tubes
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were then put in the oven at 66°C for 5hours to remove the liquid present. The powder formed
at the tubes was then scraped and put in 2 ml tubes.
2.3. Characterization.
Once we ensure the proper extraction of the sample, we proceed to perform certain
characterizations such as Raman Spectroscopy, Fourier Transform Infrared Spectroscopy
(RENISHAW, model no- Basis Series, 514 nm Ar+ laser line). Figure 1d shows the Raman
spectra of the sample via the SDBS route. Likewise, Figures 2a and b refer to the Raman
Spectroscopy and FTIR of the sample via the LiCl route.
3. Results and Discussion
The characterizations mentioned above turn out to be quite convincing so far the results
from other published results are concerned. As seen from Figure 1d, the sample yielded a giant
peak. As mentioned in the synthesis section, we did not obtain sufficient yield via SDBS as
SDS. We then switched to a basic medium by incorporating NaCl, which was eventually
followed by LiCl. However, the sample produced using NaCl and LiCl produced few flakes,
enough to undergo the tests.
(a) (b)
(c) (d)
Figure 1. Systematic way of production of graphene from the rods (a) mosquito repellant rods; (b) exfoliation
of rods; (c) prepared sample; (d) Raman spectra of SDBS sample.
Quite interestingly, the yield via LiCl was considerably better, which led us to take
these confirmatory characterizations. The obtained Raman Curve and FTIR spectra of the
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sample via LiCl was found to be in excellent conformity with Raman and FTIR spectra of the
pure sample [10-12, 15-20]. However, few portions in the spectra also implicate the existence
of graphene oxide. It is essential to mention here that the surfactant used plays an important
role. Likewise, the pH of the solution has to be considered before the process is initialized.
Further, before the rods are used as electrodes, one must remove all sorts of impurities.
(a) (b)
Figure 2. (a) Raman spectroscopy of the sample prepared using LiCl as a surfactant; (b) FTIR spectroscopy for
the sample prepared by LiCl.
4. Conclusions
In summary, we report a novel route for producing graphene via used mosquito
repellant rods. We used different surfactants, and our results showed promising yields in a basic
electrolyte medium. The one produced with LiCl as a surfactant gave Raman spectra sharp
peaks, but some inference could be drawn from it. The confirmatory tests through FTIR and
Raman provide a substantial match with already published results. Relatively, the proposed
synthesis route seems to be more prudent as compared to other published reports. Therefore, it
can pave a new way for the synthesis of other derivatives as well.
Funding
This research received no external funding.
Acknowledgments
There is no one to express acknowledgment.
Conflicts of Interest
There is no known competing interest with anyone.
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