Materials Today: Proceedings xxx (xxxx) xxx

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Materials Today: Proceedings

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Study of Optical and Electrical Properties of Graphene Oxide

Neeraj Sharma a, Stuti Tomar b,c, Mohd. Shkir d, Ravi Kant Choubey c, Arun Singh a,⇑
a
Advanced Electronic and Nano-Materials Laboratory, Department of Physics, Jamia Millia Islamia (A Central University), New Delhi 110025, India
b
Applied Science & Humanities Department, ABES Engineering College, Campus -1, NH-24, Ghaziabad, UP 201009, India
c
Department of Applied Physics, Amity Institute of Applied Sciences (AIAS), Amity University, Noida Campus, Sector - 125, Noida 201313, Uttar Pradesh, India
d
Advanced Functional Materials and Optoelectronics Laboratory (AFMOL), Department of Physics, Faculty of Science, King Khalid University, Abha 61413, Saudi Arabia

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

Article history: Present work reports the Graphene oxide (GO) optical and electrical properties and its variation after gra-
Received 14 February 2020 phene oxide reduction. Modified Hummers’ method route is adopted for synthesis of present graphene
Received in revised form 25 April 2020 oxide (GO) material. Graphene oxide (GO) was reduced by voltage application in the GO solution. In volt-
Accepted 28 April 2020
age application process the Cu electrode was dipped in the GO solution with biasing of 10 V for 2 h. The
Available online xxxx
thin films of two materials graphene oxide (GO) and reduced graphene oxide (rGO) are deposited in
square shape using Masking tape by spin coating technique. The materials were characterized by X-
Keywords:
Ray Diffraction (XRD), Scanning electron microscopy (SEM) Raman spectroscopy and UV–Vis spec-
GO
rGO
troscopy. The XRD peak of GO raised at 10.4° and rGO at 25.9°. The SEM images show the sheet structure
XRD of GO and rGO. The Raman peak of GO and rGO show G peak at 1597 cm
1 , 1608 cm
1 and D peak at
Raman 1353 cm
1, 1347 cm
1 respectively. The ID/IG ratio of GO and rGO is 0.89 and 0.96, respectively. The peak
UV–Vis spectroscopy of GO and rGO UV–Vis absorbances is 230 nm and 270 nm, transmittance is 85% and 75%. respectively.
Bandgap The tauc plot gave the bandgap value of GO is 3.84 eV and rGO is 2.87 eV. The measurement of sheet resis-
tance using desktop bench multimeter of GO is 2MO/sq. and rGO is 1.5kO/sq. The calculation of Hacce figure
of merit for rGO as transparent electrode gives the value 3.75  10
5 O
1
.
Ó 2020 Elsevier Ltd. All rights reserved.
Selection and peer-review under responsibility of the scientific committee of the National Conference on
Advanced Functional Materials 2019

1. Introduction 2 s1, 2p1x 2p1y2p1z now, two carbon atoms form the p bond by shar-
ing of s, p orbital electrons and hence Graphene expresses the sp2
In term of quantity Carbon is one of the rich elements on the hybridization. In the process of oxidation the p electrons are in
earth and also well known, for the creation of different kind of allo- excited state and oxide functional groups are share this p electrons
tropes. Allotropes are those materials which has a same kind of from the graphene sheet and form the sp3 hybridization for gra-
chemical formula but different physical orientations or the struc- phene oxide material [2]. The free p electrons in the graphene
tures. Diamonds, fullerene, graphite are the naturally occurring sheet are responsible for such a high electrical conductivity of
allotropes of carbon. Here we shift our concern only towards the the graphene as these electrons confined in two dimension can tra-
graphite as it is one of the main precursors for the synthesis of gra- vel as fast as nearly speed of light and show relativistic quantum
phene oxide and reduction of graphene oxide can give the gra- effect that is why it is also known as Dirac fermions. Now, after oxi-
phene like structure. A graphene is a single layer of graphite. It is dation the hybridization changes from sp2 to sp3 that trapped these
one atom thick and has a hexagonal two-dimensional honeycomb free p electrons that results the drastically decreasing of electrical
structure. As the electronic configuration of ground state carbon conductivity in graphene oxide and makes it an insulator. The con-
atom is 1 s2, 2 s2, 2p1x 2p1y and vacant 2pz [1]. At the span of ductivity can revive after the functional groups’ elimination from
hybridization 2 s orbital electron excited to 2pz orbital and elec- graphene oxide. The graphene obtained after reduction of gra-
tronic configuration of carbon atom for transient time is 1 s2, phene oxide known as sheet reduced graphene oxide (rGO) or
chemically derived graphene oxide (CDG) [3]. The functional
groups are still existing in very negligible amount at the edges or
⇑ Corresponding author.
in the basal planes of the graphene sheet in reduced graphene
E-mail addresses: [email protected], [email protected],
[email protected] (A. Singh).
oxide (rGO) or chemically derived graphene oxide (CDG) therefore,

https://doi.org/10.1016/j.matpr.2020.04.861
2214-7853/Ó 2020 Elsevier Ltd. All rights reserved.
Selection and peer-review under responsibility of the scientific committee of the National Conference on Advanced Functional Materials 2019

Please cite this article as: N. Sharma, S. Tomar, M. Shkir et al., Study of Optical and Electrical Properties of Graphene Oxide, Materials Today: Proceedings,
https://doi.org/10.1016/j.matpr.2020.04.861
2 N. Sharma et al. / Materials Today: Proceedings xxx (xxxx) xxx

mention terms are used for these materials instead of pure gra- the addition of KMnO4 to solution as it was the exothermic reaction
phene. One of the vital strengths of functional groups presence in and explosion may be occurred, to avoid this situation the solution
the graphene oxide is that its variation in the material can tune was stirrer at the ice bath and KMnO4 was poured steadily [15].
the electrical, mechanical, thermal, physical and other properties The graphite to graphene oxide transition is demonstrated in Fig. 1.
[4]. It is very interesting that same material can cover the range
from conductor to semiconductor and then to insulator on the 2.2. Reduction of graphene oxide
account of oxidation variation [5]. This tuning property of gra-
phene oxide makes it a good candidate for its wide range of appli- Presently the ecofriendly reduction processes are emphasis for
cation. The fully oxidized graphene oxide shows the insulating the reduction of graphene oxide (GO). In the obligation of this, volt-
behavior and reduction results the removal of functional groups age application reduction process has been adopted for present
that makes the material semiconductor and somehow if functional case graphene oxide (GO) reduction. In this process two Cu elec-
groups removed nearly to zero the material shows the excellent trodes are dipped in the graphene oxide solution under the biasing
conductivity. The dispersion relation of graphene, means the rela- voltage of 10 V for 2 h. The reduction processes exfoliated the func-
tion between Energy (E) and momentum (K) shows the linear rela- tional groups from the graphene oxide basal plane. The result of
tion in low energy region however in case of conductor the reduction can be perceived by the changing in the colour of gra-
dispersion relation between E and K is parabolic. This linear rela- phene oxide from brown to blackish yellow colour solution. In con-
tionship is arising as a consequence of 2D hexagon brillouin zone tinuation of this the reduced in the resistance of graphene oxide
experiences the zero effective mass of electron and holes due to from 2MX to 1.5kX, as measured from desktop bench multimeter
Dirac fermions [6]. In the Dirac fermions case, the point where is consequence of the removal of functional groups from graphene
valance band and conduction bands are meet known as Dirac oxide indicates the reduction. The obtained materials GO and rGO,
points. Now, a graphene like structure can be obtained by reduc- were deposited on glass substrate that were got the heat treatment
tion of graphene oxide therefore, the research in the field GO at 120 °C Fig. 1.
increases considerably in recent past years. There are subsequently
many procedures, methods, paths and technique of GO reduction.
Few of the examples are mechanical exfoliation, chemical exfolia- 3. Result and discussion
tion, electrochemical reduction, biological agents reduction and
other effective methods [7–9]. In present work voltage application 3.1. Characterization techniques
is used to reduce the graphene oxide solution as it is one of the eco-
nomic and environmental-friendly method [10]. As it is previously Each material has unique properties, phases, individuality,
discussed that the tuning of oxidation increases the potential absorbance, transmittance, bandgap and other, chemicals physical
application of graphene oxide and reduced graphene oxide, the qualities that make materials distinguishable to each other. Char-
possible area of applications are supercapacitor, different sensors, acterization techniques exploited the distinctiveness property of
different power storage devises, optoelectronics application, trans- the materials and can assist to identify the materials. In present
parent electrodes etc. [11–14]. Here our work concern is over opti- work, the characterization techniques are used X-Ray Diffraction
cal and electrical properties of graphene oxide. Therefore, we are (XRD), Raman Spectroscopy, UV–Vis spectroscopy and for mor-
more concern to study the changes that occur in absorbance, trans- phology SEM analysis was performed.
mittance, bandgap and resistance before and after reduction of gra-
phene oxide (GO). In other words, present works supports the 3.1.1. X-ray diffraction (XRD)
reduced graphene oxide as transparent electrode. X-Ray Diffraction (XRD) technique can perform only either on
powder formed or on thin film crystal sample. Now, crystal can
be categorized either ordered long range crystal (true crystal) or
2. Experimental short-range crystal (pseudo crystal or amorphous crystal). The true
crystal samples show the sharp narrower XRD peaks corresponds
2.1. Synthesis of graphene oxide (Modified Hummers’ Method) to different phases present in the sample. Whereas in the case of
amorphous crystal XRD peaks are hump and wider in shape. The
The laboratory prevalent process Modified Hummers’ method graphene oxide (GO) are arranged in AB stacking format and stack-
was use to synthesis the graphene oxide. The precursors required ing height changes on the account of oxidation variation. Conse-
for this technique are graphite powder, sodium nitrate (NaNO3), sul- quently, GO XRD peak corresponds to (0 0 1) plane lies in
furic acid (H2SO4), Hydrogen peroxide (H2O2), Distilled water and between 7° to 12° [16]. After reduction of graphene oxide, the
additional accessories required are ice bath, beakers, magnetic stir- (0 0 1) peak diminishes and new peak is arising corresponds to
rer with thermometer, weighing machine. At first take the ice bath (0 0 2) plane in reduced graphene oxide. As graphite exhibit the
and fill it with ice to provide the cold environment below 20 °C to peak at 26° corresponding to (0 0 2) plane and graphene is the sin-
the solution. the mixture of graphite powder and sodium nitrate gle layer of graphite subsequently the peak is shifted from (0 0 1)
(NaNO3) 1.5 g each were dissolved in the 50 mL con. Sulfuric acid to (0 0 2) as transition from graphene oxide (GO) to reduced gra-
(H2SO4) and stirrer the mixture solute and sulfuric acid solvent on phene oxide (rGO). Present work graphene oxide (GO) and reduced
the magnetic stirrer at 600 rpm. After 1½ hrs. (one and a half hours) graphene oxide (rGO) raised up the XRD peak at 10.4°, 25.9°,
of stirring, 3g potassium permanganate (KMnO4) was steadily added respectively. The peaks of materials are shown in Fig. 2. Using
to the solution. Stirrer the solution for next 15 min and then take out the Scherrer formula one can estimate the crystallite size of the
from the ice bath. Now, solution was stirred for 4 h at 35 °C with graphene oxide (GO) and reduced graphene
room temperature environment that rigorously oxidized the gra- oxide (rGO). Eq. (1) represents the Scherrer formula [17].
phite powder. After 4 h the 50 mL distilled water was poured into
Kk
the beaker and further stirred for 15 min at 98 °C. The 75 mL distilled s¼ ð1Þ
bcosh
water was additionally poured to bring the solution temperature
down to room temperature and stirred for further 30 min. The reac- Here, the average size is ‘s’ (Å), Shape factor is K ,0.93 for spher-
tion was ended with the pouring of 1.5 mL hydrogen peroxide ical shape materials. Full Width at Half Maximum is b and the
(H2O2) in the final solution. Attention should be taken place during angle of x-ray diffraction is h. The wavelength k of Cu ka line

Please cite this article as: N. Sharma, S. Tomar, M. Shkir et al., Study of Optical and Electrical Properties of Graphene Oxide, Materials Today: Proceedings,
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 N. Sharma et al. / Materials Today: Proceedings xxx (xxxx) xxx 3

the principle of inelastic scattering. The accumulation and removal

of functional groups in the material substantially change the vibra-
tion mode of material on the account of which functional groups
variation can be recognized. The fundamental graphitic peak
known as G peak is arises in all materials that have a hexagonal
graphitic structure i.e. CNT, Graphite, fullerene, graphene, gra-
phene oxide and its derivatives due to graphitic ring vibration.
The attachment of functional groups in graphene structure arises
the imperfection and impurity in the hexagonal structure sources
the D peak. The functional group generally vibrate perpendicular
to the graphitic sheet and its own natural mode. The G peak of
GO is observed at 1597 cm
1 and D peak at 1353 cm
1. The G peak
of rGO is observed at 1608 cm
1 and D peak at 1347 cm
1 [18].
There is shift observed in the graphene oxide G peak after reduc-
tion from 1597 cm
1 to 1608 cm
1. This may due to the removal
of functional group restore the structure of graphene hexagonal
sheet from sp3 hybridization to sp2 hybridization. The shift is also
observed for D peak from 1353 cm
1 to 1347 cm
1 as the attach-
ments of functional groups generally create the imperfection in
the sheet structure but in the process of removal of functional
group the torn of sheet and also some location change from hexag-
onal to pentagonal that can result the shift in D peak of graphene
oxide after reduction. Besides these two major peaks, other peaks
due to first, second and third overtone is also arising, 2D at
2696 cm
1, D + G at 2946 cm
1 and 2D’ at 3197 cm
1. The intensity
of these overtones is not expressively visible in case of graphene
oxide (GO) but after reduction in case of reduced graphene oxide
(rGO) these peaks are significantly increasing and visible. The qual-
ity of the graphene oxide (GO) and reduced graphene oxide (rGO)
can be determined by the intensity ratio of D peak (ID) and G peak
(IG), lesser is the ratio lesser would be the imperfection and impu-
Fig. 1. Graphite to graphene oxide and reduced graphene oxide conversion. rity in the material. The calculated value of ID/IG ratio of graphene
oxide is 0.89 and after reduction in the case of rGO it is increased to
source is = 1.5406 Å. The XRD peak of GO and rGO are in 2 h degree 0.96. The Raman spectroscopy of graphene oxide (GO) and reduced
and half of the 2 h gives the value of h. Therefore, h for GO is 5.2° graphene oxide(rGO) is shown in Fig. 3.
and for rGO is 12.85°, putting these values of h with other required
parameters in Eq. (1) gave the crystallite size of GO, 16.48 nm and 3.1.3. UV–Vis spectroscopy
rGO, 6.47 nm. The SEM images of GO and rGO is also incorporated The basic optical properties such as transmittance, absorbance,
in Fig. 2 inset. These images show the sheet like structure of GO reflectance can be studied using UV–Vis Spectroscopy. In the pro-
and rGO. The GO SEM is more stretched and flatter whereas rGO cesses of UV–Vis spectroscopy a range from Ultra-violet to visible
SEM is rolled and folded. The folding of sheet may happen due to light is projected to the sample and response of transmittance,
weak Van der Waals force was experienced by the edges of the absorbance, reflectance is observed. The sample either in solution
reduced graphene oxide sheet. or thin film can be observed in UV–Vis spectroscopy analysis.
The absorbance peak dominated in the graphene oxide is due to
3.1.2. Raman spectroscopy p to p* transition. The shoulder is also present in graphene oxide
Raman spectroscopy determines the material by virtue of char- due to n to p* transition. Occasionally the shoulder is effortlessly
acteristic material vibrational modes. It fundamentally works on noticeable and sometime it is hard to even recognize it. In present

Fig. 2. XRD with inset SEM of (a) GO and (b) rGO.

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4 N. Sharma et al. / Materials Today: Proceedings xxx (xxxx) xxx

Fig. 3. Raman spectroscopy of GO and rGO. Fig. 5. Transmittance spectroscopy of GO and rGO.

Fig. 4. Absorption spectroscopy of GO and rGO.

Fig. 6. Bandgap of GO and rGO from tauc plot along with GO and rGO thin films.

work the graphene oxide (GO) peak has been observed at 230 nm
drawn between (ahm) and Energy (hm)n. a is known as absorbance
and shoulder at 300 nm [19]. The dominated peak due to p to p*
coefficient, h is Planck constant, m is the frequency of incident light.
transition is shifted to 270 nm in reduced graphene oxide (rGO).
The order parameter n is material dependent and its value is ½ for
The absorbance of graphene oxide (GO) and reduced graphene
direct bandgap materials and 2 for indirect bandgap materials. The
oxide (rGO) is shown in Fig. 4. once one knows the absorbance
estimation of bandgap using tauc plot is done by extrapolation of
spectroscopy, there is the conversion formula by which one can
linear portion in the graph corresponds to the energy of wave-
obtain the transmittance spectroscopy. The Eqs. (2) to (4) covers
length nearly to the absorbance peak. The value of bandgap is
the conversion formula between absorbance (A) to transmittance
the value of energy at which extrapolated linear line hits the x-
(T) [20].
axis (energy) for the value of y-axis (coefficient) is zero. In other
A ¼ 2
log10 T% ð2Þ words, bandgap is extrapolated line x-intercept value. There is
relation between energy and wavelength. In Eq. (5), The conversion
log10 T% ¼ 2
A ð3Þ formula between energy (E) and wavelength (k) in shown [1].

T% ¼ eð2
AÞ ð4Þ hc
E ¼ hm ¼ ð5Þ
k
Here, Absorbance (A) is in absolute number and Transmittance
(T) is in percentage. The obtained transmittance of graphene oxide here, Planck’s constant is h, the speed of light is c, the frequency is m
(GO) and reduced graphene oxide (rGO) from conversion formula is and the wavelength of the incident light is k. The tauc plot result as
shown in Fig. 5. The Fig. 5. graph shows that the GO transmittance shown in Fig. 6. gives the information of bandgap value of GO is
approached the 85% and rGO transmittance approached to 75%. 3.84 eV and rGO is 2.87 eV. The images of GO and rGO thin films
Using absorbance spectroscopy, the bandgap of material can also deposited on a glass substrate heated at 120 °C is also incorporated
be estimated by tauc plot relation. Basically, tauc plot is the graph in the Fig. 6.

Please cite this article as: N. Sharma, S. Tomar, M. Shkir et al., Study of Optical and Electrical Properties of Graphene Oxide, Materials Today: Proceedings,
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Table 1
The observed value of XRD, Raman, absorbance, transmittance, resistance and U of GO and rGO.

Material XRD Raman (cm-1) Absorbance Peak Transmittance Bandgap Sheet Resistance U
(2h degree) (nm) (%) (eV) (O-1)
D G
GO 10.4o 1353 1597 230 85 3.84 2MO/sq 9.84  10
8
rGO 25.9o 1347 1608 270 75 2.87 1.5kO/sq 3.75  10
5

3.2. Resistance measurement CRediT authorship contribution statement

The present work concern is over optical and electrical property Arun Singh was supervised the work, Funding acquisition,
of graphene oxide. The last section discussed the optical property Investigation, Methodology, Project administration, Resources.
of graphene oxide and its variation after reduction. Now, we are Neeraj Sharma was Conceptualized and performed the experiment,
interested to know about the electrical property variation in term formal analysis, take the Primary measurements and Data curation.
of resistance in graphene oxide and after its reduction. For the Neeraj Sharma, Stuti Tomar processed the experimental data,
resistance measurement purpose, the desktop bench multimeter drafted the manuscript and designed the figures. Mohd. Shkir, Ravi
VC8245 model was used. The measured value of resistance of Kant Choubey and Arun Singh were discussed on data analysis,
square shape GO thin films was nearly 2MX whereas for rGO it software, Validation and Visualization. Neeraj Sharma and Arun
was 1.5 kX. Undoubtedly, after reduction the resistance of gra- Singh aided in interpreting the results and worked on the manu-
phene oxide is decreased from 2MX to 1.5 kX. This indicated the script Writing - original draft. Authors thoroughly, discussed the
removal of functional groups and restoration of sp2 bond from results, commented on the manuscript and aided the significant
sp3 hybridization. Now, the square shaped thin film resistance is revision of scientific phenomenon and substantial modification
independent of its shape and equal to the sheet resistance of mate- on manuscript improvement and Writing - review & editing.
rial. Therefore, we can term, GO sheet resistance is 2MX/sq and
rGO sheet resistance is 1.5 kX/sq. Now, the value of transmittance
and sheet resistance are known. Therefore, Haccke figure of merit Declaration of Competing Interest
(U) can be calculated for transparent conductive thin film using
following Eq. (6) [21] The authors declare that they have no known competing finan-
cial interests or personal relationships that could have appeared
T 10 to influence the work reported in this paper.
/¼ ð6Þ
Rs
Here, the average visible transmittance is T and the sheet resis- Acknowledgements
tance is Rs. For reduced graphene oxide (rGO) using the transmit-
tance (T) 75% and sheet resistance (Rs), 1.5kO/sq., the Haccke The authors are grateful to the Department of Science and Tech-
figure of merit, U is calculated 3.75  10
5 O
1. The results of GO nology (DST), University Grants Commission and, Government of
and rGO all characterization XRD, Raman, Absorbance, Transmit- India, for financial assistance. The author (AS) would like to express
tance and parameters Resistance, figure of merit (U) is listed in sincere thanks to DST for the award of Young Scientist and BOY-
the Table 1. SCAST Fellowship. The author (NS) is thankful to Council of Scien-
tific & Industrial Research (CSIR), India for Junior research
fellowship.
4. Conclusion

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Please cite this article as: N. Sharma, S. Tomar, M. Shkir et al., Study of Optical and Electrical Properties of Graphene Oxide, Materials Today: Proceedings,
https://doi.org/10.1016/j.matpr.2020.04.861