1086 Indones. J. Chem.

, 2021, 21 (5), 1086 - 1096

The Influence of Permanganate Enhancement to Graphite on Chemical Structure

and Properties of Graphene Oxide Material Generated by Improved Tour Method

Dyah Ayu Fatmawati1*, Triyono Triyono1**, Wega Trisunaryanti1***, Haryo Satriya Oktaviano2,3,
and Uswatul Chasanah1
1
Department of Chemistry, Faculty of Mathematics and Natural Sciences, Universitas Gadjah Mada,
Sekip Utara, 55281 Yogyakarta, Indonesia
2
Department of Chemistry, Faculty of Science and Computer, Universitas Pertamina,
Simprug, Kebayoran Lama, Jakarta Selatan, DKI Jakarta, 12220, Indonesia
3
Research & Technology Center, PT. Pertamina (Persero), Sopo Del Tower A, Floor 51,
Jl. Mega Kuningan Barat III, Kawasan Mega Kuningan, Jakarta Selatan, DKI Jakarta, 12950, Indonesia

* Corresponding author: Abstract: Synthesis of graphene oxide (GO) material with variations in
permanganate/graphite ratio has been carried out. This research purposes to study
email: [email protected]*;
the impact of increasing oxidizing agents to graphite on the chemical structure and
[email protected]**; [email protected]***
properties of the GO material produced. All GOs were synthesized using the
Received: June 30, 2020 improved Tour method with three variations of permanganate/graphite ratios of 5,
Accepted: November 15, 2020 6, and 7. The results obtained include GO-5, GO-6, and GO-7, respectively, having
DOI: 10.22146/ijc.57423 a d spacing value of 0.843; 0.891; 0.894 nm by XRD analysis and 0.768; 0.756; 0.772
nm by SAED analysis. Based on the FTIR data, all GO materials bring up the peaks
of oxygen-functionalized carbon absorption such as O–H, C–H sp3, C=O, C–O–C
of ether and ester, and C-OH for carboxylic acids and alcohols. The oxidation levels
(O/C ratio taken from EDX data) of GO-5, GO-6, and GO-7 are 0.67, 0.88, and
1.50, respectively. SEM images display the appearance of an exfoliated layer with a
wrinkled and irregular surface. TEM images show thin and transparent layers. The
main peaks with the highest absorbance at the wavelength around 230-240 nm,
meanwhile the band gap energy produced was 3.53; 3.71; 3.55 eV for GO-5, GO-6,
and GO-7, respectively.

Keywords: chemical properties; chemical structure; graphene oxide; improved

tour method; permanganate/graphite ratio

■ INTRODUCTION modulus of 1 TPa and ultimate strength of 130 GPa,

single-layer graphene is the most robust material ever
Graphene is a carbon derivative containing a thin
investigated [2]. These distinctive qualities of graphene
layer of sp2 hybridized carbon atoms in a honeycomb
could bring out great implementations as batteries [3],
crystal grid [1]. Graphene displays superior electronic and
sensors [4], electrochemical supercapacitors [5],
mechanical characters as well as the electrical
electrocatalysis [6], polymer solar cells [7], etc.
conductivity of up to 6000 S cm–1, the thermal
Some methods have been declared for the synthesis
conductivity of 5000 W m–1 K–1, charge-carrier mobility
of graphene that can be principally divided into two
of 250000 cm2 V–1 s–1 at ambient temperature, and a broad
diverse ways: the bottom-up [8] and top-down [9] ways.
theoretical specific surface area of 2630 m2 g–1. Moreover,
The bottom-up growth of graphene layers is an option
graphene is exceptionally translucent, with the absorption
for the mechanical exfoliation of bulk graphite. In
of < 2.3% against visible light and even, with Young's
bottom-up processes, graphene is prepared by a type of

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methods like chemical vapor deposition (CVD) and and co-workers have noticed cracks in GO that were
epitaxial growth on SiC. Both of them regularly generate immediately concerned with the oxidation process. In
big-sized, lack free graphene in a small amount particular, a few variations in the level of oxidation can
appropriate for basic research and electronic lead to significant modifications in the structure and
performances. They are over interesting than the nature of the materials [16]. Hence, in the current work,
mechanical cleavage method [10]. Nevertheless, these and we will investigate the influence of adding
other methods called before are not compatible with the permanganates as oxidants on the structure and
synthesis of graphene required to prepare graphene-based properties of GO produced by the improved Tour
nanocomposites that generally need significant quantities method.
of graphene layers worthy of a functionalized surface
■ EXPERIMENTAL SECTION
formation. Accordingly, for the fabricating of graphene-
based nanocomposites, which mostly involves bulk Materials
amounts of homogeneously disparted graphene layers, All materials utilized in this experiment were from
the top-down way (i.e.) chemical and, or thermal commercial sources (E-Merck Germany) and were
reduction of graphite derivatives such as graphite oxide implemented without the subsequent purification.
(GO) emerges to be the supremely convenient and Materials used involved graphite powder, potassium
expeditious device [2]. permanganate (KMnO4, p.a.), sulfuric acid (H2SO4 98%,
GO is a precursor for graphene synthesis, which is p.a.), ortho-phosphoric acid (H3PO4 85%, p.a.),
oxygen loaded carbonaceous layered material highly hydrogen peroxide (H2O2 30%, p.a.), hydrochloric acid
identical to graphite [11]. However, graphite composes (HCl 37%, p.a.), absolute ethanol (p.a.), silver nitrate
simply sp2 hybridized carbon atoms, while GO includes (p.a.), and barium chloride (p.a.). For washing the GO
both sp3 and sp2 hybridized carbon atoms. The sp3 solution, deionized (DI) water, phosphate-buffered
hybridized carbon atoms in GO are covalently bonded saline (PBS), and bi-distilled water were utilized.
with oxygen functional groups as well as carboxyl, epoxy,
Instrumentation
hydroxyl, etc. [12]. In graphite, two-dimensional layers
are organized with each other under weak van der Waals X-Ray Diffraction (XRD, Bruker D2 Phaser) at a
interactions [13]. Nevertheless, whether of GO, the layers wide angle of 5–90° was used to determine the
are detached by epoxy and water molecules amongst the crystallinity of the materials. The functional groups of
layers. Consequently, the interlayer spacing of GO is the materials were characterized by Fourier Transform
much wider contrasted to graphite [14]. Infra-Red Spectrometer (FTIR, Shimadzu Prestige 21) at
GO has been notably resulted by several differences 4000–400 cm–1. The structure and polycrystalline ring
of Brodie, Staudenmaier, and Hummers methods that images of the materials were taken using a Transmission
implicate the oxidation of graphite in the attendance of Electron Microscope-Selected Area Electron Diffraction
strong acids (nitric acid or sulfuric acid) and an oxidizing (TEM-SAED, JEOL JEM-1400). The surface
agent (KMnO4, KClO3, NaNO3). Many different slightly morphology and metal content of the materials were
modified and improved versions have also been evaluated by Scanning Electron Microscope-Energy
expanded, including the Tour method [15]. Notably, it Dispersive X-ray (SEM-EDX, JSM-6510LA). The
has been established that the structure and properties of wavelength absorption of the materials was observed
GO, especially turn on three parameters: the typical using UV-Visible Spectrophotometer (UV-Vis, UV-
synthesis methods, the level of oxidation, and the raw 1800 Shimadzu) at a wavelength of 200–800 nm.
material of graphite utilized. Procedure
In this section, throughout their work on the
Our method was taken from Ranjan and co-
influence of oxidation on the morphology of GO, Lojka
workers [17] with a few modifications. In the beginning,

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1088 Indones. J. Chem., 2021, 21 (5), 1086 - 1096

potassium permanganate to graphite powder in various and a very weak peak at 2θ = 42.327° originated from the
ratios of 5, 6, 7 were combined and mashed up hkl plane of 100. This corresponds to graphite standards
homogeneously. The mixture was placed into Beaker A, on ICDD (International Centre for Diffraction Data) of
and the mixture of sulfuric acid and ortho-phosphoric 01-075-1621. The peak of plane 002 indicates the
acid in a ratio of 9 was put into Beaker B. The two beakers aromatic conjugated-carbon bond [18] with layered
were kept at a temperature below 5 °C for 6 h. The structures. Due to this nature, the presence of plane 002
solution in beaker B was then poured into beaker A and is used widely to monitor the conversion of graphite into
stirred until the solution was greenish-black, later heated GO material. From Fig. 1, it can be seen that when
at 65 °C for 24 h. After the heating time was finished, the graphite is oxidized using a sufficient amount of
color of the solution became brownish, the beaker left permanganate, the principal peak at ~26° will shift to a
until it reached room temperature. The solution was smaller 2θ of around 9–10°. XRD data interpretation has
poured into another beaker containing 500 g of deionized been compiled in Table 1. By using the Bragg equation
water ice, added with 7 mL of hydrogen peroxide, and (Eq. (1)), we could see that the interlayer spacing (d)
stirred using a stirring rod. Instantly, the color of the between the graphene layer significantly changed from
solution became golden yellow, marking the formation of 0.34 nm in graphite to 0.8–0.9 nm in GO. Such a
GO. The solution was left to precipitate the solids GO. GO difference is caused by the presence of oxygen-
was washed by centrifugation at 5000 rpm for 5 min using containing groups in GO material [19-20]. The
a solution of hydrochloric acid (2 times), ethanol absolute introduction of oxygen functional groups between the
(3 times), and phosphate-buffered saline (PBS) until the graphene layer of GO will increase the d-spacing.
pH of the solution became 7. PBS was used to make the =nλ 2dsin θ (1)
washing process more efficient, so it did not need a lot of
bi-distilled water. The solution was then checked for
chloride ions content using silver nitrate and barium
chloride for sulfate ions content. The washing process
using bi-distilled water was repeated several times until
the solution was free from both of them. The GO solids
obtained were dried in an oven, then characterized using
XRD, FTIR, SEM-EDX, TEM-SAED, and UV-Visible
Spectrophotometer.
■ RESULTS AND DISCUSSION
X-ray Diffraction Analysis
The diffractogram of each GO material is shown in
Fig. 1. The graphite shows a sharp and narrow central Fig 1. XRD patterns of (a) Graphite, (b) GO-5, (c) GO-
peak at 2θ = 26.213° originated from the hkl plane of 002 6, (d) GO-7

Table 1. XRD data interpretation of all materials

Peak (002) Peak (100)
No. Material
2θ (deg) d (nm) FWHM H (nm) n 2θ (deg) d (nm) FWHM D (nm)
1 Graphite 26.213 0.340 0.744 10.963 32 42.327 0.213 0.458 38.027
2 GO-5 10.487 0.843 1.603 4.977 5-6 42.404 0.213 1.183 14.726
3 GO-6 9.916 0.891 2.030 3.928 4-5 42.216 0.214 1.384 12.579
4 GO-7 9.888 0.894 1.675 4.761 5-6 42.573 0.212 0.967 18.026

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where n is the order of diffraction (1), λ is X-ray Fourier Transform Infra-Red Spectrophotometry
wavelength (spectrum Cu Kα of 0.154 nm), d is the Analysis
distance between lattice plane (nm), θ is diffraction angle. Fig. 3 displays the IR spectrum of graphite and GO
By utilizing the Debye-Scherrer equation (Eq. (2)) samples. In the graphite spectrum, there are no peaks
from peak 002 and 100, we could calculate the height of except for a very weak peak at 3402.58 cm–1 [22]. This
the stacking layer (H) and the average diameter of the peak designates the presence of O–H groups in graphite,
stacking layer (D), respectively. From the H value, we which usually comes from dissolved water molecules
could estimate the number of graphene layers (n = H/d). [23]. Meanwhile, all GO materials revealed characteristic
The dimensions of the plane of each material can also be peaks of oxygen-containing groups. These characteristic
evaluated from D × H calculation [21]. Graphite has a peaks include strong intensity at wavenumbers of ~3400
field dimension of 38 × 11 nm with several layers of 32 for O–H, the weak intensity at ~2800 for C–H sp3, the
pieces, GO-5 has a field dimension of 15 × 5 nm with weak intensity at ~1700 for C=O, the medium intensity
some layers of 5–6 pieces, GO-6 has a field dimension of at ~1500 for C=C of aromatic carbon, the weak intensity
16 × 4 nm with many layers of 4–5 nm, and GO-7 has of ~1300 for C–O–C of ether and ester, and weak intensity
dimensions 18 × 5 nm field with several layers 5–6 nm.
The higher the oxidation level, the resulted layer will be
lower. This can be understood due to the nature of
permanganate oxidation is to exfoliate the graphene
layers from graphite structure. The visualization of the
change in the structure of graphite to graphene oxide has
been presented in Fig. 2.
K λ
D= (2)
B cos θ
where D for plane 100, H for plane 002 is crystallite size
(nm), K is constant (Scherrer constant (0.9) for plane 002,
Warren constant (1.84) for plane 100), λ is X-ray
wavelength (spectrum Cu Kα of 0.154 nm), B is Full
Width at Half Maximum (FWHM) value (radian), and θ Fig 3. FTIR spectra of (a) Graphite, (b) GO-5, (c) GO-6,
is diffraction angle (radian). (d) GO-7

Fig 2. Visualization of changes in the structure of graphite to graphene oxide

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of ~1000 for C–OH for carboxylic acids and alcohols as elemental content in the GO material that had been
the previous work report [7]. The presence of these synthesized. As shown in Fig. 4, graphite powder only
oxygen groups explained the shifting of plane 002 of contains the element carbon. After the graphite was
graphite and GO, which is resulted from the increase of d- oxidized using KMnO4, the carbon content decreases,
spacing due to the introduction of oxygen groups into and the oxygen content appears, which indicates the
graphene layers. All GO materials also contain C=C success of the oxidation reaction. Based on the data in
aromatic bonds in the ~1500–1600 cm–1 region because Table 3, it can be concluded that the more permanganate
this material mostly contains sp2-hybridized carbon is added to graphite, the oxidation level (ratio O/C) will
bonds, and a few regions contain sp3-hybridized carbon also increase. The presence of impurities in the form of
bonds due to the presence of oxygen. Looking at all the Na content in GO-5 of 6.45%, GO-6 of 0.50%, and GO-
peaks of absorption of the oxygen functional groups that 7 of 23.03% was derived from the PBS involved in the
arise, we conclude that these peaks generally have not process of washing the material.
significantly different intensities. For a detailed
Selected Area Electron Diffraction Analysis
interpretation of FTIR data, see Table 2.
SAED is utilized to confirm the polycrystalline
Energy-Dispersive X-ray Spectroscopy Analysis properties of a nanomaterial. This nature is
EDX analysis was conducted to determine the characterized by the presence of diffraction rings that

Table 2. FTIR data interpretation of all materials

Wavenumber of bond type (cm–1)
No Material
O–H C–H C=O C=C C–O–C C–OH
1 Graphite 3402.58 - - - - -
2 GO-5 3427.65 2889.49 1712.86 1619.31 1350.23 1054.14
3 GO-6 3414.15 2890.45 1627.03 1521.90 1326.12 1036.78
4 GO-7 3409.33 2881.77 1713.83 1631.85 1320.33 1043.53

Fig 4. EDX spectra of (a) graphite, (b) GO-5, (c) GO-6, (d) GO-7

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Table 3. Oxidation level of all materials

No Material Mass % of O Mass % of C Ratio O/C
1 Graphite 0 100 0
2 GO-5 37.49 56.06 0.67
3 GO-6 41.04 46.58 0.88
4 GO-7 46.24 30.73 1.50

appear. The SAED pattern of the synthesized GOs is results using SAED, the d-spacing of GO has a value close
shown in Fig. 5. From the pattern above, all GO materials to 0.8 nm in the crystal plane of 002 and around 0.2 nm
revealed a polycrystalline structure with low crystallinity in the crystal plane of 100, which confirms the d-spacing
as denoted by the obscurity of the ring lines, in line with calculation using XRD. We could see a slightly different
previous results [21]. This is likely rendered by the value of d-spacing obtained from SAED and XRD
presence of oxygen functional groups attached to the analysis. The difference may arise from the different
graphene stacking layer containing sp2 hybridized- sizes of analysis. As we have known, SAED analysis is
carbon, resulting in defects in crystals with the emergence carried out in a focused area with several hundred
of new sp3 carbon hybridization [24]. Graphite has nanometers in size, whereas XRD typically samples areas
polycrystalline properties with very high crystallinity and that cover several centimeters of a bulk sample.
bright diffraction rings. According to calculations on the
Scanning Electron Microscopy Analysis
SAED pattern, after oxidation of graphite is executed, the
distance between the graphite layers becomes wider. This The surface morphology of the GO material was
result has been listed in Table 4. Based on the calculation analyzed using SEM. Based on Fig. 6, Graphite shows large

Fig 5. SAED pattern of (a) Graphite, (b) GO-5, (c) GO-6, (d) GO-7

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Table 4. SAED pattern analysis of all materials region indicates the stack layer, which has not been
d (nm) d (nm) exfoliated or has a small distance between layers due to
No Materials
Peak 002 Peak 100 the lack of oxygen functional groups entering the layers.
1 Graphite 0.302 0.156 Meanwhile, the bright area shows the layer which has
2 GO-5 0.768 0.199 been successfully exfoliated [16]. Graphite has a stacked
3 GO-6 0.756 0.218 sheet structure; this indicates its nature, which contains
4 GO-7 0.772 0.243
a graphene multilayer. For GO-5, the material exhibits
the presence of long and fine sheets are folded together.
chunks with a rough and crumpled surface. GO-5 and
Meanwhile, for GO-6 and GO-7, both appear to have a
GO-6 materials have a morphology similar to the
thin layer that is rather wide with slightly different
appearance of an exfoliated layer with a wrinkled and
transparency. Although there are slight differences in
irregular surface. In comparison, GO-7 displays a
transparency and the resulting layers, most of the
morphology like a lot of small gravel, indicating excessive
structures of these three materials are classified as having
oxidation reactions.
similar nanostructures that support the d spacing data
Transmission Electron Microscopy Analysis on XRD and SAED and the intensity of oxygen function
TEM images are applied to evaluate the morphology absorption on FTIR.
of each material (Fig. 7). According to the literature, the UV-Visible Spectrophotometry Analysis
permanganate provides a product with wrinkled
UV-Visible spectra of various GO are disclosed in
structures, while the chlorates lead to the synthesis of
Fig. 8. GO has two characteristic absorption bands on
graphite oxide with the planar structure of the material
UV-Visible spectra. The central peak at a wavelength of
[25]. These images have bright and dark areas. The dark

Fig 6. SEM images of (a) Graphite, (b) GO-5, (c) GO-6, (d) GO-7

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Fig 7. TEM images of (a) Graphite, (b) GO-5, (c) GO-6, (d) GO-7

preparation for analysis.

We also evaluate the band gap energy values on the
resulted GO materials to determine the optoelectronic
properties. Optical band gap energies of GO were
estimated using the Tauc plot as presented in Fig. 9,
following Eq. (3):
( αhν )1/m
= A ( hν − Eg ) (3)
where α is absorption coefficient, hν is photon energy, A
is constant, Eg is band gap energy, and m is nature of
transition, m = 1/2 for direct allowed transitions.
Graphite is known as a conductor with a band gap
Fig 8. UV-Vis absorption spectra and visual appearances of about zero eV [27-28]. Following the oxidation from
of (a) GO-5, (b) GO-6, (c) GO-7 GO, we could see an increase in band gap values to
approximately 3 eV. The increase in band gap value is
230–240 nm correlated to the transition π→π* of the caused by oxygen molecules on the surface. It has been
aromatic C=C bond and the shoulder peak at a reported that the greater d-spacing between graphene
wavelength of 290–300 nm, which is responsible for the layers will limit the overlap of p orbitals, thereby
n→π* transition of the C=O bond [26]. Unfortunately, we reducing the effectiveness of the conjugate length of the
could not show UV-Vis spectra of graphite due to the π bond [29]. Furthermore, the oxygen functional group
non-polar characteristic, which inhibiting the solution with sp3 hybridization could results in structural changes

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Fig 9. A Tauc plot of (a) GO-5, (b) GO-6, (c) GO-7

on the GO surface so that it disrupts the flow of electrons, used as a window layer in heterojunction solar cells [31].
thus limiting the electronic conduction. Therefore, we may Based on the results and discussion above, it can be
say that the presence of oxygen functional groups reduces considered that GO material synthesis has been
the electrical properties of GO, as evidenced by the increase successfully carried out through several evaluations. XRD
in the value of the band gap [30]. However, we could not data states that the d-spacing value increases with an
see any significant difference in band gap value to the increasing number of permanganates added, which is also
number of oxidants. This may suggest that the oxidant supported by SAED data. Band gap analysis of the three
ratio we used in this report is not significantly affecting to materials produced a value of around 3 eV confirmed by
amount of oxygen functional groups as supported by the the absorption intensity of oxygen-containing groups
similarity of FTIR results. The use of FTIR also limits our similar in the FTIR spectra. GO with a band gap value of
capability to distinguish the type of oxygen functional 3 eV is very potential for further applications in the solar
groups. With a 3 eV band gap, GO is the potential to be cell field.

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■ CONCLUSION [3] Zhu, J., Duan, R., Zhang, S., Jiang, N., Zhang, Y.,
and Zhu, J., 2014, The application of graphene in
Research on the effect of adding permanganate to
lithium-ion battery electrode materials,
graphite has been carried out using the Improved Tour
SpringerPlus, 3 (1), 585.
oxidation method, resulting in GO-5, GO-6, and GO-7.
[4] Nag, A., Mitra, A., and Mukhopadhyay, S.C., 2018,
The results showed that the three GO materials have
Graphene and its sensor-based applications: A
similar chemical properties and structures. Starting from
review, Sens. Actuators, A, 270, 177–194.
the results of XRD analysis, the d spacing value is around
[5] Yang, W., Ni, M., Ren, X., Tian, Y., Li, N., Su, Y.,
0.8 nm, while from the results of SAED, the d spacing
and Zhang, X., 2015, Graphene in supercapacitor
value is approximately 0.7 nm. FTIR spectra also display
applications, Curr. Opin. Colloid Interface Sci., 20
typical absorption peaks of oxygen functionalized carbon
(5-6), 416–428.
at several wavenumbers with characteristic intensities.
[6] Li, J., Zhao, Z., Ma, Y., and Qu, Y., 2017, Graphene
The oxidation level exhibits an increase in the O/C ratio
and their hybrid electrocatalysts for water splitting,
with the addition of permanganate to graphite. The
ChemCatChem, 9 (9), 1554–1568.
morphological structure of both SEM and TEM also
[7] Velasco-Soto, M.A., Pérez-García, S.A., Alvarez-
indicates insignificant differences. The results of UV-
Qiuntana, J.A., Cao, Y., Nyborg, L., and Licea-
Visible spectroscopy analysis denote a main peak with the
Jiménez, L., 2015, Selective band gap manipulation
highest absorbance at a wavelength of about 230 nm and
of graphene oxide by its reduction with mild
the shoulder peak at a wavelength of about 300 nm. At the
same time, the resulting band gap energy is around 3.5– reagents, Carbon, 93, 967–973.
3.7 eV. With this band gap value, GO can be utilized for [8] Luong, D.X., Bets, K.V., Algozeeb, W.A., Stanford,
further applications in the solar cell field. M.G., Kittrell, C., Chen, W., Salvatierra, R.V., Ren,
M., McHugh, E.A., Advincula, P.A., Wang, Z.,
■ ACKNOWLEDGMENTS Bhatt, M., Guo, H., Mancevski, V., Shahsavari, R.,
The authors thank the Ministry of Research, Yakobson, B.I., and Tour, J.M., 2020, Gram-scale
Technology, and Higher Education, Republic of bottom-up flash graphene synthesis, Nature, 577
Indonesia, for the fund through the PMDSU Research (7792), 647–651.
Grant 2020 (Contract Number: 3150/UN1.DITLIT/DIT- [9] Eswaraiah, V., Aravind, S.S.J., and Ramaprabhu, S.,
LIT/PT/2020) and also Universitas Gadjah Mada for the 2011, Top-down method for synthesis of highly
financial support of this work under the scheme of the conducting graphene by exfoliation of graphite
Rekognisi Tugas Akhir (RTA) 2020. oxide using focused solar radiation, J. Mater.
Chem., 21 (19), 6800–6803.
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