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Materials Express
2158-5849/2019/9/813/008
Copyright © 2019 by American Scientific Publishers
All rights reserved. doi:10.1166/mex.2019.1565
Printed in the United States of America www.aspbs.com/mex
Investigation on nanographene generation and
its molecule adsorption
Junxia Zhang1, 2, ∗ , Zehua Wang1 , Binwu Wang2 , and Xiaopeng Song2
1
School of Mechanical and Energy Engineering, Shaoyang University, Shaoyang 422000, Hunan Province, PR China
2
School of Energy and Building Environment, Guilin University of Aerospace Technology, Guilin 541000,
Guangxi Province, PR China
ABSTRACT
An experimental method was applied to prepare nanographene, in which its surface feature was analyzed using
Article
scanning electron microscope and Fourier infrared ray analyzer. A methylene blue (MB) solution was adopted
to measure the molecule adsorption of nanographene and graphite and demonstrated that nanographene had
IP:that
more molecule adsorption than 192.168.39.211 On:the
by graphite. As Tue, 09 Nov 2021of23:13:04
concentration MB solution increased, the molecule
Copyright: American Scientific Publishers
adsorption of nanographene ascended. As Delivered
the stirringbytime of
Ingentaa magnetic stirrer decreased, the molecule
adsorption of nanographene in the MB solution increased significantly. Meanwhile, the increment in the absorp-
tion amount of graphite reduced. As the dosage of nanographene and graphite increased, the absorption
capacity of nanographene reached a peak value of 40 mg, which was two- or threefold higher than that of
graphite. Hence, nanographene has higher molecule adsorption capacity than graphite.
Keywords: Nanographene, Graphite, Preparation, Molecule Adsorption.
1. INTRODUCTION Graphenano Company and Kerr Maria University in Spain.
In 2004, AndreGeim and Konstantin [1] used a special The load capacity of this polymerized battery was three-
tape to exfoliate graphene successfully (named after a fold higher than existing batteries. At present, nanoma-
micromechanical cleavage method), which demonstrated terials have been widely applied in catalytic degradation,
the existence of graphene. In June 2011, the first inte- biomedicine, defense-related science and technology, opti-
grated circuit in the world was prepared with graphene in cal materials, microelectronic devices, sensors, and mag-
the research center of IBM [2]. In March 2013, a super- netic materials.
capacitor made in graphene was investigated by several Many scholars have investigated the preparation and
American scientists; its charge efficiency is much higher structural performance of nanographene. Wu et al. [4]
than that of ordinary materials. When this supercapaci- adopted a one-step hydrothermal synthesis to generate
tor was used to make cellphone, the charge time is sev- graphene quantum dots that possess a strong absorption
eral seconds only. Researchers in the Berkeley Institute of band at the UV region and a strong, narrow, and excitation-
California University prepared photodetector [3] that can independent emission peak. Graphene quantum dots can
realize fast data communication in several milliseconds. be used to measure Mn2+ ions. Liu et al. [5] synthe-
In 2015, a polymerized battery with considerable load sized graphene with a Mn compound via a hydrother-
and discharge capacities was made with graphene by the mal method. These researchers analyzed the effects of
the mole ratio of KMnO4 to citric acid on the MnOOH
∗
Author to whom correspondence should be addressed. and MnCO3 contents and found that graphene synthe-
Email: wyb700411@163.com sis with MnOOH has excellent cycle stability and the
Mater. Express, Vol. 9, No. 7, 2019 813
Materials Express Investigation on nanographene generation and its molecule adsorption
Zhang et al.
best super-capacitance when the mole ratio of KMnO4 2. EXPERIMENTS ON GENERATING
to citric acid is 8:3. The specific capacitance can reach NANOGRAPHENE
267.7 F/g at a current density of 0.5 Å/g. Wang et al. [6] 2.1. Experiments on Generating Nanographene
developed a composite material involving cobalt oxide Existing methods to prepare graphene mainly include the
nanoparticles and graphene (CoO/RGO) via the hydrother- chemical vapor deposition (CVD), the micro-mechanical
mal method. CoO nanoparticles loaded on the surface cleavage method, the oxidation–reduction method and the
of graphene nanosheets can prevent graphene aggrega- epitaxial growth method. In the CVD method, hydrocar-
tion, thereby forming a large 3D electron conductive bon is added on the heating base metal to react to the
network that can promote the electrical conductivity of base metal and produce multiple and single graphene lay-
composites. Du et al. [7] prepared two functionality-type ers. This reaction is a displacement reaction. In particular,
single-layer graphene types by using a low-temperature this method, which can displace a C atom in the hydro-
thermal exfoliation approach, in which the maximum spe- carbon with the metal to form graphene, requires a low
cific capacitance is approximately 220 F/g in the KOH reaction temperature to obtain graphene with good quality
system of 2 mol/L. Sui et al. [8] prepared graphene and large size and realize large-scale production. However,
with the reduction of graphene oxide through glycol by the cost of raw materials and devices are high, and the
using a hydrothermal method. Zeng et al. [9] adopted a thickness of graphene cannot be controlled mainly because
hydrothermal method to synthesize TiO2 -pillared graphene a small quantity of C during deposition is transformed into
nanocomposites and investigated its effect on photocatal- graphene. This process occurs in C growth and connec-
ysis. These researchers found that the kind of mate- tion because a complex conversion is difficult to control.
rial influences photocatalysis during methylene blue (MB) In 2004, scientists used mechanical cleavage method to
degradation. Bi et al. [10] developed an optical modula- prepare graphene by repeatedly removing the specific tape
tor on the basis of graphene. Lu et al. [12] had developed adhered on graphene to obtain graphene with the size in
a fluorescence quenching based approach using grapheme the range of 10–100 m. The graphene obtained using this
oxide for rapid detection of miRNAs. Dan et al. [12] method has high quality and low cost, and the operation
Article
introduced a 2D CCA into a layer-by-layer composite is simple. However, this method requires a long time, and
membrane based on reduced graphene oxide and two-
IP: 192.168.39.211 On: Tue,is09unsuitable
Nov 2021 for23:13:04
large-scale production.
dimensional colloidal crystal array. Copyright:
Zhang et American
al. [13] Scientific
In the Publishers
oxidation reduction method, a strong acid (e.g.,
developed a PEGylated reduced graphene oxide (PEG- bysulfuric
Delivered Ingentaacid) and an oxidizer (e.g., potassium perman-
RGO) nanovector for efficient delivery of ssRNA. Wang ganate) are added into the graphene powder. Graphite
et al. [14] reported a simple and efficient preparation oxide was obtained at an appropriate temperature. The part
method of an inverse-opal-like macroporous polytetraflu- of graphite oxide was prepared via ultrasonic dispersion.
oroethylene (IO-PTFE) film with a reusable matrix. Xia Then, a strong reducer was added into the solution to
et al. [15] prepared a kind of three dimensional phytic obtain graphene. This method required low-cost raw mate-
acid-induced graphene coating by hydrothermal synthe- rial and devices, can be easily operated, and can be used
sis and fabricated on a stainless-steel wire using physical in large-scale production. However, the obtained graphene
coating method as a solid phase microextrastion coating. had large defects due to the lack of –OH functional
Zhang et al. [16] studied the size-dependent viscoelasticity group and incomplete structure. Graphene is also easy to
in polymer nanofibers and reported the first experimen- reunite, thereby affecting the measurement of electrical
tal evidence of significant size-dependent stress relaxation and mechanical properties and limiting its application.
in electrospan nanofibers as well as size-dependent poly- The epitaxial growth method was divided into the epi-
lactic acid/modified graphene of the confined amorphous taxial growths of SiC and metal catalysis. The reaction
regions. Li and Xie [17] reported an effective strategy for mechanism of SiC epitaxial growth method was to heat
the polyolefin-functionalized graphene oxide using two- SiC in the vacuum at high temperature, separating Si from
step methods. its surface, and leave a processing of C atom solving, reor-
Investigations on nanographene molecule adsorption in ganizing, and growing. This method can obtain graphene
the literature are limited. In this work, graphite pow- with single or two layers.
der was used to prepare nanographene by means of an The epitaxial growth of metal catalysis is achieved by
improved hydrothermal method. The structural features of pouring hydrocarbon onto the metal surface in a vacuum
nanographene were investigated using a scanning elec- at high temperature to obtain graphene through dehy-
tron microscope (SEM) and Fourier infrared ray analyzer, drogenation. Large-scale graphene production and high-
and a part of nanographene was placed in the MB solu- quality of graphene is obtained with this method. However,
tion to analyze the effects of MB solution concentration, this method requires costly raw materials and devices and
nanographene dosage, pH value of MB solution and stir- is difficult to maintain at high temperature of 1400 C
ring time on nanographene molecule adsorption compared and vacuum atmosphere. Forming film is also difficult.
with that of graphite. Other methods of generating graphene include C nanotube
814 Mater. Express, Vol. 9, 2019
Investigation on nanographene generation and its molecule adsorption
Zhang et al.
Materials Express
Table I. Agents needed for the graphene preparation. (5) The conical flask was immersed in water at 35 C
and reacted for 30 min, and the solution was diluted with
Agent Chemical Place of
name formula Size production deionized water of 69 mL at the temperature of 57 C, and the thin
added into the conical flask by means of a glass rod
layer of the obtained bright silver graphene was ground
drainage. Meanwhile, the system temperature was con-
into the powder after drying.
trolled at 7 C
and reaction time of 2 h;
Table II. Main experimental devices used in experiments.
Devices Size Place of production
Digital display type magnetic stirrer DF-II Chongqing in China
Electric-heated thermostatic HH-S6 Beijing in China
water bath
High speed freezing centrifuge TGL21M Hunan in China
Integrated ice maker AM-200 Shanghai in China
Ultrasonic cleaner 2013QT Con son in China
Electronic balance YP20002 Shanghai in China
Vacuum drying oven DZF-6050B Shanghai in China
Sliding vane rotary vacuum pump 2XZ-2 Linhai in China
Scanning electron microscope 300 Zeiss in Germany
Visible range spectrophotometer 722N Shanghai in China
Fourier Infrared-ray analyzer IR Prestige-21 Shimadzu in Japan
Fig. 1. Graphite oxide solution.
Mater. Express, Vol. 9, 2019 815
Materials Express Investigation on nanographene generation and its molecule adsorption
Zhang et al.
solution was washed with HCl and deionized water alter-
nately several times until the pH value became neutral.
The obtained supernatant by centrifugation showed a faint
yellow color, and the graphite oxide displayed a brown
yellow color, as shown in Figure 2. The graphite oxide
washed with absolute ethyl alcohol showed the presence
of debris, and the obtained supernatant after centrifugation
and sticky sediment showed a bright black color. The thin
layer of graphene after drying and precipitation displayed
a bright silver color, as shown in Figure 3.
3. RESULTS AND DISCUSSION
3.1. Structural Performance of Graphene
Fig. 2. Centrifugated supernatant and diluted graphite oxide
3.1.1. SEM Analysis
precipitates. SEM can use electron beams to scan the sample surface
microscopically, thereby revealing information on the sam-
ple surface. SEM identifies the surface structure by obtain-
molecules into the layer of graphite powder and deco- ing a 3D high-resolution diagram of the sample surface
rate the O-containing functional groups on the surface according to the interaction between the electrons and the
of graphene, thereby increasing the distance between the material. In our experiments, the patterns of sample surface
graphite powder layers. These processes can enable the were measured by a SEM with 300 (Germany), in which
oxidation of strong oxidants. The function of the fourth its magnification ranged from 0.1 to 1 million and accel-
step was to oxidize graphite powder with the strong oxi- eration voltage was within 0.02–30 kV. Figure 4 shows a
dation of potassium permanganate and concentrated sul-
Article
SEM diagram of graphene. Before the SEM characteriza-
furic acid for the decoration of hydroxyl and carboxyl tion, a sample was made by coating graphene powder on
groups by changing the acting IP: 192.168.39.211
force On: Tue,the
between molecules 09plate
Nov through
2021 23:13:04
metal spraying to obtain a good obser-
Copyright:
and increasing the hydrophilicity of graphite powder.American
Thus, Scientific Publishers
Delivered vation effect. The sealing chamber of the SEM was filled
graphite powder is convenient to dissolve in water. Here, bywith
Ingenta
N to isolate air and avoid sample pollution by the
washing with ice ensures the safety of experiments and substances suspended in air. As shown in Figure 4, the
reaction velocity. The addition of deionized water in the surface of graphene was smooth, and some evident fold
fifth step reduces the acidic property and improves the structures can be observed at 5.58 k× magnification. How-
pH value. The functions of the seventh and eighth steps ever, at 7.13 k× magnification, these folds displayed in
were to extract the prepared graphite oxide. The addi- the way of single-layer structure, were complete and had
tion of 5% HCl prevented the expansion and hydrophilic- considerable transparency. This finding indicated that the
ity of graphite oxide, while washing with deionized water reduction state of nanographene is ideal.
made the pH value of the solution neutral and remove sul-
fate ions in sample detection. In preparing graphite oxide, 3.1.2. FI-IR Analysis
H2 O2 was added into the solution at 80 C, which changed
The FI-IR spectrum can be used to investigate the vari-
in the color of the solution from brown to bright yel-
ation law of the surface O functional groups before and
low, as shown in Figure 1. The obtained graphite oxide
after the reduction reaction of graphite oxide. Figure 5
shows the diagram of FI-IR spectrum on graphite oxide
and graphene. As shown in Figure 5, graphene obtained
through reduction reaction had more intensive molecule
absorption property at the ranges of 550 cm−1 ∼3240 cm−1
and 3440 cm−1 ∼4000 cm−1 wavelength, and the transmit-
tance reduced accordingly. It is indicated that the graphene
has more intensive molecule absorption property than that
by the graphite oxide.
3.2. Comparison of Graphite and
Molecule Adsorption
A 722N-type visible spectrophotometer (Shanghai Jinghua
Technological Instruments Co., Ltd.) with measurable
Fig. 3. Thin layer graphene. wavelength range between 190 and 100 nm was used
816 Mater. Express, Vol. 9, 2019
Investigation on nanographene generation and its molecule adsorption
Zhang et al.
Materials Express
Fig. 4. SEM images of graphene.
to analyze the component and structure of graphite and of 100 mL each were added into these conical flasks,
nanographene samples quantitatively. The device could be and their concentrations were 1, 2, 3, 4, and 5 mg/L.
applied to evaluate the sample structures and their interac- These conical flasks were shaken to disperse graphite and
tions according to their absorption spectrum because the nanographene in the MB solution. At the pH value of 6
molecule and electron exhibit a transition when the photon and a temperature of 20 C, the solutions in these conical
in incident light was absorbed by the substances. Then, flasks were stirred and centrifuged using a magnetic stir-
nanographene and graphite were used as adsorbents to rer at constant temperature. The supernatant liquids were
absorb the MB solution, and their molecule adsorption was removed, the molecule adsorptions were measured with
detected by the 722N-type visible spectrophotometer. The the 722N-type visible spectrophotometer, and the absorp-
Article
MB solution concentrations were 1, 2, 3, 4, and 5 mg/L. tion amounts were calculated, as shown in Figure 7. When
The molecule adsorption of the MB solution in the wave- the MB solution concentration ranged from 1 mg/L to
length from 200 nm to 900 nm isIP: 192.168.39.211
shown On: Tue, 09 Nov 2021 23:13:04
in Figure 6, which 5 mg/L, as the concentration of MB solution increased, the
Copyright: American Scientific Publishers
conformed with the following linear equation: Delivered byadsorption
Ingenta amount of nanographene increased instantly.
y = 0.182x − 0.063 (1) Although the absorption amount of graphite also rose, it
gradually tended to a balance and no longer increased
where y is the molecule adsorption, and x is the concen- as the MB solution concentration increased. Therefore,
tration of the MB solution (mg/L). Therefore, MB solution nanographene has greater absorption effect than that by
concentration displays a good linear variation. graphite mainly because nanographene has a larger spe-
cific surface area than that of graphite, which increases the
3.2.1. Effect of MB Solution Concentrations on absorption points.
Sample Molecule Adsorption
Ten copies of graphite and nanographene with the mass
of 20 mg each were placed into ten 150 mL coni-
cal flasks. Ten copies of MB solution with the volume
Fig. 5. FI-IR spectra diagram of graphite oxide and graphene. Fig. 6. Standard curve of MB solution molecule adsorption.
Mater. Express, Vol. 9, 2019 817
Materials Express Investigation on nanographene generation and its molecule adsorption
Zhang et al.
Fig. 8. Effect of stirring time on graphite and graphene molecule
Fig. 7. Effect of MB solution concentration on graphite and graphene adsorption.
molecule adsorption.
3.2.3. Effect of Graphite and Graphene Dosages on
MB Solution Molecule Adsorption
3.2.2. Effect of Stirring Time on the Molecule
Five copies each of graphite and nanographene respec-
Adsorption of Samples
tively were placed into five 150 mL conical flasks, with
Article
Two copies each of graphite and graphene with 20 mg the masses of 5, 10, 15, 20, and 25 mg, respectively.
mass were placed into two 150IP: mL192.168.39.211
conical flasks sepa-
On: Tue,The MB 2021
09 Nov solutions with the volume of 100 mL and the
23:13:04
rately. Two MB solution copies with the volume ofAmerican
Copyright: 100 mL Scientific Publishers
concentration of 3 mg/L were added into these coni-
each and the concentration of 3 mg/L were placed Delivered
into bycal
Ingenta
flasks. At pH value of 6 of the MB solution and a
two conical flasks. The two conical flasks were shaken to solution temperature of 20 C, the MB solutions were
disperse graphite and graphene in the MB solution. At pH stirred for 120 min and centrifuged using a magnetic stir-
value of 6 and temperature of 20 C, the solutions in the rer at a constant temperature. The supernatant liquids were
two conical flasks were stirred using a magnetic stirrer removed and centrifuged, the graphite and nanographene
at constant temperature. A total of 15 mL of the solu- molecule adsorption were measured by the 722N-type vis-
tion was taken out every 30 min and centrifuged, and then ible spectrophotometer, and their absorption amounts were
its supernatant liquid was removed. The 722N-type visi- calculated. Figure 9 shows the effects of the dosages of
ble spectrophotometer was used to measure the molecule graphite and nanographene on the molecule adsorption
adsorption, and the absorption amounts of graphite and of MB solution. As shown in Figure 9, as the dosage
graphene were calculated. The effects of stirring time of graphite and nanographene increased, the absorption
on molecule adsorptions of graphite and graphene are amounts of nanographene and graphite in the MB solution
shown in Figure 8. The molecule adsorption curve of fluctuated. When the nanographene dosage was 40 mg, its
graphite and nanographene rapidly increased at stirring absorption amount in the MB solution reached its max-
time ofInvestigation on nanographene generation and its molecule adsorption
Zhang et al.
Materials Express
Fig. 10. Effects of the pH value on graphite and nanographene
Fig. 9. Effects of graphite and graphene dosages on MB solution
molecule adsorption.
molecule adsorption.
intensive than that of graphite, and its optimal dosage was occupied the absorption sites with the MB molecules in the
40 mg. MB solution, thereby reducing the absorption amount of
MB molecules on the graphite or nanographene surfaces.
3.2.4. Effect of MB Solution pH on Sample When the pH value of MB solution was 4, the graphite
Article
Molecule Adsorption and nanographene surfaces possessed a large amount of
Five copies each of graphite and IP:nanographene
192.168.39.211 the Tue,negative
withOn: 09 Novcharges, while the MB solution possessed many
2021 23:13:04
Copyright:
mass of 20 mg each were placed five 150 mL conical American Scientific
cationic Publishers
dyes. Thus, graphite and nanographene have a
Delivered
flasks, and the MB solutions with the volume of 100 mL by Ingenta
good adsorption function on the MB solution under the
and the concentration of 3 mg/L were placed into these function of static electricity. Graphite and nanographene
conical flasks. Diluted HCl and NaOH solutions were used also have optimum absorption effects when the pH value
to adjust the pH values of the MB solution to 2, 4, 6, 8, and of the solution is 4.
10, respectively. A treater was placed in each conical flask
and stirred for 120 min, and then the supernatant liquid
4. CONCLUSION
was removed after centrifugation. The molecule adsorp-
An improved oxidation reduction method was used to
tion for each sample was measured with the 722N-type
prepare nanographene. The absorption performances of
visible spectrophotometer, and the absorption amount was
graphene and nanographene were investigated by adjust-
then calculated. Figure 10 shows the effects of the pH
value of the MB solution on the molecule adsorptions of ing the dosages of graphite and nanographene, pH, MB
graphite and nanographene. The absorption amounts of solution concentration, and stirring time to determine their
graphite and nanographene in the MB solution increased molecule adsorption capabilities. The conclusions are sum-
first and then decreased with the increase in the pH value marized as follows:
of the MB solution from 2 to 10. When the pH of MB (1) Given the atmosphere temperature and MB solu-
solution was 4, the absorption curves of graphite and tion (volume of 200 mL and concentration of 1 mg/L),
nanographene showed a peak value and reached the max- the maximum absorption amount of nanographene was
imum value. When the pH value of MB solution was 3.215 mg/g at the nanographene dosage of 40 mg and the
>4, the absorption curves of graphite and nanographene stirring time of 180 min when the pH value of the MB
showed a slowly decreasing trend mainly because the pH solution was 4.
value of MB solution affects the charge distribution on (2) The absorption amount of nanographene was two-
the graphite and nanographene surfaces, thereby causing or threefold higher than that of graphite under the same
the change between graphite or nanographene and the conditions.
MB solution. Both OH− and MB molecules occupied the (3) The prepared nanographene had a good absorption
absorption sites on nanographene and graphite surfaces, performance, large specific surface area, and additional
thereby causing a decrease in the absorption amounts of absorption site points.
MB molecules on graphite or nanographene. When the (5) The nanographene molecule adsorption was larger
pH value of MB solution was 2, a large amount of H+ than that of graphite.
Mater. Express, Vol. 9, 2019 819Materials Express Investigation on nanographene generation and its molecule adsorption
Zhang et al.
Acknowledgments: We are grateful for the support of 9. Zeng, X.F., Wang, M.H., Lu, Y.L., Zhang, Y.L. and Chen, L.,
Project of Science and Technology Department of Shaanxi 2018. Synthesis and enhanced photocatalytic activity of TiO2 pillared
graphene nanocomposites. Powder Metallurgy Technology, 36(2),
Provincial [Grant numbers 2018CG-026], National Natural
pp.130–136.
Science Foundation of China [Grant numbers 51866015] 10. Bi, W.H., Wang, X.Y., Fu, G.W. and Wang, Y.Y., 2015. Review on
and the Project of Guangxi Natural Science Foundation of optical modulator based on graphene. Journal of Yanshan University,
China [Grant numbers 2018JJA160070]. 39(3), pp.189–198.
11. Lu, Z.X., Zhang, L.M., Deng, Y., Li, S. and He, N.Y., 2012.
Graphene oxide for rapid MicroRNAs detection. Nanoscale, 4(19),
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Received: 23 May 2019. Accepted: 27 August 2019.
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