KR101856163B1 - Method for improving the yield of graphene and the graphene made thereby - Google Patents
Method for improving the yield of graphene and the graphene made thereby Download PDFInfo
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- KR101856163B1 KR101856163B1 KR1020160028699A KR20160028699A KR101856163B1 KR 101856163 B1 KR101856163 B1 KR 101856163B1 KR 1020160028699 A KR1020160028699 A KR 1020160028699A KR 20160028699 A KR20160028699 A KR 20160028699A KR 101856163 B1 KR101856163 B1 KR 101856163B1
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- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/182—Graphene
- C01B32/184—Preparation
- C01B32/19—Preparation by exfoliation
- C01B32/192—Preparation by exfoliation starting from graphitic oxides
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- C01B32/00—Carbon; Compounds thereof
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- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C207/00—Compounds containing nitroso groups bound to a carbon skeleton
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- C07D403/00—Heterocyclic compounds containing two or more hetero rings, having nitrogen atoms as the only ring hetero atoms, not provided for by group C07D401/00
- C07D403/02—Heterocyclic compounds containing two or more hetero rings, having nitrogen atoms as the only ring hetero atoms, not provided for by group C07D401/00 containing two hetero rings
- C07D403/04—Heterocyclic compounds containing two or more hetero rings, having nitrogen atoms as the only ring hetero atoms, not provided for by group C07D401/00 containing two hetero rings directly linked by a ring-member-to-ring-member bond
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- C07D403/00—Heterocyclic compounds containing two or more hetero rings, having nitrogen atoms as the only ring hetero atoms, not provided for by group C07D401/00
- C07D403/14—Heterocyclic compounds containing two or more hetero rings, having nitrogen atoms as the only ring hetero atoms, not provided for by group C07D401/00 containing three or more hetero rings
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- C01B2204/00—Structure or properties of graphene
- C01B2204/20—Graphene characterized by its properties
- C01B2204/22—Electronic properties
Abstract
The present invention relates to a method for producing graphene capable of water dispersion with improved yield and graphene produced thereby,
A first step of pretreating graphite with chlorosulfonic acid (CSA) and hydrogen peroxide; A second step of mixing the pretreated graphite with an N-oxide compound and graphite; A third step of mixing the mixture of the second step with a dispersion treatment and a solvent; And a fourth step of obtaining a graphene from the mixture of the third step. The present invention also relates to a method for producing graphene having an improved yield.
Description
The present invention relates to a process for producing graphene capable of improving water dispersion and a graphene produced thereby and more particularly to a process for producing graphene which can be utilized in various fields due to improved yield and electric conductivity of graphene Method and graphene produced thereby.
With the rapid growth of the industry in recent years, there is a growing demand for nanocomposites that can be applied to a variety of products such as food packaging, semiconductors, gasketing, automotive articles, and portable electronic equipment. These nanocomposites require excellent electrical conductivity and thermal conductivity, along with tensile strength, abrasion resistance, thermosetting and thermoplastic properties.
Carbon nanotubes are now known as nanocomposite materials having excellent mechanical properties and electrical conductivity. However, there is a disadvantage in that the production cost is very high because the addition of the metal catalyst is required in the gas phase process in order to produce pure single-walled carbon nanotubes. In addition, since single-walled carbon nanotubes are characterized in that their metal and semiconductor characteristics are different according to the chirality and diameter, single-walled carbon nanotubes must be separated to suitably use the metal characteristics of single-walled carbon nanotubes. In this case, It is known that purification / separation is very difficult because of the presence of heavy metal contaminants in the final material.
Therefore, it is absolutely urgent to develop new nanocomposite materials having excellent chemical and mechanical properties applicable to various fields.
In this regard, since Andre Geim's research group at Manchester University in the United Kingdom in 2004 introduced how to make graphene from graphite, graphene has become the most It has become a subject of much interest.
Graphite has a structure in which sheets of carbon aggregates connected in a hexagonal honeycomb shape are stacked two-dimensionally. Graphene refers to a sheet of a thickness of a carbon atom layer or a sheet structure of an aqueous layer thickness separated from the laminated sheet constituting the graphite, and the sheet thickness thereof is 0.3 nm which is approximately one carbon atom.
The graphene has an advantage in that the electrical characteristic can be changed according to the crystal orientation of the graphene having a given thickness, so that the user can easily design the device by expressing the electrical characteristic in the selecting direction. For example, the electron transfer rate in graphene is about 20,000 to 50,000 cm 2 / Vs, which is 100 times faster than copper, and the heat resistance and strength have physicochemical characteristics comparable to those of carbon nanotubes. Therefore, according to the characteristics of graphene, carbon-based electric devices or carbon-based electromagnetic devices can be effectively used in the future.
The present invention provides a graphene having improved water dispersibility and a method for producing the graphene, wherein the N-methyl morpholine-N-oxide monohydrate (NMMO ) To prepare water-dispersible graphene. It has excellent electrical conductivity because there is no defect in graphene. However, this patent has a problem in that the yield of graphene produced using NMMO is low. In addition, as in the case of carbon nanotubes, there is a disadvantage in that it is very difficult to mass-produce and manufacture high-purity materials as well as to incur huge costs in the production method.
DISCLOSURE Technical Problem Accordingly, the present invention has been made to solve the above-mentioned problems, and it is an object of the present invention to provide a method of manufacturing graphene, which can produce graphene with a simple process, And to provide a manufacturing method of graphene.
Another object of the present invention is to provide graphene produced by the above-mentioned method for producing graphene.
It is another object of the present invention to provide a polypyrrole composite produced by using the graphene.
According to an aspect of the present invention, there is provided a process for preparing a graphite powder, comprising: a first step of pretreating graphite with chlorosulfonic acid (CSA) and hydrogen peroxide; A second step of mixing the pretreated graphite with an N-oxide compound and graphite; A third step of mixing the mixture of the second step with a dispersion treatment and a solvent; And a fourth step of obtaining a graphene from the mixture of the third step. The present invention also provides a method for producing graphene having an improved yield.
According to another aspect of the present invention, there is provided a graphene produced by a process for producing graphene having improved yield.
In addition, the present invention for solving still another problem of the present invention relates to the provision of the graphene-containing polypyrrole composite.
The graphene production method of the present invention can produce graphene by a simple process and has an effect of increasing the yield of graphene.
In addition, the graphene produced by the method has improved water dispersion and electric conductivity and is applicable to various fields.
1 is a photograph showing a manufacturing process of graphene according to an embodiment of the present invention.
2 is a photograph of graphene prepared according to an embodiment of the present invention before and after ultrasonic treatment.
3 is a photograph before and after ultrasonication of graphene prepared according to an embodiment of the present invention.
FIG. 4 shows the results of measuring the dispersion stability of graphene prepared according to an embodiment of the present invention.
5 is an SEM image of graphene prepared according to one embodiment of the present invention.
Figure 6 is a Raman stacker of graphene prepared according to one embodiment of the present invention.
Figure 7 is an XPS spectra of graphene prepared according to one embodiment of the present invention.
8 is an XRD photograph of graphene prepared according to an embodiment of the present invention.
9 is a photograph showing a process for producing a composite of graphene and polypyrrole according to an embodiment of the present invention.
10 is a cyclic voltammetry curve of a polypyrrole composite prepared according to an embodiment of the present invention.
Figure 11 is a charge-discharge curve of a polypyrrole composite prepared according to one embodiment of the present invention.
12 is a graph showing the capacitance lifetime evaluation of polypyrrole composites prepared according to one embodiment of the present invention.
Hereinafter, the present invention will be described in more detail.
The present invention relates to a process for producing graphene with improved yield and to graphene produced thereby.
More specifically, according to one aspect of the present invention,
A first step of pretreating graphite with chlorosulfonic acid (CSA) and hydrogen peroxide; A second step of mixing the pretreated graphite with an N-oxide compound and graphite; A third step of mixing the mixture of the second step with a dispersion treatment and a solvent; And a fourth step of obtaining a graphene from the mixture of the third step. The present invention also provides a method for producing graphene having an improved yield.
First, a first step of pretreating graphite with chlorosulfonic acid (CSA) and hydrogen peroxide is performed. Through this pretreatment, the distance between the layers of graphite can be widened, and thus, in the NMMO treatment, the NMMO can be inserted more easily between the layers of the graphite. The greater the amount of NMMO contained between the layers of graphite, the less stimulation can be separated into one layer influences the increase in yield.
Next, a second step of mixing the pretreated graphite with an N-oxide compound and graphite is carried out. The N-oxide compound is not particularly limited as long as it can be used in the production of graphene, but N-methylmorpholine-N-oxide (NMMO), amine-N-oxide N-oxide, pyridine-N-oxide, N-methyl-2-pyrrolidone, dimethylformamide, trimethylamine- trimethylamine-N-oxide and hydrates thereof, more preferably N-methylmorpholine-N-oxide (NMMO) and N-methylmorpholine-N-oxide -Methylmorpholine-N-oxide compound hydrate, and the like.
The hydrate is not particularly limited as long as it is a hydrate of an N-oxide compound, but it may preferably be one of hydrates of an N-oxide compound of 0.5 to 2.5 equivalents.
The mixing ratio of the N-oxide compound and graphite is not particularly limited as long as it is usually used in the production of graphene. Preferably, the N-oxide compound may include 50 to 500,000 parts by weight of N-oxide compound per 100 parts by weight of graphite. Preferably 500 to 100,000 parts by weight of an N-oxide compound per 100 parts by weight of graphite. If less than 50 parts by weight of the N-oxide compound is mixed with 100 parts by weight of the graphite, the graphite is not sufficiently contacted with the solvent in the mixture, and as the concentration of the graphite increases, It is not preferable because peeling of graphite can not be easily expected.
Next, the third step of mixing the mixture of the second step with a dispersion treatment and a solvent is carried out. The solvent may include at least one selected from the group consisting of water, ethyl alcohol, methyl alcohol, ethylene glycol, isopropyl alcohol and acetone. Preferably, the solvent may be water.
The dispersion treatment is not particularly limited as long as it is a dispersion treatment that can be usually applied to a solvent containing a solute. Preferably, the dispersion treatment is carried out using a homogenizer, a homo-mix, an extruder , Microwave irradiation, corona discharge treatment, mixing, stirring, ultrasonic treatment, microwave irradiation, and corona discharge treatment.
Next, a fourth step of obtaining a graphene from the mixture of the third step is carried out. In order to obtain graphene from the mixture of the third step, a method including at least one of the group consisting of centrifugation, filtration and precipitation separation may be performed. According to one embodiment of the present invention, the obtained graphene can be dried and / or heat-treated.
The drying is not particularly limited as long as it is usually used in the graphene production process, but it may be carried out at 30 to 100 ° C for 10 to 40 hours.
Also, the graphene produced by the method for producing graphene of the present invention provides graphene having an average thickness of 0.4 to 4 nm and a carbon / hydrogen ratio (C / O ratio) of 20 to 500. The water dispersion having a water dispersion of 0.0000001 to 4 mg / ml is prepared by adding water to the graphene, measuring the amount of precipitate after centrifugation, and measuring the concentration of graphene remaining in the water.
Further, the present invention provides a polypyrrole composite in which graphene and polypyrrole are mixed to improve electrochemical characteristics.
Hereinafter, the present invention will be described in more detail with reference to the following examples. However, the following examples should not be construed as limiting the scope of the present invention, and should be construed to facilitate understanding of the present invention.
[Example]
Example 1. Preparation of graphene (eGPNc)
200 mL of cholorosulfonic acid (CSA) and 3 g of expanded graphite are placed in a round flask, soaked for one day, and then pre-treated by slowly dropping 70 mL of hydrogen peroxide (H 2 O 2 ). 500 ml (about 550 g) of N-methylmorpholine-N-oxide (NMMO) was put in a round cylinder and dissolved in an oil bath at 90 ° C, and graphite, And 3 g of synthetic powder (Aldrich Corp., <20 μm, synthetic) were added and sonicated at 750 W and 20 kHz for 3 hours using a horn-type sonicator (Vibracell, VCX-750) A
Then, the
A photograph of the above-described manufacturing process is shown in Fig.
Example 2. Composite of graphene and polypyrrole
The complex was prepared by polymerization of eGPNc obtained in Example 1 with polypyrrole, which is a typical conductive polymer.
Specifically, graphene and pyrrole were prepared by mixing graphene and pyrrole in water at 0, 0.5, 1, 2, 3, 4 and 5 wt% of graphene and then using a horn-type sonicator (Vibracell, VCX-750) Were prepared by treating ultrasonic waves of 750 W and 20 kHz for 3 hours. Then, graphene and pyrrole prepared in a 3 neck round flask with a nitrogen substitution at 0 to 4 ° C. were added, and
A photograph of the manufacturing process as described above is shown in Fig.
Comparative Example 1. Preparation of graphene (GPN)
Graphene (GPN) was prepared in the same manner as in Example 1, except that expanded graphite pretreated with CSA / H 2 O 2 was not included.
Comparative Example 2 Preparation of graphene (eGPN)
The procedure of Example 1 was repeated, except that CSA / H 2 O 2 pretreatment was performed on the expanded graphite, and the mixture was prepared by mixing the pretreated graphite with the N-oxide compound and the expanded graphite Graphene (eGPN) was prepared.
Comparative Example 3. Preparation of graphene (GPNc)
(GPNc) was prepared in the same manner as in Example 1, except that pretreatment of CSA / H 2 O 2 was performed on graphite, and the mixture was prepared by mixing the pretreated graphite with an N-oxide compound and graphite. .
The yields of graphene prepared from the above Examples and Comparative Examples are summarized in Table 1 below. Initial in the following Table 1 means the amount of graphite initially loaded, and Fianl means the amount of graphene finally obtained. Referring to Table 1, it can be confirmed that graphene (eGPNc) prepared by pretreating CSA / H 2 O 2 with expanded graphite has the highest yield.
The amount deposited (g)
The amount deposited (g)
Experimental Example 1. Measurement of water solubility
FIG. 2 is a photograph of graphene prepared in Examples and Comparative Examples of the present invention before and after treatment of 750 W and 20 kHz ultrasonic waves using Hitachi's S-4800 at 15 kV for 2 hours. Fig. 2 (a) shows water added with 0.001 mg of GO, and Fig. 2 (b) shows water added with 0.001 mg of eGPNc.
Referring to FIG. 2, eGPNc is also similar to the previously reported GO dispersibility and can be confirmed to be stable and well dispersed in water.
3 is a photograph before and after ultrasonication of graphene produced according to an embodiment of the present invention. 3 (b) is a photograph of 0.001 mg / ml of eGPNc added to water, and Fig. 3 (c) is a photograph of 0.01 mg / ml of GPN It is a photograph added to water.
Referring to FIG. 3, it can be confirmed that dispersion is stable and well after one day of ultrasonic treatment (dispersion treatment) as a whole.
Experimental Example 2. Measurement of dispersibility
4 is a graph showing the dispersibility of graphene prepared in Examples and Comparative Examples of the present invention. The dispersibility was determined by treating the prepared graphene at a concentration of 0.001 mg / ml in water using an ultrasonic type ultrasonic wave crusher for 2 hours at 750 W and 20 kHz, placing it in a cylindrical glass tube, by using a Lab scan charter ® Expert (Turbiscan Lab Expert ®) to measure the dispersion of graphene in the solvents.
Referring to FIG. 4, it can be seen that eGPNc has very little variation of about 2% even after one day after the initial ultrasonic treatment similar to GPN, and thus it is confirmed that the dispersion stability is very excellent .
Experimental Example 3.
Experimental Example 3-1: SEM image
FIG. 5 is a SEM image of graphene prepared according to an embodiment of the present invention, taken using a scanning electron microscope (SEM). The SEM image was prepared by adding the prepared graphene to a concentration of 0.001 mg / ml in water, treating ultrasonic waves of 750 W and 20 kHz for 2 hours using a mixed ultrasonic wave crusher, and measuring the S- 4800 < / RTI >
Referring to FIG. 5, it can be seen that there is a transparent graphene. If there is no graphene in one sheet, for example, when two or more graphenes are overlapped, the graphene is not transparent, It becomes darker or darker, so that the eGPNc identified by SEM can be confirmed to be a single graphene.
Experimental Example 3-2: Raman spectroscopic analysis
Figure 6 is a Raman spectrum of graphene prepared according to an embodiment of the present invention. Raman spectroscopy at 600 ~ 4,000 cm -1 wavelength range was performed in a backscattering geometry with a 532 ㎚ argon laser line stimulated by Ntegra spectra NT-MDT Raman spectrometer.
Referring to FIG. 6, the G peak (1578.4 cm -1 ) of eGPNc was found to be blue-shifted compared to graphite, and the 2D peak (2,711.8 cm -1 ) of GPM was red (Red-shift). This migration is because the interaction of the recombined eGPNc is weaker than the GO.
Experimental Example 3-3: X-ray photoelectron spectroscopy (XPS)
Figure 7 is a spectra measured by X-ray photoelectron spectroscopy of graphene prepared according to an embodiment of the present invention. The X-ray photoelectron spectroscopy was performed using a
Referring to FIG. 7, oxygen bonds can be confirmed. The element content% of
Experimental Example 3-4: X-ray diffraction
8 is an X-ray diffraction analysis of graphene prepared according to an embodiment of the present invention. The X-ray diffraction analysis was performed using a PLS-III U-SAXS beamline of the Pohang Accelerator Laboratory.
8, the distance between the graphene sheets becomes q = 18.6 ANGSTROM -1 (d-spacing = 3.39 ANGSTROM). The size of the graphene peak produced is smaller than that of the expanded graphite, New peaks appear at 18.0 Å -1 (d-spacing = 3.54 Å), which is the result of the expansion of the expanded graphite into the graphene sheet.
Experimental Example 4: Electrochemical Properties
Experimental Example 4-1: Cyclic voltammetry curve
10 is a CV graph of the graphene and polypyrrole composite prepared according to an embodiment of the present invention. The cyclic voltammetry was measured at a scanning speed of 1 mV / s in a range of -0.1 to 0.6 V using a potentiometer (PARSTAT 4000-PLUS, AMTEK Princeton Applied Research) of the composite of graphene and polypyrrole of Example 2.
Referring to FIG. 10, graphene was added in an amount of 0, 0.5, 1, 2, 3, 4 and 5 wt%, and the graphene-added polypyrrole composite was found to have a larger area than pure polypyrrole , The above results show that a polypyrrole composite having a high graphene content has a higher electric capacity.
EXPERIMENTAL EXAMPLE 4-2: Charge-discharge curve
11 shows the charge-discharge curve of the polypyrrole composite according to Example 2 of the present invention. -0.1 to 0.6 V at the same current of 0.1 A / g and discharging at -0.1 A / g.
Referring to FIG. 11, it can be seen that the more the graphene content is added in the content of 0, 1, 2, 3, 4, 5 wt%, the better the electric capacity.
EXPERIMENTAL EXAMPLE 4-3: Capacitance Life Evaluation
12 is a graph showing the evaluation of the capacitance lifetime of the polypyrrole composite according to Example 2 of the present invention. The capacitance lifetime was evaluated by measuring 1000 cy at a scan rate of 50 mV / s in the range of -0.1 to 0.6 V using samples of 0, 1, 2, and 3 wt%.
Referring to FIG. 12, it can be seen that as the graphene content increases, the lifetime of the capacitor increases further.
From the results of the above examples, it was found that the graphenes of the present invention improved the yield and water dispersibility, and in the case of the composite prepared by mixing with polypyrrole, the polypyrrole composite having a high content of graphene of the present invention had a higher electric capacity and It was confirmed that the lifetime of the electric capacity was better.
The present invention has been described with reference to the preferred embodiments. It will be understood by those skilled in the art that various changes in form and details may be made therein without departing from the spirit and scope of the invention as defined by the appended claims. Therefore, the disclosed embodiments should be considered in an illustrative rather than a restrictive sense. The scope of the present invention is defined by the appended claims rather than by the foregoing description, and all differences within the scope of equivalents thereof should be construed as being included in the present invention.
Claims (8)
Wherein the graphene content is 0.5 to 5 wt% based on the composite,
Wherein the composite has a current density of -0.15 to 0.15 A / g when measured at a scan rate of 1 mV / s in the range of -0.1 to 0.6 V. The graphene-
The dispersion treatment may be carried out using a homogenizer, a homo-mix, an extruder, a stir, a sonication, a microwave, and a corona discharge. Wherein the graphene-polypyrrole composite is a graphene-polypyrrole composite.
Wherein the solvent comprises at least one member selected from the group consisting of water, ethyl alcohol, methyl alcohol, ethylene glycol, isopropyl alcohol and acetone.
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| Wenbo Lu 외 8인, High-yield, large-scale production of few-layer graphene flakes within seconds: using chlorosulfonic acid and H2O2 as exfoliating agents, J. Mater. Chem., 2012, vol. 22, pp. 8775-8777 1부. * |
| Yun Liu 7인, Graphene/polypyrrole intercalating nanocomposites assupercapacitors electrode, Electrochimica Acta 2013, vol. 112, pp. 44-52 1부. * |
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