KR101799639B1 - Fabricating method for reduced graphene oxide composites and reduced graphene oxide composites fabricated by the method and supercapacitor having the reduced graphene oxide composites - Google Patents
Fabricating method for reduced graphene oxide composites and reduced graphene oxide composites fabricated by the method and supercapacitor having the reduced graphene oxide composites Download PDFInfo
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- KR101799639B1 KR101799639B1 KR1020150116075A KR20150116075A KR101799639B1 KR 101799639 B1 KR101799639 B1 KR 101799639B1 KR 1020150116075 A KR1020150116075 A KR 1020150116075A KR 20150116075 A KR20150116075 A KR 20150116075A KR 101799639 B1 KR101799639 B1 KR 101799639B1
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- C—CHEMISTRY; METALLURGY
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- C—CHEMISTRY; METALLURGY
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
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- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/13—Energy storage using capacitors
Abstract
The present invention relates to a method for producing a reduced graphene oxide composite, wherein in the process of preparing a reduced graphene oxide composite by injecting a microwave into a mixture of graphite oxide and a conductive agent, by using nano-reduced graphene oxide as the conductive agent , A reduced graphene oxide composite in which no foreign matter remains can be produced. In addition, since the reduced graphene oxide composite produced by such a manufacturing method does not contain any foreign material, it is possible to prevent the reduction of the ratio of the total active material due to the foreign material contained in the reducing graphene oxide in the conventional manufacturing process of the conventional super capacitor Thereby improving the performance of the super capacitor.
Description
The present invention relates to a method for producing a reduced graphene oxide composite, and more particularly, to a method for producing a reduced graphene oxide composite suitable as an active material of a supercapacitor and a reduced graphene oxide composite And a super capacitor including the same.
Supercapacitor, which shows a rapid increase in demand in recent years, is a power source that collects a lot of energy and emits high energy. It replaces or supplements lithium secondary battery, which can fulfill performance characteristics that conventional capacitors and secondary cells can not accommodate. It is the next generation energy storage device.
A representative example of such a super capacitor is an electric double layer capacitor (EDLC), which uses an electric double layer formed on the surface when a voltage is applied to the electrode, And a current collector applied thereon.
The electrode material for the supercapacitor is an environmentally friendly carbon material with its own safety properties. It is generally used as an activated carbon powder (ACP), a carbon nanotube (CNT), a graphite, a vapor grown carbon fiber Carbon nanofibers (carbon nanofibers) produced by carbonizing polymers such as carbon black, Grown Carbon Fiber, VGCF, carbon aerogels, polyacrylonitrile (PAN) and polyvinylidenefluoride (PVdF) Nano Fiber, CNF) and Activated Carbon Nano Fiber (ACNF) are used. As the specific surface area of the carbon material is larger, it is known that the specific capacity of the supercapacitor is increased. In recent years, Efforts have been made to develop a graphene electrode having a two-dimensional (2D) structure having electrical conductivity.
In order to produce the graphene electrode having such a two-dimensional structure, the graphene may be produced by a micromechanical method, a chemical vapor deposition (CVD) method, an oxidation-reduction method and oxidation-reduction. Among them, graphite is oxidized to oxidize graphite, and each layer of graphite oxide is separated in a solution. The graphene oxide thus obtained is reduced again, The method of obtaining reduced graphene oxide has the advantage of obtaining a large amount of graphene based material.
In order to produce the reduced graphene oxide, a conductive agent having a high electrical conductivity is added in addition to the carbon material, and Super-P, acetylene black or the like is used as the conductive agent .
However, conventionally, the conductive agent added to the final material of the reduced graphene oxide (RGO) is left as it is, but the remaining conductive agent is difficult to separate and usually used as it is in the state of remaining conductive agent.
In addition, since the conductive agent is added in the process of forming the electrode, the amount of the pure active material is reduced and the density of the electrode active material is lowered. When the density of the electrode active material is low, the resistance generally increases and the charge capacity decreases.
Therefore, it is an object of the present invention to provide a reduced graphene oxide composite which does not cause a reduction in the proportion of the active material due to a conductive agent remaining using a reduced graphene oxide as an active material in the process of manufacturing an electrode of a supercapacitor, And a manufacturing method thereof.
It is still another object of the present invention to provide a reduced graphene oxide composite in which no foreign matter such as a conductive agent produced by the reduced graphene oxide composite manufacturing method remains, and a super capacitor including the same.
In order to accomplish the above object, a reduced graphene oxide composite according to the present invention comprises a graphite oxide forming step (S110) of oxidizing graphite using an acid to form a graphite oxide (S110) (S130) of mixing a nano-reduced graphene oxide (N-RGO) (S130), and a reducing step (S140) of forming a reduced graphene oxide complex by injecting microwave into the compound.
(N-RGO) preparation step (S120) before the mixture forming step (S130), and the nano-reduced graphene oxide preparation step may include a step of preparing nano graphite having a particle size of about 20 to 100 nm (S121) of oxidizing nano-graphite to form nano graphite oxide (S121), and forming nano-reduced graphene oxide (N-RGO) by injecting microwave into the nano graphite oxide To prepare nano-reduced graphene oxide (N-RGO).
At this time, it is preferable that the nano-reduced graphene oxide (N-RGO) serves as a conductive agent in the microwave reduction, and the particle diameter is preferably in the range of 20 to 100 nm.
In the step of producing the mixture (S130), the graphite oxide and nano-reduced graphene oxide (N-RGO) may be mixed in a weight ratio of 9: 1.
Meanwhile, in the reducing step (S140), a 700W microwave is injected for 1 minute in a glove box filled with an inert gas to form a reduced graphene oxide composite, and after the reducing step, And further injecting microwaves to remove residual groups.
The reduced graphene oxide composite of the present invention is produced by the above production method and is characterized in that no foreign matter remains in the reduced graphene oxide composite.
Also, the supercapacitor according to the present invention is a supercapacitor composed of cells having an anode and a cathode, wherein one of the anode and the cathode is an electrode active material and comprises the reduced graphene oxide composite of the present invention described above, The graphene oxide composite is prepared by including nano-reduced graphene oxide (N-RGO) as a conductive material.
INDUSTRIAL APPLICABILITY The present invention constituted as described above can be achieved by using nano-reduced graphene oxide (N-RGO) as a conductive agent in the process of producing a reduced graphene oxide composite using graphite oxide, reducing graphene oxide There is an effect that a composite can be produced.
Also, by preparing a reduced graphene oxide composite in which no noble residue remains using nano-reduced graphene oxide (N-RGO) as a conductive agent, it is possible to reduce the amount of foreign particles contained in reduced graphene oxide in a conventional general super- There is an effect of improving the performance of the supercapacitor by preventing the problem that the ratio of the total electrode active material is reduced.
FIG. 1 is a flow chart of a method for producing a reduced graphene oxide composite according to an embodiment of the present invention.
2 is a scanning electron microscope (SEM) photograph of the composite nano-reduced graphene oxide composite (CN-RGO) of Example 1. Fig.
3 is a transmission electron microscope (TEM) photograph of the composite nano-reduced graphene oxide composite (CN-RGO) of Example 1. Fig.
4 is a scanning electron microscope (SEM) photograph of a general reduced graphene oxide composite (MS-RGO) of Comparative Example 1. Fig.
5 is a transmission electron microscope (TEM) photograph of the general reduced graphene oxide composite (MS-RGO) of Comparative Example 1. Fig.
6 is a scanning electron microscope (SEM) photograph of a general nano-reduced graphene oxide composite (NS-RGO) of Comparative Example 2. Fig.
7 is a transmission electron microscope (TEM) photograph of the general nano-reduced graphene oxide composite (NS-RGO) of Comparative Example 2. Fig.
8 is a scanning electron microscope (SEM) photograph of the complex-reduced graphene oxide composite (CS-RGO) of Comparative Example 3. Fig.
9 is a transmission electron microscope (TEM) photograph of the complex-reduced graphene oxide composite of Comparative Example 3. Fig.
10 is a pore distribution result obtained by measuring the composite nano-reduced graphene oxide composite (CN-RGO) of Example 1 by the non-local density functional theory (NLDFT) method.
11 is a pore distribution obtained by measuring the general reduced graphene oxide composite (MS-RGO) of Comparative Example 1 by the non-local density functional theory (NLDFT) method.
12 shows the results of void distribution obtained by measuring the general nano-reduced graphene oxide composite (NS-RGO) of Comparative Example 2 by the non-local density functional theory (NLDFT) method.
FIG. 13 shows the result of pore distribution obtained by measuring the composite reduced graphene oxide composite (CS-RGO) of Comparative Example 3 by the non-local density functional theory (NLDFT) method.
14 is a current-potential curve measured for the composite nano-graphene oxide composite (CN-RGO) of Example 1. Fig.
15 is a current-potential curve measured for the general reduced graphene oxide composite (MS-RGO) of Comparative Example 1. Fig.
16 is a current-potential curve measured for the general nano-reduced graphene oxide composite (NS-RGO) of Comparative Example 2. Fig.
17 is a current-potential curve measured for the complex-reduced graphene oxide composite (CS-RGO) of Comparative Example 3. Fig.
Hereinafter, preferred embodiments of the present invention will be described, and the embodiments described herein can be embodied in many different forms without departing from the scope of the present invention. The present invention is not limited to the embodiments.
As shown in FIG. 1, a method for producing a reduced graphene oxide composite as an active material of a supercapacitor according to the present invention includes the steps of oxidizing graphite using an acid to produce graphite oxide (GO) Forming a mixture of graphite oxide and nano-reduced graphene oxide (N-RGO) (S130), and forming the mixture (S130) And a reducing step (S140) of forming a reduced graphene oxide complex by injecting microwave into the nanoparticles.
The graphite oxide (GO) formation step (S110) is a step of oxidizing graphite by an acid treatment by a chemical method. Specifically, 3 g of graphite is dissolved in 360 ml of sulfuric acid (H 2 SO 4 ) And phosphoric acid (H 3 PO 4 ), and the mixture is stirred for 30 minutes. Thereafter, the graphite oxide solution stirred in an ice bath at 0 ° C was cooled for about 10 minutes, 18 g of potassium permanganate (KMnO 4 ) was slowly added, and the mixture was stirred for another 30 minutes. The stirred graphite oxide solution The reaction is allowed to proceed at 55 占 폚 for 24 hours. In order to remove excess potassium permanganate (KMnO 4 ) added to the graphite oxide solution that has been reacted, hydrogen peroxide (H 2 O 2 ) was added and the potassium permanganate was removed by adding in a range of 3 to 18 mL until the color turned yellow I will.
Then, the graphite oxide solution from which potassium permanganate was removed was added to a solution prepared by mixing 100 ml of hydrochloric acid (HCl), 100 ml of ethanol and 100 ml of water (H 2 O) and stirred for 1 hour. After stirring the mixture for 1 hour, Is not less than 5, and then dried to obtain graphite oxide.
As the graphite, nano-graphite having a particle size of about 20 to 100 nm and having a nano-scale size by physical methods can be used for ordinary graphite and graphite having a particle size of about 4 탆, Nano graphite oxide (hereinafter also referred to as N-GO) prepared using 3 g of nano graphite alone, 2 g of common graphite and 2 g of nano graphite prepared by using 3 g of ordinary graphite alone (hereinafter referred to as M-GO) (Hereinafter, also referred to as C-GO) prepared by mixing 1 g of a graphite oxide in powder form.
In the mixture forming step (S130), a mixture may be formed by mixing the powdery graphite oxide formed in the graphite oxide forming step and the conductive agent in a weight ratio of 9: 1. As the conductive agent, Super-P and nano-reduced graphene oxide (N-RGO) having a particle size of about 20 to 100 nm prepared according to the present invention can be used. Acetylene black, carbon black, carbon nanotubes, and activated carbon, which are widely used as a general conductive agent, can be used.
The 'nano-reduced graphene oxide (N-RGO)' described here is prepared separately from the manufacturing process of the reduced graphene oxide composite of the present invention. The nano-reduced graphene oxide N-RGO) will be described in detail with reference to an example of the present invention to be described later.
The graphite oxide may be any one selected from among general graphite oxide (M-GO), nano graphite oxide (N-GO) and composite graphite oxide (C-GO) .
The reduction step (S140) is a step of forming a reduced graphene oxide composite (RGO) from the mixture. The mixture is immersed in a 1000 ml beaker and then heated in a glove box filled with argon (Ar) a reduced graphene oxide composite (RGO) exhibiting black color can be obtained by reducing the graphite oxide dispersed in the mixture by injecting a microwave for 1 minute. Here, when the microwave is scanned, the graphite oxide is peeled and reduced, and the color of the mixture changes from yellow to black.
In order to further remove functional groups such as hydroxy, epoxy, and ketone remaining in the reduced graphene oxide after the reducing step (S140), a microwave of 100 W was further injected for about 6 minutes to obtain a final reduced graphene oxide composite (RGO) can be produced.
Meanwhile, the nano-reducing graphene oxide (N-RGO) preparation step (S120) of the present invention is performed before the mixture forming step, and a nano-graphite having a particle size of about 20 to 100 nm is used as the graphite (S130) and a reduction step (S140) according to an embodiment of the present invention, except that the graphite oxide is reduced without using a conductive agent.
More specifically, the nano-graphite is oxidized by the same method as that for forming the graphite oxide (GO) using a nano-graphite having a particle diameter of about 20 to 100 nm to form a nano graphite oxide (N- (N-RGO) by injecting 700W of microwave for 1 minute without adding a conductive agent to the formed nano graphite oxide (N-GO) Forming a nano-reduced graphene oxide (N-RGO).
Hereinafter, the present invention will be described in detail with reference to the accompanying drawings. The following examples are provided for illustrative purposes only, and the scope of the present invention is not limited thereto.
In Example 1 of the present invention, the composite graphite oxide (C-GO) prepared by mixing ordinary graphite and nano graphite as the graphite oxide produced in the above-mentioned graphite oxide forming step and the nano-reduced graphene oxide (N-RGO ) Was mixed at a ratio of 9: 1 to form a mixture. In a glove box filled with argon (Ar) gas, 700 W of microwave was injected for 1 minute, and furthermore, 100 W of microwave was supplied for 6 minutes (CN-RGO), which is a final product, is prepared by injection.
Comparative Example 1 was carried out in the same manner as in Example 1, except that normal graphite oxide (M-GO) prepared using only graphite oxide as the graphite oxide and Super-P as the conductive agent were used to prepare a general reduced graphene oxide composite (MS-RGO).
Comparative Example 2 was the same as Example 1 except that nano graphite oxide (N-GO) prepared using only nano graphite having a particle size of about 20 to 100 nm as graphite oxide and Super-P as a conductive agent were used. To produce a general nano-reduced graphene oxide composite (NS-RGO).
In Comparative Example 3, the same process as in Example 1 was carried out except that a composite graphite oxide (C-GO) and Super-P, which were prepared by mixing normal graphite and nano graphite as graphite oxide, were used, Graphene oxide complex (CS-RGO).
FIGS. 2 to 9 are graphs showing the results of a scanning electron microscope (SEM) and a transmission electron microscope (TEM) of the reduced graphene oxide composite of Example 1 and Comparative Examples 1 to 3 according to the present invention It can be seen from the photographed images that the reduced graphene oxide composite in the form of a peeled two-dimensional structure was produced in all the Examples and Comparative Examples as shown in the figure.
Particularly, in the composite nano-reduced graphene oxide composite (CN-RGO) of Example 1, no residual particles were observed as shown in Figs. 2 and 3, but in Comparative Examples 1 to 3, The general reduced graphene oxide composite (MS-RGO) of FIG. 5, the general nano-reduced graphene oxide (NS-RGO) of FIGS. 6 and 7 and the complex reduced graphene oxide composite (CS- The super-P particles used as the conductive agent remained and adsorbed on the surface of the reduced graphene oxide.
10 to 13 show the results of measurement of the differential pore volume (dv) distribution according to the pore width of the reduced graphene oxide composite of Example 1 and Comparative Examples 1 to 3, (Brunauer Emmett Teller, BET) is a pore size distribution obtained by the Non-Local Density Functional Theory (NLDFT) method using a pore model. Can be measured.
Fig. 10 shows the results of measurement of pore distribution for the composite nano-reduced graphene oxide composite (CN-RGO) of Example 1, and the specific surface area (BET) value measured therefrom is 431.14 m 2 / g.
Fig. 11 shows the results of measurement of pore distribution for the general reduced graphene oxide composite (MS-RGO) of Comparative Example 1, and the specific surface area (BET) value measured therefrom is 476.89 m 2 / g.
Fig. 12 shows the results of measurement of pore distribution for the general nano-reduced graphene oxide composite (NS-RGO) of Comparative Example 2, and the specific surface area (BET) value measured therefrom was 271.52 m 2 / g.
Fig. 13 shows the results of measurement of pore distribution for the complex-reduced graphene oxide composite (CS-RGO) of Comparative Example 3, and the specific surface area (BET) m < 2 > / g.
Meanwhile, the supercapacitor formed in the present invention is formed as a cell which is disposed between an anode and a cathode and includes a separator for electrically separating the anode and the cathode, wherein the anode and the cathode are made of a metallic current collector and the above- The reduced graphene oxide composite produced by the method of the present invention includes an electrode active material, and the contact material may be used in the form of a metal foil.
Specifically, the composite nano-reduced graphene oxide composite (CN-RGO), the general reduced graphene oxide composite (MS-RGO), and the general nano-reduced graphene oxide composite prepared in Example 1 and Comparative Examples 1 to 3 NS-RGO) and composite reducing graphene oxide composite (CS-RGO) as active materials, and the weight ratio of the active material, the conductive agent and the binder is uniformly mixed at 8: 1: 1 to prepare an electrode slurry. As the conductive agent, Super-P may be used. As the binder, poly (vinylidenefluoride-co-hexafluoropropylene) (PVDF) may be used.
The electrode slurry thus prepared was coated on an aluminum foil with a thickness of 30 탆 and dried in a vacuum oven at 120 캜 for 12 hours to prepare an electrode. Using SK separator as a separation membrane, 2032 coin-type supercapacitors are manufactured according to the capacitor manufacturing process.
In order to evaluate the electrochemical performance of the 2032 coin type supercapacitor manufactured using the reduced graphene oxide complex as an electrode active material, the electrochemical performance of the 2032 coin type supercapacitor was evaluated by using a circulating electric potential meter for 2 mV / s and 5 mV / s in the range of 0 to 2.5 V Obtain a Current-Potential curve. Capacitance performance can be calculated from the discharge time of the non-storage capacity and the value of the applied current through the graph of the measured circulation potential curve.
Fig. 14 shows a circulating potential curve of a supercapacitor using the composite nano-reduced graphene oxide composite (CN-RGO) of Example 1 as an electrode material. The specific capacitance was 102.1 F / g at 2 mV / And it was measured to be 96.7 F / g at 5 mV.
15 shows a circulating potential curve of a supercapacitor using the general reduced graphene oxide composite (MS-RGO) of Comparative Example 1 as an electrode material, and the specific capacitance is 101.1 F / g at 2 mV / s And 83.4 F / g at 5 mV / s.
Fig. 16 shows a circulation potential curve of a supercapacitor using the general nano-reduced graphene oxide composite (NS-RGO) of Comparative Example 2 as an electrode material. The specific capacitance was 95.4 F / g at 2 mV, It was measured to be 75.7 F / g at 5 mV.
17 shows a circulation potential curve of a supercapacitor using the complex-reduced graphene oxide composite (CS-RGO) of Comparative Example 3 as an electrode material. The specific capacitance is 91.2 F / g at 2 mV, Was measured to be 66.98 F / g.
As a result, it was confirmed that the composite nano-reduced graphene oxide composite (CN-RGO) of Example 1 had an increase in the specific stock amount as compared with Comparative Examples 1 to 3. Particularly, as in Example 1, (MS-RGO) using a general graphite oxide (M-GO) as well as a composite reduced graphene oxide composite (CS-RGO) using a graphite oxide / s, the rate of increase of the non-storage capacity is higher at 5 mV / s.
While the present invention has been particularly shown and described with reference to preferred embodiments thereof, it is to be understood that the invention is not limited to the disclosed embodiments, but, on the contrary, is intended to cover various modifications and equivalent arrangements included within the spirit and scope of the appended claims. Those skilled in the art will understand. Therefore, the scope of protection of the present invention should be construed not only in the specific embodiments but also in the scope of claims, and all technical ideas within the scope of the same shall be construed as being included in the scope of the present invention.
Claims (7)
A graphite oxide forming step of oxidizing graphite using an acid to form graphite oxide (GO);
Mixing the graphite oxide and the nano-reduced graphene oxide (N-RGO) in a weight ratio of 9: 1; And
And a reducing step of injecting 700W of microwave in a glove box filled with an inert gas for 1 minute to form a reduced graphene oxide composite,
Further comprising the step of injecting microwaves to remove residual groups remaining in the reduced graphene oxide composite after the reducing step. ≪ RTI ID = 0.0 > 15. < / RTI >
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| KR20200114793A (en) | 2019-03-29 | 2020-10-07 | 한국에너지기술연구원 | Method for manufacturing graphene composite, eletrode active material and secondary battery including the same |
| KR102323879B1 (en) * | 2021-03-08 | 2021-11-09 | 박진규 | Method of repairing that provides electromagnetic shielding in concrete structures |
| KR20230063400A (en) | 2021-11-02 | 2023-05-09 | 한국전기연구원 | Reduced graphene oxide for secondary batteries, its manufacturing method, electrodes and secondary batteries using the same |
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| WO2020049336A1 (en) * | 2018-09-05 | 2020-03-12 | Arcelormittal | A method for the manufacture of microwave-reduced graphene oxide |
| KR102523378B1 (en) * | 2021-07-07 | 2023-04-19 | 제주대학교 산학협력단 | Graphene-based two-dimensional heterostructure supercapacitor and manufacturing method thereof |
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| KR20200114793A (en) | 2019-03-29 | 2020-10-07 | 한국에너지기술연구원 | Method for manufacturing graphene composite, eletrode active material and secondary battery including the same |
| KR102323879B1 (en) * | 2021-03-08 | 2021-11-09 | 박진규 | Method of repairing that provides electromagnetic shielding in concrete structures |
| KR20230063400A (en) | 2021-11-02 | 2023-05-09 | 한국전기연구원 | Reduced graphene oxide for secondary batteries, its manufacturing method, electrodes and secondary batteries using the same |
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