KR20170022869A - Fabricating method for graphene composites including post-treatment of sonification, fabricating method for active material and supercapacitor by the same - Google Patents
Fabricating method for graphene composites including post-treatment of sonification, fabricating method for active material and supercapacitor by the same Download PDFInfo
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- KR20170022869A KR20170022869A KR1020160086201A KR20160086201A KR20170022869A KR 20170022869 A KR20170022869 A KR 20170022869A KR 1020160086201 A KR1020160086201 A KR 1020160086201A KR 20160086201 A KR20160086201 A KR 20160086201A KR 20170022869 A KR20170022869 A KR 20170022869A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/08—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
- B01J19/10—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor employing sonic or ultrasonic vibrations
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/182—Graphene
- C01B32/184—Preparation
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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
- H01G11/30—Electrodes characterised by their material
- H01G11/32—Carbon-based
- H01G11/34—Carbon-based characterised by carbonisation or activation of carbon
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- 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
Description
BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method of manufacturing a graphene composite, and more particularly, to a method of manufacturing a graphene composite suitable as an active material of a supercapacitor.
Recently, there is a growing interest in supercapacitors, a next-generation energy storage device that is replacing or supplementing lithium-ion secondary batteries with a rapid increase in demand. To develop a 2D-structured graphene electrode having a large specific surface area and a high electrical conductivity Efforts are continuing.
A method of oxidizing graphite to oxidize graphite to separate each layer of graphite oxide in solution and to obtain a reduced graphene oxide by reducing the graphene oxide thus obtained again Has the advantage of obtaining a large amount of graphene-based materials.
As a technique developed thereafter, there is a method of peeling off graphite oxide by a microwave radiation technique, and graphite oxide having a particle size of about 150 탆 m as an initial starting material for producing graphite oxide use.
In order to produce reduced graphene oxide (RGO) by applying a microwave to the graphite oxide, a conducting agent having a high electrical conductivity has to be added. Conventionally, super-P (R), acetylene And about 10% of conductive material such as black (acetylene black) was used.
The RGO produced by this method has the conductive material remaining in the final material, but it is difficult to separate and is usually used as it is, and the conductive material is added in the process of making the slurry electrode using RGO as the active material.
SUMMARY OF THE INVENTION It is an object of the present invention to provide a method of manufacturing a graphene composite in which the efficiency of a supercapacitor is improved.
According to another aspect of the present invention, there is provided a method of manufacturing a graphene composite including an ultrasonic mill post-treatment process, the method comprising: injecting a microwave into a mixture of graphite oxide and a conductive material; Dispersing the resultant obtained in the above step in a liquid and ultrasonically pulverizing it; And a step of lyophilizing the obtained ultrasonic pulverized particles.
The present invention has developed a method for producing a reduced graphene oxide using microwaves. It is a method of manufacturing a graphene composite which improves the performance of a capacitor when used as an active material by adding a crushing and freeze- Lt; / RTI > The reduced graphene oxide produced by microwave irradiation is ultrasonically pulverized and lyophilized to uniformly disperse the reduced graphene oxide evenly, thereby improving the performance of the active material. This is because the problems caused by the structural difference between the conductive agent used in the synthesis of RGO and the active material and the graphene oxide in the 2D structure can be solved.
Preferably, the ultrasonic pulverizing process is performed by applying an ultrasonic wave having a frequency of 20 kHz or more to an output of 350 W or more for 1 hour or more, and the freeze-drying process is preferably performed at a temperature of -45 or less for 20 hours or more.
The graphite oxide is obtained by oxidizing graphite, and the graphite powder is oxidized. The size of the graphite oxide is not particularly limited, and it is possible to use a general graphite powder having a particle diameter of several micrometers and a graphite powder having a particle size smaller by nanometer by processing it. These may be mixed and used.
The conductive material is preferably at least one material selected from super-P, graphene oxide, acetylene black and ketjen black.
It is preferable that the microwave scanning process is performed in an inert gas atmosphere at an output of 600 W or more for a time of 50 seconds or more.
The graphene composite according to another aspect of the present invention is characterized by being manufactured by the above-described method.
The reduced graphene oxide contained in the graphene composite produced by the method of the present invention is the same as the conventional reduced graphene oxide in terms of material, but in view of the microstructure considering the physical properties such as particle size, particle size distribution and dispersibility, Lt; RTI ID = 0.0 > of graphene oxide. ≪ / RTI > As described above, the reduced graphene oxide included in the graphene composite of the present invention is different from the conventional reduced graphene oxide in particle size, particle size distribution, and dispersibility, but it can be expressed specifically with respect to the graphene composite containing the reduced graphene oxide There is no standard, so it is expressed in this specification as the difference according to the manufacturing method.
According to an aspect of the present invention, there is provided a method of manufacturing an active material for a supercapacitor, comprising: injecting a microwave into a mixture of graphite oxide and a conductive material; Dispersing the resultant obtained in the above step in a liquid and ultrasonically pulverizing it; Obtaining ultrasonic pulverized particles and lyophilization; And a step of mixing the activated carbon for active material with a graphene composite containing lyophilized reduced graphene oxide.
At this time, it is preferable to use spherical activated carbon as the active carbon for the active material, and more specifically, AC0830 activated carbon is preferably used.
An active material according to another embodiment of the present invention is characterized by being manufactured by the above-described method.
The active material produced by the method of the present invention differs from the conventional active material in its properties as an active material due to the physical properties of the reduced graphene oxide contained in the graphene composite used for the active material. However, since there is no criterion that can express this, it is expressed in this specification as the difference according to the manufacturing method.
According to another aspect of the present invention, there is provided a method of manufacturing a supercapacitor, comprising: preparing a cathode current collector and an anode current collector; Attaching an active material to surfaces of the positive electrode collector and the negative electrode collector; And packaging the positive electrode current collector and the negative electrode current collector, the separator separating the positive electrode and the negative electrode, and the electrolyte having the active material attached thereto, and manufacturing the active material using the active material manufacturing method.
The supercapacitor according to another embodiment of the present invention is manufactured by the above-described manufacturing method. The difference in the process of manufacturing the graphene composite containing the reduced graphene active material used in the active material causes the electrochemical characteristics Which is different from the conventional super capacitor. However, since there is no criterion that can express this, it is expressed in this specification as the difference according to the manufacturing method.
The present invention constructed as described above is characterized in that by adding a post-treatment process to a method of producing a graphene composite containing reduced graphene oxide using graphite oxide, graphene having improved bonding property to activated carbon used for producing active material There is an effect that a composite can be manufactured.
Further, there is an effect of providing an active material and a super capacitor by using a post-treated graphene composite material, thereby providing a supercapacitor with thinner and more densely applied active material and improved performance.
1 is an electron micrograph of a sample of a RGO-containing graphene composite without a post-treatment process according to the present embodiment.
FIG. 2 is an electron micrograph of a sample of a RGO-containing graphene composite material subjected to an ultrasonic pulverization process in a post-treatment process according to the present embodiment.
FIG. 3 is an electron micrograph of a sample of the RGO-containing graphene composite performed to the freeze-drying process according to the present embodiment.
4 is an electron micrograph of AC0830 activated carbon used in this embodiment.
5 to 7 are electron micrographs of the AC-RGO active material prepared according to the present embodiment.
8 shows the results of measuring the capacitance of the active material of the present embodiment and the active material of the comparative example.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS Referring to the accompanying drawings, embodiments of the present invention will be described in detail.
Graphite oxide synthesis
3 g of graphite, 360 ml of H 2 SO 4 and 40 ml of H 3 PO 4 are mixed and stirred for 30 minutes. After cooling for about 10 minutes under an ice bath, 18 g of KMNO 4 is slowly added and stirred for 30 minutes, and the stirred sample is allowed to react at 55 ° C for 24 hours. The graphite of the present embodiment uses commercially available graphite powder which is generally used without additional finishing, and the average particle size of the powder is about 4 탆.
To remove excess KMNO 4 from the reaction-completed sample, add H 2 O 2 in small increments ranging from 3 to 18 ml until the color of the sample turns yellow.
100 ml of HCl, 100 ml of ethanol and 100 ml of H 2 O were mixed and stirred for 1 hour. The mixture was added to the above-mentioned sample and stirred for 1 hour.
After washing with distilled water until the pH reaches 5 or above, the GO powder is obtained by drying.
Creation of graphene composites containing reduced graphene oxide (RGO)
The synthesized GO powder and super-P, which is a conductive material, are mixed at a ratio of 9: 1 and placed in a 1000 ml beaker. Subsequently, the internal conditions are replaced by Ar using a glove box.
Thereafter, a microwave of 700 W is injected for 1 minute in a glove box in an inert gas atmosphere to reduce the GO powder. When the color of the sample changes from yellow to black, it is peeled off. In order to further remove the functional groups remaining after the reduction process, a microwave of 100 W is injected for about 6 minutes to mix the final product, RGO, with the super- Graphene composite. Hereinafter, the graphene composite refers to a material in which a material used as a conductive material is combined with RGO prepared by injecting a microwave. At this time, in this embodiment, super-P is used as a conductive material for RGO production, but the present invention is not limited thereto.
Post-treatment process for graphene composites
In the above procedure, 3 g of the RGO-containing graphene composite produced by scanning the microwave is dispersed in 800 ml of distilled water to form a colloid solution, and a pulverization process is performed by applying ultrasonic waves to the colloid solution. The ultrasonic pulverizing process was carried out at a power of 410 W for 2 hours by using a pulverizer having a frequency of 40 kHz.
The colloidal solution after ultrasonication is centrifuged at 9000 rpm for 10 minutes and separated into supernatant and precipitate. The supernatant is removed and a precipitate is obtained and dried in a lyophilization process. The freeze-drying process was carried out at -55 ° C for 24 hours.
FIG. 1 is an electron micrograph of a sample of a RGO-containing graphene composite without performing a post-treatment process according to the present embodiment. FIG. 2 is a graph showing the RGO content of the RGO- FIG. 3 is an electron micrograph of a sample of the RGO-containing graphene composite performed up to the freeze-drying process according to the present embodiment. FIG.
As shown in the figure, the RGO contained in the graphene composite not subjected to the post-treatment has a large size in the form of aggregate, but when the ultrasonic pulverization process is performed by the post-treatment process, the RGO becomes small and the lyophilization process is performed You can see that it spreads evenly.
In FIG. 1, RGO agglomerates having a layer thickness of 14 to 20 nm are formed in a honeycomb shape having a size of about 10 탆, but in FIG. 3, the agglomerates have a size of 1 to 2 탆 and a layer thickness is 5 to 9 nm It can be seen that the distribution of the particle size becomes narrower and the thickness of the layer becomes thinner. It can be seen that the RGO is evenly dispersed.
Composite active material manufacturing
The active material was prepared using RGO - containing graphene composites which had been subjected to a post - treatment process.
Two kinds of active materials were prepared by mixing AC0830 activated carbon and RGO containing graphene composites. Specifically, RGO - containing graphene complex and activated carbon were prepared at a weight ratio of 1: 1, Lt; / RTI >
Hereinafter, an AC-RGO is used to denote an active material produced using AC0830 activated carbon.
FIG. 4 is an electron micrograph of AC0830 activated carbon used in this embodiment, and FIGS. 5 to 7 are electron micrographs of AC-RGO active material prepared according to this embodiment.
As shown in the figure, since the RGO-containing graphene composite of the present embodiment subjected to a post-treatment process has a small particle size and is evenly dispersed, it can be confirmed that the activated carbon and RGO are evenly mixed by mixing with AC0830 activated carbon. Further, it can be confirmed that the adhesion between the activated carbon and the RGO is improved by increasing the uniformity of the RGO particles.
As described above, when the active carbon and the RGO are uniformly mixed and the adhesiveness is increased, the same amount can be applied more thinly in the process of applying the active material to the current collector, and more active materials can be obtained with the same thickness. In addition, since the adhesion between activated carbon and RGO is excellent, it is expected that the electrode will be stabilized and the conductivity will be increased to improve the storage performance.
Electrochemical Characterization
The active material prepared in the previous step and super-P and polyvinylidene fluoride (PVDF) were mixed in an amount of 8: 1: 1 and applied to an aluminum foil having a thickness of 30 탆, followed by drying in a vacuum oven at 120 캜 for 12 hours , And then a coin cell (2032 kit) was prepared.
8 shows the results of measurement of the non-discharge capacity with respect to the active material of this embodiment and the active material of the comparative example.
The active material (Sonic AC_RGO) produced according to this embodiment is designated as "Sonic ACrGO (Sonic) ", and the remainder corresponds to a comparative example.
Specifically, ultrasonic pulverization was performed as post-treatment on graphene oxide. However, only the active material (Only Sonic-rGO) which did not constitute the complex active material was designated as "Only_rGO", and AC0830 active carbon and graphene oxide were used as the composite material. The non-Sonic AC-RGO (non-Sonic AC-RGO) as post-treatment is designated as "NS_ACRGO" and the active material marked as "Only_NSrGO" )to be.
As shown in the figure, all of the active materials of the comparative examples exhibited a lower non-reactive capacity than the pure AC0830 active carbon alone (Only ACO830), but the active material prepared according to this example exhibited an improved non-reactive capacity than AC0830 active carbon alone.
This indicates that the active material of the present invention exhibits excellent noncircuitable capacity due to the combination of the two features that constitute the complex active material with spherical activated carbon for performing the post-treatment process of reduced graphene oxide. On the other hand, the improved effect exhibited by the active material of the present invention is attributable to the effect of the post-treatment of the graphene oxide and the effect of composing the complex active material with the active carbon for the active material and the effect The results are even better.
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 (12)
Dispersing the resultant obtained in the above step in a liquid and ultrasonically pulverizing it; And
A method for preparing a graphene composite comprising the steps of: ultrasonic pulverizing particles obtained and lyophilized.
Wherein the ultrasonic pulverizing step is performed by applying an ultrasonic wave at an output of 350 W or more for 1 hour or more.
Wherein the freeze-drying process is performed at a temperature of -45 캜 or lower for 20 hours or longer.
Characterized in that the graphite oxide is obtained by oxidizing graphite powder. ≪ RTI ID = 0.0 > 8. < / RTI >
Wherein the conductive material is at least one selected from the group consisting of super-P, graphene oxide, acetylene black, and ketjen black.
Wherein the microwave scanning process is performed in an inert gas atmosphere at an output of 600 W or more for a time of 50 seconds or more.
Injecting a microwave into a mixture of graphite oxide and conductive material;
Dispersing the resultant obtained in the above step in a liquid and ultrasonically pulverizing it;
Obtaining ultrasonic pulverized particles and lyophilization; And
And mixing the graphene composite containing the freeze-dried reduced graphene oxide with the activated carbon for the active material.
Wherein the activated carbon for the active material is spherical.
Preparing a positive electrode current collector and a negative electrode current collector;
Attaching an active material to surfaces of the positive electrode collector and the negative electrode collector; And
And packaging the positive electrode current collector and the negative electrode current collector with the active material attached thereto, the separator separating the positive electrode and the negative electrode, and the electrolyte,
The method of manufacturing a super capacitor according to claim 8, wherein the active material is manufactured.
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| US15/237,950 US10176932B2 (en) | 2015-08-19 | 2016-08-16 | Method of manufacturing graphene composite including ultrasonic-wave pulverization post-treatment process and method of manufacturing active material using the same |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR101970134B1 (en) * | 2018-04-16 | 2019-04-18 | 한국지질자원연구원 | Electrode comprising activated carbon and graphene sheet, method of manufacturing the electrode, and super capacitor comprising the electrode |
| KR102157182B1 (en) * | 2020-04-29 | 2020-09-17 | 한국지질자원연구원 | Electrode for supercapacitor comprising activated carbon and reduced graphene oxide, method of manufacturing the electrode, and super capacitor comprising the electrode |
| KR20200114793A (en) * | 2019-03-29 | 2020-10-07 | 한국에너지기술연구원 | Method for manufacturing graphene composite, eletrode active material and secondary battery including the same |
| CN112320796A (en) * | 2020-10-30 | 2021-02-05 | 浙江锂宸新材料科技有限公司 | Preparation method for simply increasing graphite layer spacing |
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| KR20150015151A (en) * | 2013-07-31 | 2015-02-10 | 한국에너지기술연구원 | Manufacturing method of zinc oxide/reduced graphite oxide composite using microwave |
| KR20150021614A (en) * | 2013-08-20 | 2015-03-03 | 한국에너지기술연구원 | Method for fabricating graphite oxide and method for manufacturing graphene nano seat using the graphite oxide |
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| KR20130079735A (en) | 2012-01-03 | 2013-07-11 | 부산대학교 산학협력단 | Method of manufacturing graphene/metal oxide nanocomposites through microwaved-assisted synthesis |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| KR101970134B1 (en) * | 2018-04-16 | 2019-04-18 | 한국지질자원연구원 | Electrode comprising activated carbon and graphene sheet, method of manufacturing the electrode, and super capacitor comprising the electrode |
| KR20200114793A (en) * | 2019-03-29 | 2020-10-07 | 한국에너지기술연구원 | Method for manufacturing graphene composite, eletrode active material and secondary battery including the same |
| KR102157182B1 (en) * | 2020-04-29 | 2020-09-17 | 한국지질자원연구원 | Electrode for supercapacitor comprising activated carbon and reduced graphene oxide, method of manufacturing the electrode, and super capacitor comprising the electrode |
| CN112320796A (en) * | 2020-10-30 | 2021-02-05 | 浙江锂宸新材料科技有限公司 | Preparation method for simply increasing graphite layer spacing |
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