KR20150038915A - Method of fabricating graphene flake for electrode material of electric double layer capacitor, graphene flake fabricated by the same and electric double layer capacitor including the same by electrode material - Google Patents
Method of fabricating graphene flake for electrode material of electric double layer capacitor, graphene flake fabricated by the same and electric double layer capacitor including the same by electrode material Download PDFInfo
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- KR20150038915A KR20150038915A KR20130117298A KR20130117298A KR20150038915A KR 20150038915 A KR20150038915 A KR 20150038915A KR 20130117298 A KR20130117298 A KR 20130117298A KR 20130117298 A KR20130117298 A KR 20130117298A KR 20150038915 A KR20150038915 A KR 20150038915A
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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
- H01G11/84—Processes for the manufacture of hybrid or EDL capacitors, or components thereof
- H01G11/86—Processes for the manufacture of hybrid or EDL capacitors, or components thereof specially adapted for electrodes
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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
- B01J19/12—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor employing electromagnetic waves
- B01J19/122—Incoherent waves
- B01J19/126—Microwaves
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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
- C01B32/19—Preparation by exfoliation
- C01B32/192—Preparation by exfoliation starting from graphitic oxides
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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
- C01B32/194—After-treatment
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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
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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
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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
The present invention relates to a method for producing a graphene flake for an electrode material of an electric double layer capacitor, a graphene flake produced thereby and an electric double layer capacitor comprising the same as an electrode material. More particularly, (P) and nitrogen (N) at the same time to improve the electrochemical characteristics of graphene flakes, and a method for producing graphene flakes for an electrode material of an electric double layer capacitor, Lt; RTI ID = 0.0 > capacitor. ≪ / RTI >
To this end, the present invention provides a method for preparing a solution, comprising: preparing a solution to which graphene oxide or graphene is added; Adding a phosphorus (P) doping source to said solution; A microwave treatment step of microwave-treating the solution to which the doping source is added; And a thermal reduction treatment step of subjecting the microwaved solution to a thermal reduction treatment. The method for producing graphene flakes for an electrode material of an electric double layer capacitor, Electric double layer capacitor.
Description
The present invention relates to a method for producing a graphene flake for an electrode material of an electric double layer capacitor, a graphene flake produced thereby and an electric double layer capacitor comprising the same as an electrode material. More particularly, (P) and nitrogen (N) at the same time to improve the electrochemical characteristics of graphene flakes, and a method for producing graphene flakes for an electrode material of an electric double layer capacitor, Lt; RTI ID = 0.0 > capacitor. ≪ / RTI >
Among the electrode materials of the electric double layer capacitor, the core material that determines the capacity performance of the device is the electrode active material. As such an electrode active material, a carbon-based material having a high specific surface area is utilized. For example, activated carbon having a high specific surface area of 1,500 to 2,000 m 2 / g has been commercially used. However, since the activated carbon has a problem of lowering the electrical conductivity despite its high specific surface area, carbon black having excellent electrical conductivity is used as the conductive material (for example, activated carbon: conductive material = 8: 2).
On the other hand, graphene is attracting attention in various fields due to its excellent electrical properties and mechanical properties. Such graphene is particularly attracting attention as an electrode for ultracapacitors due to its wide specific surface area and excellent electrical properties.
At this time, an electrode for an ultracapacitor including graphene as an electrode material is manufactured by various methods. Among them, electrode fabrication using oxide graphene, which is easy to produce at low cost in a solution process, has been actively studied.
Thus, as graphenes are used as electrode materials for ultracapacitors, there is a demand for the production of graphene having excellent electrical characteristics.
SUMMARY OF THE INVENTION It is an object of the present invention to overcome the problems of the prior art as described above and it is an object of the present invention to provide a graphene flake, The present invention provides a method for producing graphene flakes for an electrode material of an electric double layer capacitor capable of improving the electrochemical characteristics of the graphene flakes and an electric double layer capacitor comprising the graphene flakes.
To this end, the present invention provides a method for preparing a solution, comprising: preparing a solution to which graphene oxide or graphene is added; Adding a phosphorus (P) doping source to said solution; A microwave treatment step of microwave-treating the solution to which the doping source is added; And a thermal reduction step of subjecting the microwaved solution to a thermal reduction treatment. The present invention also provides a method for manufacturing graphene flakes for an electrode material of an electric double layer capacitor.
In the doping source addition step, a phosphonic acid-based powder may be used as the phosphorus (P) doping source.
At this time, in the doping source addition step, phenylphosphonic acid may be used as the phosphorus (P) doping source.
Further, in the doping source addition step, a nitrogen (N) doping source may be further added to the solution.
At this time, as the nitrogen (N) doping source, any one of ammonia, hydrazine, and pyrrole may be used.
And preparing the oxidized graphene before the solution preparation step.
The step of preparing the graphene oxide may include a first step of treating the graphite with an acid to produce graphite oxide and a second step of separating the graphene oxide from the oxidized graphite.
On the other hand, the present invention provides a graphene flake characterized in that phosphorus (P) or phosphorus (P) and nitrogen (N) are covalently bonded.
In addition, the present invention provides an electric double-layer capacitor comprising the graphene flake as an electrode material.
According to the present invention, the electrochemical properties of graphene flakes are improved by simultaneously doping phosphorus (P) or phosphorus (P) and nitrogen (N) in the graphene flake through a series of microwave reactions and thermal reduction Therefore, when the prepared graphene flake is used as an electrode material of an electric double layer capacitor, capacity characteristics of the electric double layer capacitor can be improved.
BRIEF DESCRIPTION OF THE DRAWINGS FIG. 1 is a flow chart showing a process for producing graphene flakes for an electrode material of an electric double layer capacitor according to an embodiment of the present invention; FIG.
FIG. 2 is a graph showing the relationship between the amount of phenylphosphonic acid (a) and nitrogen (N) used as the phosphorus (P) doping source in the step of adding the doping source in the method for producing graphene flakes for an electrode material of an electric double- (B) used as a doping source.
FIGS. 3 and 4 are XPS analysis results of graphene flakes prepared by the method of producing graphene flakes for an electrode material of an electric double layer capacitor according to an embodiment of the present invention. FIG.
Hereinafter, a method for manufacturing a graphene flake for an electrode material of an electric double layer capacitor according to an embodiment of the present invention, a graphene flake manufactured thereby, and an electric double layer capacitor including the electrode material will be described in detail with reference to the accompanying drawings .
In the following description of the present invention, detailed description of known functions and configurations incorporated herein will be omitted when it may make the subject matter of the present invention rather unclear.
The graphene flake manufacturing method according to an embodiment of the present invention is a method for manufacturing a graphene flake used as an electrode material of an electric double layer capacitor. Here, the electric double-layer capacitor is an energy storage device using a pair of charge layers (electric double layer) having different signs generated. It has better output characteristics than ordinary batteries and has a short charging / discharging time and excellent durability and stability. Have. Such an electric double layer capacitor generally comprises a cell in which two electrodes of an anode and a cathode are arranged so as to face each other with a separator interposed therebetween and then impregnated with an electrolyte. That is, the method for producing graphene flakes according to an embodiment of the present invention is a method for producing graphene flakes used as at least one electrode material of two electrodes of the electric double layer capacitor. As shown in Fig. 1, this graphene flake production method includes a solution preparation step S1, a doping source addition step S2, a microwave treatment step S3 and a thermal reduction treatment step S4.
First, the solution preparation step (S1) is a step of preparing a solution to which graphene oxide or graphene is added. Here, prior to the solution preparation step (S1), a step of producing graphene oxide or a step of producing graphene is preceded. For example, a method for preparing graphene grains includes firstly treating graphite with Hummer's method to form a hydroxide group, an epoxide group and a carboxylic group on the surface, ≪ / RTI > Then, graphene oxide is obtained through layer separation from the produced graphite oxide. At this time, the layer separation process may be performed by adding liquid graphite to distilled water as a solvent at a predetermined concentration, followed by liquid-phase sonication. As a method for producing graphene, graphene can be peeled off from a carbon material such as graphite.
In the solution preparation step (S1), an oxidized graphene solution or a graphene solution is prepared by immersing the graphene oxide or graphene thus produced in, for example, methanol or the like.
Next, the doping source addition step (S2) is a step of adding a phosphorus (P) doping source to the graphene oxide solution or graphene solution to dope phosphorus (P) in the graphene flake. In the doping source addition step (S2), a phosphonic acid-based powder may be used as a phosphorus (P) doping source. For example, in the doping source addition step (S2), phenylphosphonic acid, which is well soluble in an aqueous solution as shown in FIG. 2 (a), may be added to the oxidized graphene solution or the graphene solution . By adding phenylphosphonic acid, the effect of maintaining the dispersibility of the solution can also be obtained.
In the doping source addition step S2, a nitrogen (N) doping source is further added to the graphene oxide solution or the graphene solution so as to simultaneously doping phosphorus (P) and nitrogen (N) in the graphene flake . At this time, ammonia or hydrazine may be used as a nitrogen (N) doping source, or pyrrole may be used as shown in FIG. 2 (b). As shown in the XPS analysis result of FIG. 3, after the microwave treatment step (S3) and the thermal reduction treatment step (S4) proceeding to the subsequent step, the addition of the nitrogen (N) nitrogen (N) is doped in pyridinic and pyrrolic forms.
Next, the microwave processing step S3 is a step of processing the graphene solution or graphene solution in which the phosphorus (P) doping source or the phosphorus (P) doping source and the nitrogen (N) microwave. In the microwave treatment step (S3), a graphene solution or a graphene solution to which a doping source is added is microwave-treated at a high temperature (for example, 180 degrees) and under a high pressure. Thus, in the microwave treatment step (S3), thermal degradation of the doping source and doping in the graphene flake are induced.
Finally, the thermal reduction treatment step S4 is a step of subjecting the microwaved solution to a thermal reduction treatment. In the thermal reduction treatment step S4, the graphene is reduced by inducing thermal decomposition at a temperature of 800 degrees or more to induce carbonization of the doping source, whereby phosphorus (P) or phosphorus (P) is introduced into the graphene flake Nitrogen (N) is doped. FIG. 4 shows that when phosphorus (P) doping source is doped, phosphorus (P) is well doped into the graphene flake as a result of XPS element analysis.
As described above, when the thermal reduction step S4 is completed, phosphorus (P) or phosphorus (P) and nitrogen (N) are doped to produce graphene flakes which are covalently bonded to graphene. Like the graphene flake manufacturing method according to the embodiment of the present invention, graphene flakes doped with phosphorus (P) can introduce excess charges unlike graphenes without defects or doping of dopants. Accordingly, when the graphene flake manufactured by the method of manufacturing graphene flakes according to the embodiment of the present invention is applied to an electrode material of an electric double layer capacitor, the distance between the graphene flake and the ions in the electrolyte is shortened, , A large amount of charge can be introduced, and the impedance of the electrolyte and the interface also decreases, so that the capacity of the electrode can be increased. Also, the graphene flake manufactured by the method of the present invention has high charge density due to simultaneous doping of phosphorus (P) or phosphorus (P) and nitrogen (N) . Accordingly, the characteristics of the electric double layer capacitor including the graphene flake fabricated by the method of manufacturing the graphene flake according to the embodiment of the present invention as an electrode material can be further improved.
While the invention has been shown and described with reference to certain preferred embodiments thereof, it will be understood by those of ordinary skill 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. This is possible.
Therefore, the scope of the present invention should not be limited by the described embodiments, but should be determined by the scope of the appended claims as well as the appended claims.
Claims (9)
Adding a phosphorus (P) doping source to said solution;
A microwave treatment step of microwave-treating the solution to which the doping source is added; And
A thermal reduction treatment step of subjecting the microwaved solution to a thermal reduction treatment;
Wherein the graphene flake is formed of an electrically conductive material.
Wherein the phosphonic acid-based powder is used as the phosphorus (P) doping source in the step of doping the dopant source.
Wherein the step of adding the doping source uses phenylphosphonic acid as the phosphorus (P) doping source.
Wherein the doping source addition step further comprises adding a nitrogen (N) doping source to the solution.
Wherein the nitrogen (N) doping source is one selected from the group consisting of ammonia, hydrazine, and pyrrole.
Further comprising the step of preparing the graphene oxide grains before the solution preparation step.
The step of preparing the oxide grains comprises:
A first step of acid-treating graphite to produce graphite oxide, and
And separating the graphene oxide layer from the oxidized graphite layer. The method for producing graphene flake for an electrode material of an electric double layer capacitor according to claim 1,
Priority Applications (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| KR20130117298A KR20150038915A (en) | 2013-10-01 | 2013-10-01 | Method of fabricating graphene flake for electrode material of electric double layer capacitor, graphene flake fabricated by the same and electric double layer capacitor including the same by electrode material |
| PCT/KR2014/009155 WO2015050353A1 (en) | 2013-10-01 | 2014-09-30 | Method for fabricating graphene flake for electrode material of electric double-layer capacitor, graphene flake fabricated by same, and electric double-layer capacitor comprising same as electrode material |
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| KR20130117298A KR20150038915A (en) | 2013-10-01 | 2013-10-01 | Method of fabricating graphene flake for electrode material of electric double layer capacitor, graphene flake fabricated by the same and electric double layer capacitor including the same by electrode material |
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| KR20150038915A true KR20150038915A (en) | 2015-04-09 |
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| WO (1) | WO2015050353A1 (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR101629835B1 (en) * | 2015-11-11 | 2016-06-14 | 한국지질자원연구원 | Manufacturing method of three-dimensional graphene composite via multi-doping and supercapacitor using thereof |
| CN107331530A (en) * | 2017-06-26 | 2017-11-07 | 中国科学技术大学 | A kind of low-temperature-doped graphene and preparation method thereof and ultracapacitor |
| CN108772079A (en) * | 2018-04-26 | 2018-11-09 | 昆明理工大学 | A kind of preparation method of nanometer of black phosphorus/graphene composite material |
Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP6498210B2 (en) | 2013-12-29 | 2019-04-10 | チュアラボ オンコロジー, インコーポレーテッドCurelab Oncology, Inc. | Methods and compositions relating to P62 / SQSTM1 for the treatment and prevention of inflammation-related diseases |
| CN106276864A (en) * | 2015-06-12 | 2017-01-04 | 中国石油化工股份有限公司 | The synthetic method of phosphorus doping Graphene |
| CN106276866A (en) * | 2015-06-12 | 2017-01-04 | 中国石油化工股份有限公司 | The production method of phosphorus doping Graphene |
| CN106276865A (en) * | 2015-06-12 | 2017-01-04 | 中国石油化工股份有限公司 | The method producing phosphorus doping Graphene |
| CN112420991A (en) * | 2020-08-21 | 2021-02-26 | 华南农业大学 | Doping method of novel carbon material and application thereof |
Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US8354323B2 (en) * | 2010-02-02 | 2013-01-15 | Searete Llc | Doped graphene electronic materials |
| KR101886871B1 (en) * | 2011-08-25 | 2018-08-10 | 한국과학기술원 | Nitrogen-doped graphene, ultracapacitor using the same and doping methode of the same |
| KR101275282B1 (en) * | 2011-09-07 | 2013-06-18 | 성균관대학교산학협력단 | Field-effect transistor using n-doped graphene and preparing method of the same |
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2013
- 2013-10-01 KR KR20130117298A patent/KR20150038915A/en not_active Application Discontinuation
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- 2014-09-30 WO PCT/KR2014/009155 patent/WO2015050353A1/en active Application Filing
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR101629835B1 (en) * | 2015-11-11 | 2016-06-14 | 한국지질자원연구원 | Manufacturing method of three-dimensional graphene composite via multi-doping and supercapacitor using thereof |
| CN107331530A (en) * | 2017-06-26 | 2017-11-07 | 中国科学技术大学 | A kind of low-temperature-doped graphene and preparation method thereof and ultracapacitor |
| CN108772079A (en) * | 2018-04-26 | 2018-11-09 | 昆明理工大学 | A kind of preparation method of nanometer of black phosphorus/graphene composite material |
| CN108772079B (en) * | 2018-04-26 | 2021-03-02 | 昆明理工大学 | Preparation method of nano black phosphorus/graphene composite material |
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| WO2015050353A1 (en) | 2015-04-09 |
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