CN103839683A - Graphene electrode plate and preparation method thereof - Google Patents
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- CN103839683A CN103839683A CN201210484427.4A CN201210484427A CN103839683A CN 103839683 A CN103839683 A CN 103839683A CN 201210484427 A CN201210484427 A CN 201210484427A CN 103839683 A CN103839683 A CN 103839683A
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Abstract
The invention pertains to the field of electrochemistry materials, and discloses a grapheme electrode plate and a preparation method thereof. The grapheme electrode plate comprises a current collector and an electrode active material coating the surface of the current collector. The electrode active material comprises, by mass, 90-96% of graphene, 2-5% of conductive agent, and 2-5% of binder. According to the graphene electrode plate provided in the invention, a oxygen-containing functional group is formed on the surface of the grapheme, so when the grapheme electrode plate is used in a supercapacitor electrode, the oxygen-containing functional group and ions in an electrolyte can be subjected to Faraday redox reaction to increase the pseudocapacitance, so the graphene electrode plate has both of the electrical double-layer capacitance and the pseudocapacitance, so that the supercapacitor capacity can be improved.
Description
Technical field
The present invention relates to electrochemical material field, relate in particular to a kind of Graphene electrodes sheet and preparation method thereof.
Background technology
The strong K sea nurse of the peace moral of Univ Manchester UK (Andre K.Geim) etc. was prepared grapheme material in 2004, pay attention to widely because its unique structure and photoelectric property have been subject to people.Mono-layer graphite is due to its large specific area, good conduction, heat conductivility and low thermal coefficient of expansion and be considered to desirable material.As: 1, high strength, Young mole, (1,100GPa), fracture strength: (125GPa): 2, high heat conductance, (5,000W/mK): 3, high conductivity, carrier transport rate, (200,000cm2/V*s): 4, high specific area, (calculated value: 2,630m2/g).Especially its high conductivity matter, the structural property of large specific surface character and the nanoscale of its monolayer two dimension can be used as electrode material in ultracapacitor and lithium ion battery.
Up to the present, known to the method for preparing Graphene have multiple, as (1) micromechanics stripping method.This method can only produce the very limited graphene film of quantity, can be used as basic research: (2) ultra high vacuum Graphene epitaxial growth method.The structural limitations of the expensive and sequin of this method its application: (3) chemical vapour deposition technique (CVD).The method can meet the requirement that high-quality graphene is prepared in scale, but cost is higher, complex process.(4) solvent stripping method.The method shortcoming is that productive rate is very low, limits its business application: (5) oxidation-reduction method.
Ruoff group utilizes the Graphene of chemical modification as electrode material, has tested the performance of the ultracapacitor based on Graphene.The capacity of the capacitive property of this grapheme material in water system and organic electrolyte can reach respectively 135F/g and 99F/g.The people such as Rao have compared the capacitive property of the Graphene of preparing by two kinds of methods.In sulfuric acid electrolyte, the Graphene obtaining by graphite oxide dilatometry and Nano diamond conversion method has higher capacity, can reach 117F/g; In organic electrolyte, when voltage is 3.5V, its capacity and energy density can reach 71F/g and 31.9Wh/kg.
Graphene improves as super capacitor energy density, but compared with lithium ion battery, also has a certain distance, is necessary further to improve the energy density of material.
Summary of the invention
Problem to be solved by this invention is to provide a kind of Graphene electrodes sheet of energy density.
Technical scheme of the present invention is as follows:
A kind of Graphene electrodes sheet, comprises collector, it is characterized in that, be coated with electrode active material at described collection liquid surface, this electrode active material comprises that mass percent is respectively 90 ~ 96%, 2 ~ 5%, 2 ~ 5% Graphene, conductive agent and binding agent.
Described Graphene electrodes sheet, wherein, described conductive agent comprises acetylene black, Ketjen black, SP conductive black: described binding agent comprises Kynoar, polytetrafluoroethylene, polyvinyl alcohol: described solvent comprises NMP, absolute ethyl alcohol.
Described Graphene electrodes sheet, wherein, described collector comprises aluminium foil, nickel screen, titanium foil and stainless steel foil.
Described Graphene electrodes sheet, wherein, the thickness of the layer structure that described electrode active material forms at collection liquid surface is 50 ~ 300 μ m.
The preparation method of above-mentioned Graphene electrodes sheet, comprises the steps:
Mass percent is respectively after 90 ~ 96%, 2 ~ 5% and 2 ~ 5% Graphene, conductive agent and binding agent are uniformly mixed and is added in solvent, be configured to gelatinous electrode active material: wherein, in gelatinous electrode active material, solvent accounts for 10 ~ 30% of total weight:
The thickness that described electrode active material is coated on collector and control gelatinous electrode active material is 50 ~ 300 μ m, and then dry processing, obtains Graphene electrodes sheet sample:
Using described Graphene electrodes sheet sample as work electrode, platinized platinum is as auxiliary electrode, silver/silver chloride electrode is as reference electrode, described Graphene electrodes sheet is connected to work electrode, platinized platinum to be connected to after auxiliary electrode and silver/silver chloride electrode are connected to reference electrode and to insert in electrolyte, be connected respectively to subsequently China's 660 type electrochemical workstations in morning, then adopt cyclic voltammetry to carry out electrochemical oxidation:
After electrochemical oxidation reactions finishes, then the Graphene electrodes sheet sample that oxidation processes is crossed is placed on 80 ~ 100 DEG C of vacuumizes in vacuum drying chamber, obtains described Graphene electrodes sheet after dry.
The preparation method of described Graphene electrodes sheet, wherein, described conductive agent comprises acetylene black, Ketjen black, SP conductive black: described binding agent comprises Kynoar, polytetrafluoroethylene, polyvinyl alcohol: described solvent comprises NMP, absolute ethyl alcohol.
The preparation method of described Graphene electrodes sheet, wherein, described collector comprises aluminium foil, nickel screen, titanium foil and stainless steel foil.
The preparation method of described Graphene electrodes sheet, wherein, the dry processing of described electrode active material is carried out in baking oven, and the temperature of baking oven is 80 ~ 100 DEG C, the dry 6 ~ 12h that processes.
The preparation method of described Graphene electrodes sheet, wherein, the thickness of the layer structure that described electrode active material forms at collection liquid surface is 50 ~ 300 μ m.
The preparation method of described Graphene electrodes sheet, wherein, described electrolyte comprises that concentration is nitric acid, hydrochloric acid, sulfuric acid, potassium chloride or the sodium chloride solution of 0.5 ~ 3mol/L.
The preparation method of described Graphene electrodes sheet, wherein, when described cyclic voltammetry electrochemical oxidation, voltage scan range 0.5 ~ 2V, sweep speed is 10 ~ 100mv/s, scanning times is 10 ~ 50 times.
Graphene electrodes sheet provided by the invention, be formed with oxygen-containing functional group on Graphene surface: in the time that Graphene electrodes sheet is used to electrode of super capacitor, these oxygen-containing functional groups can with electrolyte in ion there is faraday redox reaction, increase fake capacitance, make Graphene electrodes sheet not only there is electric double layer capacitance but also have fake capacitance, and then improved the capacity of ultracapacitor.
The present invention adopts the method for electrochemical activation to prepare Graphene electrodes sheet, method can improve Graphene electrodes sheet capacity, and can form oxygen-containing functional group on the surface of Graphene, the oxygen-containing functional group on these Graphene surfaces can react with electrolyte ion generation fake capacitance and carry out energy storage, improve energy density, there is good electrochemical stability at the oxygen-containing functional group on Graphene surface, can keep the life-span of growing simultaneously.
Brief description of the drawings
Fig. 1 is preparation technology's flow chart of Graphene electrodes sheet of the present invention:
Fig. 2 is the charging and discharging curve figure that embodiment 1 and comparative example 1 make electrode slice:
Fig. 3 is the charging cycle number of times of the Graphene electrodes sheet that makes of embodiment 1 and the curve chart of specific capacity.
Embodiment
Graphene electrodes piece preparation method provided by the invention, as shown in Figure 1, its processing step is as follows:
1, prepare gelatinous electrode active material:
According to mass percent, 90 ~ 96% Graphene, 2 ~ 5% conductive agent, 2 ~ 5% binding agent are added in solvent, stir, be configured to gelatinous electrode active material: wherein, in electrode active material, solvent accounts for the 10-30% of total weight:
Conductive agent comprises acetylene black, Ketjen black, SP conductive black: binding agent comprises Kynoar, polytetrafluoroethylene, polyvinyl alcohol: described solvent comprises NMP, absolute ethyl alcohol:
2, preparation Graphene electrodes sheet sample: electrode active material is coated on collector equably, and to control coating thickness be 50 ~ 300 μ m, then put it into baking oven, at 80-100 DEG C of dry 6-12h, obtain Graphene electrodes sheet sample:
Collector can be selected aluminium foil, nickel screen, titanium foil, stainless steel foil etc.:
3, electrochemicial oxidation: electrochemical oxidation adopts three-electrode system to carry out, using the Graphene electrodes sheet sample obtaining as work electrode, platinized platinum is auxiliary electrode, silver/silver chloride electrode is reference electrode, Graphene electrodes sheet is connected to work electrode, platinized platinum is connected to after auxiliary electrode and silver/silver chloride electrode are connected to reference electrode and inserts in electrolyte, be connected respectively to subsequently China's 660 type electrochemical workstations in morning, adopt cyclic voltammetry to carry out electrochemical oxidation: wherein, when electrochemical oxidation, voltage scan range 0.5 ~ 2V, sweep speed is 10 ~ 100mv/s, scanning times is 10 ~ 50 times:
Electrolyte can be selected nitric acid, hydrochloric acid, sulfuric acid, potassium chloride or the sodium chloride solution of 0.5 ~ 3mol/L:
4, dry processing: after electrochemical oxidation reactions completes, then the Graphene electrodes sheet sample that oxidation processes is crossed is placed on 80 ~ 100 DEG C of vacuumizes in vacuum drying chamber, obtains Graphene electrodes sheet after dry.
Below in conjunction with accompanying drawing, preferred embodiment of the present invention is described in further detail.
1, prepare gelatinous electrode active material:
According to mass percent, 90% Graphene, 5% acetylene black, 5% Kynoar (PVDP) are added in nmp solvent, stir, be configured to gelatinous electrode active material: wherein, in electrode active material, solvent accounts for 30% of total weight:
2, preparation Graphene electrodes sheet sample: electrode active material is coated on aluminium foil equably, and to control coating thickness be 50 μ m, then put it into baking oven, at 80 DEG C of dry 12h, obtain Graphene electrodes sheet sample:
3, electrochemicial oxidation: electrochemical oxidation adopts three-electrode system to carry out, using the Graphene electrodes sheet sample obtaining as work electrode, platinized platinum is auxiliary electrode, silver/silver chloride electrode is reference electrode, three electrodes are placed in the salpeter solution of 0.5mol/L after electrochemical workstation respectively, adopt cyclic voltammetry to carry out electrochemical oxidation: wherein, when electrochemical oxidation, voltage scan range 0.5V, sweep speed is 10mv/s, scanning times is 10 times:
4, dry processing: after electrochemical oxidation reactions completes, then the Graphene electrodes sheet sample that oxidation processes is crossed is placed on 80 DEG C of vacuumizes in vacuum drying chamber, obtains Graphene electrodes sheet after dry.
Fig. 2 is the charging and discharging curve figure that embodiment 1 and comparative example 1 make electrode slice: as shown in Figure 2, the electrode slice that the present embodiment makes increases discharge time to some extent, illustrates that electrochemistry capacitance is greatly improved, and energy density is also improved.
Fig. 3 is the charging cycle number of times of the Graphene electrodes sheet that makes of embodiment 1 and the curve chart of specific capacity: as shown in Figure 3, Graphene electrodes sheet is through 1000 circulations, and capacity also can also keep more than 90%, illustrating and having the good life-span.
Table 1 is that embodiment 2 to 7, embodiment 2 to 7 is identical with the technological process of embodiment 1, and difference refers to following table 1:
Table 1
Comparative example 1
Please inventor provide the preparation technology of comparative example 1, or directly provide the structure composition of the electrode slice of comparative example.
Comparative example 1 electrode slice preparation technology
1, prepare gelatinous electrode active material:
According to mass percent, 90% Graphene, 5% acetylene black, 5% Kynoar (PVDP) are added in nmp solvent, stir, be configured to gelatinous electrode active material: wherein, in electrode active material, solvent accounts for 30% of total weight:
2, preparation Graphene electrodes sheet sample: electrode active material is coated on aluminium foil equably, and to control coating thickness be 50 μ m, then put it into baking oven, at 80 DEG C of dry 12h, obtain Graphene electrodes sheet sample:
Should be understood that, the above-mentioned statement for preferred embodiment of the present invention is comparatively detailed, can not therefore think the restriction to scope of patent protection of the present invention, and scope of patent protection of the present invention should be as the criterion with claims.
Claims (10)
1. a Graphene electrodes sheet, comprises collector, it is characterized in that, is coated with electrode active material at described collection liquid surface, and this electrode active material comprises that mass percent is respectively 90 ~ 96%, 2 ~ 5%, 2 ~ 5% Graphene, conductive agent, binding agent.
2. Graphene electrodes sheet according to claim 1, is characterized in that, described conductive agent comprises acetylene black, Ketjen black, SP conductive black; Described binding agent comprises Kynoar, polytetrafluoroethylene, polyvinyl alcohol; Described solvent comprises NMP, absolute ethyl alcohol.
3. Graphene electrodes sheet according to claim 1, is characterized in that, described collector comprises aluminium foil, nickel screen, titanium foil and stainless steel foil.
4. Graphene electrodes sheet according to claim 1, is characterized in that, the thickness of the layer structure that described electrode active material forms at collection liquid surface is 50 ~ 300 μ m.
5. a preparation method for Graphene electrodes sheet, is characterized in that, comprises the steps:
Mass percent is respectively after 90 ~ 96%, 2 ~ 5% and 2 ~ 5% Graphene, conductive agent and binding agent are uniformly mixed and is added in solvent, be configured to gelatinous electrode active material; Wherein, in electrode active material, solvent accounts for 10 ~ 30% of total weight;
Described electrode active material is coated on collector, and then dry processing, obtains Graphene electrodes sheet sample;
Using described Graphene electrodes sheet sample as work electrode, platinized platinum is as auxiliary electrode, silver/silver chloride electrode is as reference electrode, described Graphene electrodes sheet is connected to work electrode, platinized platinum to be connected to after auxiliary electrode and silver/silver chloride electrode are connected to reference electrode and to insert in electrolyte, be connected respectively to subsequently China's 660 type electrochemical workstations in morning, then adopt cyclic voltammetry to carry out electrochemical oxidation;
After electrochemical oxidation reactions finishes, then the Graphene electrodes sheet sample that oxidation processes is crossed is placed on 80 ~ 100 DEG C of vacuumizes in vacuum drying chamber, obtains described Graphene electrodes sheet after dry.
6. the preparation method of Graphene electrodes sheet according to claim 5, is characterized in that, described conductive agent comprises acetylene black, Ketjen black, SP conductive black; Described binding agent comprises Kynoar, polytetrafluoroethylene, polyvinyl alcohol; Described solvent comprises NMP, absolute ethyl alcohol.
7. the preparation method of Graphene electrodes sheet according to claim 5, is characterized in that, described collector comprises aluminium foil, nickel screen, titanium foil and stainless steel foil.
8. the preparation method of Graphene electrodes sheet according to claim 5, is characterized in that, the dry processing of described electrode active material is carried out in baking oven, and the temperature of baking oven is 80 ~ 100 DEG C, the dry 6 ~ 12h that processes.
9. the preparation method of Graphene electrodes sheet according to claim 5, is characterized in that, the thickness of the layer structure that described electrode active material forms at collection liquid surface is 50 ~ 300 μ m.
10. the preparation method of Graphene electrodes sheet according to claim 5, it is characterized in that, described electrolyte comprises that concentration is nitric acid, hydrochloric acid, sulfuric acid, potassium chloride or the sodium chloride solution of 0.5 ~ 3mol/L: when described cyclic voltammetry electrochemical oxidation, voltage scan range 0.5 ~ 2V, sweep speed is 10 ~ 100mv/s, and scanning times is 10 ~ 50 times.
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Cited By (10)
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| CN105405676A (en) * | 2015-12-24 | 2016-03-16 | 同济大学 | Novel structured supercapacitor taking graphene and cement as materials and fabrication of supercapacitor |
| CN106024411A (en) * | 2016-07-26 | 2016-10-12 | 锦州凯美能源有限公司 | Electrode material and preparation method of electrode material, electrode piece and supercapacitor |
| CN108888865A (en) * | 2018-06-29 | 2018-11-27 | 成都三乙医疗科技有限公司 | A kind of thermal physical therapeutical electrode slice |
| CN109216648A (en) * | 2018-08-21 | 2019-01-15 | 中国科学院金属研究所 | Ion is embedded in the intercalation electrode and its preparation method and application that two-dimensional layer material is constructed in advance |
| CN109721135A (en) * | 2019-01-08 | 2019-05-07 | 烟台大学 | The graphite felt electrode and its method of modifying and purposes of a kind of modification |
| CN110706942A (en) * | 2018-07-10 | 2020-01-17 | 中国科学院上海硅酸盐研究所 | Method for modifying carbon material through electrochemical oxidation |
| CN111105936A (en) * | 2019-12-16 | 2020-05-05 | 江苏第二师范学院（江苏省教育科学研究院） | Energy storage system of modified carbon-based electrode in cooperation with redox electrolyte |
| CN113184951A (en) * | 2021-04-20 | 2021-07-30 | 浙江大学 | Modification method and application of graphite felt cathode in electric over-ozonation system |
| CN113327777A (en) * | 2021-05-21 | 2021-08-31 | 大连理工大学 | Preparation method of electrode material of high pseudo-capacitance super capacitor |
| CN116514114A (en) * | 2023-07-04 | 2023-08-01 | 深圳市本征方程石墨烯技术股份有限公司 | Single-layer edge graphene oxide and preparation method thereof |
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| CN105405676B (en) * | 2015-12-24 | 2016-11-16 | 同济大学 | New structure ultracapacitor with Graphene and cement as material and making thereof |
| CN105405676A (en) * | 2015-12-24 | 2016-03-16 | 同济大学 | Novel structured supercapacitor taking graphene and cement as materials and fabrication of supercapacitor |
| CN106024411A (en) * | 2016-07-26 | 2016-10-12 | 锦州凯美能源有限公司 | Electrode material and preparation method of electrode material, electrode piece and supercapacitor |
| CN106024411B (en) * | 2016-07-26 | 2018-02-23 | 锦州凯美能源有限公司 | A kind of preparation method of electrode material and electrode plates and ultracapacitor |
| CN108888865A (en) * | 2018-06-29 | 2018-11-27 | 成都三乙医疗科技有限公司 | A kind of thermal physical therapeutical electrode slice |
| CN110706942A (en) * | 2018-07-10 | 2020-01-17 | 中国科学院上海硅酸盐研究所 | Method for modifying carbon material through electrochemical oxidation |
| CN109216648A (en) * | 2018-08-21 | 2019-01-15 | 中国科学院金属研究所 | Ion is embedded in the intercalation electrode and its preparation method and application that two-dimensional layer material is constructed in advance |
| CN109721135A (en) * | 2019-01-08 | 2019-05-07 | 烟台大学 | The graphite felt electrode and its method of modifying and purposes of a kind of modification |
| CN111105936A (en) * | 2019-12-16 | 2020-05-05 | 江苏第二师范学院（江苏省教育科学研究院） | Energy storage system of modified carbon-based electrode in cooperation with redox electrolyte |
| CN113184951A (en) * | 2021-04-20 | 2021-07-30 | 浙江大学 | Modification method and application of graphite felt cathode in electric over-ozonation system |
| CN113327777A (en) * | 2021-05-21 | 2021-08-31 | 大连理工大学 | Preparation method of electrode material of high pseudo-capacitance super capacitor |
| CN116514114A (en) * | 2023-07-04 | 2023-08-01 | 深圳市本征方程石墨烯技术股份有限公司 | Single-layer edge graphene oxide and preparation method thereof |
| CN116514114B (en) * | 2023-07-04 | 2023-10-31 | 深圳市本征方程石墨烯技术股份有限公司 | Single-layer edge graphene oxide and preparation method thereof |
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Application publication date: 20140604 |