CN105355465A - Preparation method of amorphous carbon/vertical graphene composite electrode material - Google Patents
Preparation method of amorphous carbon/vertical graphene composite electrode material Download PDFInfo
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 62
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 58
- 229910003481 amorphous carbon Inorganic materials 0.000 title claims abstract description 40
- 239000007772 electrode material Substances 0.000 title claims abstract description 35
- 238000002360 preparation method Methods 0.000 title claims abstract description 22
- 239000002131 composite material Substances 0.000 title abstract description 6
- 239000007789 gas Substances 0.000 claims abstract description 75
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims abstract description 48
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims abstract description 46
- 238000000623 plasma-assisted chemical vapour deposition Methods 0.000 claims abstract description 24
- 229910052786 argon Inorganic materials 0.000 claims abstract description 23
- 239000000463 material Substances 0.000 claims abstract description 20
- 230000001105 regulatory effect Effects 0.000 claims abstract description 20
- 238000000151 deposition Methods 0.000 claims abstract description 17
- 230000008021 deposition Effects 0.000 claims abstract description 7
- 239000012300 argon atmosphere Substances 0.000 claims abstract description 5
- 238000001816 cooling Methods 0.000 claims abstract description 5
- 238000010438 heat treatment Methods 0.000 claims abstract description 5
- 230000001276 controlling effect Effects 0.000 claims description 14
- 238000004062 sedimentation Methods 0.000 claims description 13
- 238000005086 pumping Methods 0.000 claims description 10
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 7
- 239000012298 atmosphere Substances 0.000 claims description 4
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 4
- 239000000758 substrate Substances 0.000 claims description 4
- 239000006260 foam Substances 0.000 claims description 2
- 229910002804 graphite Inorganic materials 0.000 claims description 2
- 239000010439 graphite Substances 0.000 claims description 2
- 229910052751 metal Inorganic materials 0.000 claims description 2
- 239000002184 metal Substances 0.000 claims description 2
- 229910052759 nickel Inorganic materials 0.000 claims description 2
- 229910052697 platinum Inorganic materials 0.000 claims description 2
- 229910001220 stainless steel Inorganic materials 0.000 claims description 2
- 239000010935 stainless steel Substances 0.000 claims description 2
- 239000003792 electrolyte Substances 0.000 abstract description 10
- 238000000034 method Methods 0.000 abstract description 7
- 230000002209 hydrophobic effect Effects 0.000 abstract 1
- 230000000694 effects Effects 0.000 description 4
- 230000010148 water-pollination Effects 0.000 description 4
- 230000009286 beneficial effect Effects 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- 239000011149 active material Substances 0.000 description 1
- ORILYTVJVMAKLC-UHFFFAOYSA-N adamantane Chemical compound C1C(C2)CC3CC1CC2C3 ORILYTVJVMAKLC-UHFFFAOYSA-N 0.000 description 1
- 229910001573 adamantine Inorganic materials 0.000 description 1
- 239000003990 capacitor Substances 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 229910003460 diamond Inorganic materials 0.000 description 1
- 239000010432 diamond Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000009736 wetting Methods 0.000 description 1
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-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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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
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- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
- C23C16/26—Deposition of carbon only
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
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- H—ELECTRICITY
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- 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
- H01G11/24—Electrodes characterised by structural features of the materials making up or comprised in the electrodes, e.g. form, surface area or porosity; characterised by the structural features of powders or particles used therefor
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-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
- H01G11/26—Electrodes characterised by their structure, e.g. multi-layered, porosity or surface features
- H01G11/28—Electrodes characterised by their structure, e.g. multi-layered, porosity or surface features arranged or disposed on a current collector; Layers or phases between electrodes and current collectors, e.g. adhesives
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- 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
- H01G11/36—Nanostructures, e.g. nanofibres, nanotubes or fullerenes
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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
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- 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
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Abstract
The invention provides a preparation method of amorphous carbon/vertical graphene composite electrode material, relates to a preparation method of composite electrode material, and solves the problems that the specific capacitance value of a graphene supercapacitor is relatively low caused by less effective contact area between electrolyte and graphene due to the fact that graphene and the electrolyte cannot be effectively wetted because of the fact that existing pure vertically grown graphene material is hydrophobic. The method comprises the steps that collector electrode material of which the surface is provided with vertical graphene is arranged in a plasma enhanced chemical vapor deposition vacuum device, argon is introduced, pressure intensity is regulated and temperature is increased; methane gas is introduced, gas flow of argon and methane gas is controlled, and then pressure intensity is regulated and deposition is performed; and after completion of deposition, a radio frequency power supply and a heating power supply are turned off, introducing of methane gas is stopped, and cooling is performed till room temperature under the argon atmosphere so that the amorphous carbon/vertical graphene composite electrode material is obtained. The preparation method is used for preparation of the amorphous carbon/vertical graphene composite electrode material.
Description
Technical field
The present invention relates to a kind of preparation method of combination electrode material.
Background technology
Ultracapacitor has that power density is high, charge-discharge velocity is fast, cycle life reaches more than ten thousand times, the capacitance of farad level is issued at very little volume, need not charging circuit and controlled discharge circuit especially, compare with battery overcharge, cross put not to its life-span form negative effect, consider from the angle of environmental protection, it is a kind of green energy resource, but its ratio capacitance value, energy density are lower.In recent years, the discovery of the Graphene development of electrode material is had new direction, two dimension conjugated structure makes Graphene and composite material thereof have a lot of unique character, comprises huge specific area, makes it in raising super capacitor energy density, have potential using value.But pure orthotropic grapheme material is hydrophobicity, makes can not effectively soak between Graphene and electrolyte, and then make the contact area between electrolyte and Graphene less, cause the ratio capacitance value of Graphene ultracapacitor lower.
Amorphous carbon is a kind of amorphous carbon of shortrange order longrange disorder, and it has diamond lattic structure (i.e. sp simultaneously
3key) and graphite-structure (i.e. sp
2key), there are many and their similar performances.As amorphous carbon film has high rigidity and high elastic modulus, particularly its hardness, the upper limit can reach adamantine hardness, amorphous carbon also has the excellent character such as anti-wear-resisting, optical clarity, chemical inertness and hydrophily, is thus widely used in the fields such as various coating, optical window, field emmision material and solar cell.
Summary of the invention
It is hydrophobicity that the present invention will solve existing pure orthotropic grapheme material, make can not effectively soak between Graphene and electrolyte, and then make the effective contact area between electrolyte and Graphene less, cause the problem that the ratio capacitance value of Graphene ultracapacitor is lower, and the preparation method of a kind of amorphous carbon/vertical graphene combination electrode material is provided.
A preparation method for amorphous carbon/vertical graphene combination electrode material, specifically carries out according to following steps:
One, the collector material of vertical Graphene is had on surface to be placed in plasma enhanced chemical vapor deposition vacuum plant, being evacuated to pressure is 5Pa, be that 20sccm ~ 40sccm passes into argon gas with gas flow, vacuum pumping rate is regulated to be controlled by pressure in plasma enhanced chemical vapor deposition vacuum plant as 200Pa ~ 400Pa, and under pressure is 200Pa ~ 400Pa and argon gas atmosphere, by temperature most 200 DEG C ~ 600 DEG C in 10min ~ 30min;
Two, methane gas is passed into, the gas flow controlling argon gas is 1sccm ~ 10sccm, the gas flow controlling methane gas is 5sccm ~ 50sccm, then vacuum pumping rate is regulated to be controlled by pressure in plasma enhanced chemical vapor deposition vacuum plant as 400Pa ~ 800Pa, then depositing system radio-frequency power be 50W ~ 200W, pressure deposits under be 400Pa ~ 800Pa and temperature being 200 DEG C ~ 600 DEG C conditions, sedimentation time is 1min ~ 10min;
Three, after deposition terminates, close radio-frequency power supply and heating power supply, stop passing into methane gas, under an argon atmosphere, with cooling rate be 5 DEG C/s ~ 10 DEG C/s, cool to room temperature, namely obtains amorphous carbon/vertical graphene combination electrode material.
The preparation general principle of amorphous carbon of the present invention/vertical graphene combination electrode material: utilize plasma enhanced chemical vapor deposition method, can decompose carbon-source gas (as CH by efficient cryogenic by action of plasma
4, C
2h
4deng) formed there is highly active carbon-based group in a large number, these high-activity carbon groups can graphenic surface deposition generate amorphous carbon.Due to one deck amorphous carbon at Surface Creation, and amorphous carbon has hydrophily, obviously can improve the wetability of material, improves the active material of material unit are, thus improves the ratio capacitance of Graphene ultracapacitor.The inventive method is simple, effectively and solve the problem of the wetability of Graphene ultracapacitor and can effectively improve its ratio capacitance, have a good application prospect in graphene-based ultracapacitor field.
The invention has the beneficial effects as follows:
1, the present invention utilizes plasma enhanced chemical vapor deposition method, and have the collector material of vertical Graphene for growth substrate with superficial growth, growth temperature is 200 ~ 600 DEG C, passes into a small amount of CH
4gas and Ar gas, after opening plasma electrical source, can complete the growth of amorphous carbon after a certain time.
2, the present invention is by growth amorphous carbon, utilizes its hydrophily, improves the wetability of aqueous electrolyte at graphenic surface, improves collector material unit are activity substance content simultaneously, thus improves the ratio capacitance value of Graphene ultracapacitor.
3, method of the present invention is simple, and efficiently, low cost, is convenient to suitability for industrialized production, has a good application prospect in graphene-based ultracapacitor field.
Accompanying drawing explanation
Fig. 1 is the scanning electron microscope (SEM) photograph of amorphous carbon/vertical graphene combination electrode material prepared by embodiment one.
Embodiment
Technical solution of the present invention is not limited to following cited embodiment, also comprises the combination in any between each embodiment.
Embodiment one: the preparation method of a kind of amorphous carbon described in present embodiment/vertical graphene combination electrode material, specifically carry out according to following steps:
One, the collector material of vertical Graphene is had on surface to be placed in plasma enhanced chemical vapor deposition vacuum plant, being evacuated to pressure is 5Pa, be that 20sccm ~ 40sccm passes into argon gas with gas flow, vacuum pumping rate is regulated to be controlled by pressure in plasma enhanced chemical vapor deposition vacuum plant as 200Pa ~ 400Pa, and under pressure is 200Pa ~ 400Pa and argon gas atmosphere, by temperature most 200 DEG C ~ 600 DEG C in 10min ~ 30min;
Two, methane gas is passed into, the gas flow controlling argon gas is 1sccm ~ 10sccm, the gas flow controlling methane gas is 5sccm ~ 50sccm, then vacuum pumping rate is regulated to be controlled by pressure in plasma enhanced chemical vapor deposition vacuum plant as 400Pa ~ 800Pa, then depositing system radio-frequency power be 50W ~ 200W, pressure deposits under be 400Pa ~ 800Pa and temperature being 200 DEG C ~ 600 DEG C conditions, sedimentation time is 1min ~ 10min;
Three, after deposition terminates, close radio-frequency power supply and heating power supply, stop passing into methane gas, under an argon atmosphere, with cooling rate be 5 DEG C/s ~ 10 DEG C/s, cool to room temperature, namely obtains amorphous carbon/vertical graphene combination electrode material.
The beneficial effect of present embodiment is: 1, present embodiment utilizes plasma enhanced chemical vapor deposition method, and have the collector material of vertical Graphene for growth substrate with superficial growth, growth temperature is 200 ~ 600 DEG C, passes into a small amount of CH
4gas and Ar gas, after opening plasma electrical source, can complete the growth of amorphous carbon after a certain time.
2, present embodiment is by growth amorphous carbon, utilizes its hydrophily, improves the wetability of aqueous electrolyte at graphenic surface, improves collector material unit are activity substance content simultaneously, thus improves the ratio capacitance value of Graphene ultracapacitor.
3, the method for present embodiment is simple, and efficiently, low cost, is convenient to suitability for industrialized production, has a good application prospect in graphene-based ultracapacitor field.
Embodiment two: present embodiment and embodiment one unlike: the surface described in step one has the collector material of vertical Graphene specifically to prepare according to the following steps: electrode material is placed in plasma enhanced chemical vapor deposition vacuum plant, be evacuated to below 5Pa, pass into argon gas and methane gas, the gas flow regulating methane gas is 5sccm ~ 20sccm, the gas flow regulating argon gas is 50sccm ~ 100sccm, pressure in plasma enhanced chemical vapor deposition vacuum plant is regulated to be 200Pa ~ 900Pa, then be 50W ~ 200W at radio-frequency power, temperature is 500 DEG C ~ 800 DEG C and pressure is deposit under the condition of 200Pa ~ 900Pa, sedimentation time is 5min ~ 60min,
Described collector material is metallic nickel, nickel foam, metal platinum, stainless steel substrates or graphite paper.Other is identical with embodiment one.
Embodiment three: one of present embodiment and embodiment one or two unlike: the gas flow controlling argon gas in step 2 is 5sccm ~ 10sccm.Other is identical with embodiment one or two.
Embodiment four: one of present embodiment and embodiment one to three unlike: the gas flow controlling methane gas in step 2 is 10sccm ~ 50sccm.Other is identical with embodiment one to three.
Embodiment five: one of present embodiment and embodiment one to four unlike: then regulate vacuum pumping rate to control pressure in plasma enhanced chemical vapor deposition vacuum plant for 400Pa ~ 700Pa in step 2.Other is identical with embodiment one to four.
Embodiment six: one of present embodiment and embodiment one to five unlike: in step 2 then depositing system radio-frequency power be 100W ~ 175W, pressure deposits under be 400Pa ~ 800Pa and temperature being 200 DEG C ~ 600 DEG C conditions, sedimentation time is 1min ~ 10min.Other is identical with embodiment one to five.
Embodiment seven: one of present embodiment and embodiment one to six unlike: in step 2 then depositing system radio-frequency power be 50W ~ 200W, pressure deposits under be 400Pa ~ 800Pa and temperature being 200 DEG C ~ 600 DEG C conditions, sedimentation time is 2min ~ 10min.Other is identical with embodiment one to six.
Embodiment eight: one of present embodiment and embodiment one to seven unlike: in step one in 10min ~ 30min by temperature most 300 DEG C.Other is identical with embodiment one to seven.
Embodiment nine: one of present embodiment and embodiment one to eight unlike: in step one in 10min ~ 30min by temperature most 500 DEG C.Other is identical with embodiment one to eight.
Embodiment ten: one of present embodiment and embodiment one to nine unlike: in step one in 10min ~ 30min by temperature most 310 DEG C ~ 490 DEG C.Other is identical with embodiment one to nine.
Embodiment 11: one of present embodiment and embodiment one to ten unlike: in step one in 10min ~ 30min by temperature most 40 DEG C.Other is identical with embodiment one to ten.
Embodiment 12: one of present embodiment and embodiment one to ten one unlike: the gas flow controlling argon gas in step 2 is 5sccm.Other is identical with embodiment one to ten one.
Embodiment 13: one of present embodiment and embodiment one to ten two unlike: the gas flow controlling methane gas in step 2 is 30sccm.Other is identical with embodiment one to ten two.
Embodiment 14: one of present embodiment and embodiment one to ten three unlike: in step 2 then depositing system radio-frequency power be 125W, pressure deposits under be 400Pa ~ 800Pa and temperature being 200 DEG C ~ 600 DEG C conditions, sedimentation time is 1min ~ 10min.Other is identical with embodiment one to ten three.
Embodiment 15: one of present embodiment and embodiment one to ten four unlike: in step 2 then depositing system radio-frequency power be 50W ~ 200W, pressure deposits under be 400Pa ~ 800Pa and temperature being 200 DEG C ~ 600 DEG C conditions, sedimentation time is 6min.Other is identical with embodiment one to ten four.
Embodiment 16: present embodiment and one of embodiment one to ten five unlike: in step one, in 10min ~ 30min, by temperature most 300 DEG C ~ 500 DEG C, other is identical with embodiment one to ten five.
Following examples are adopted to verify beneficial effect of the present invention:
Embodiment one:
The preparation method of a kind of amorphous carbon described in the present embodiment/vertical graphene combination electrode material, specifically carries out according to following steps:
One, the collector material of vertical Graphene is had on surface to be placed in plasma enhanced chemical vapor deposition vacuum plant, being evacuated to pressure is 5Pa, be that 20sccm passes into argon gas with gas flow, vacuum pumping rate is regulated to be controlled by pressure in plasma enhanced chemical vapor deposition vacuum plant as 200Pa, and under pressure is 200Pa and argon gas atmosphere, by temperature most 500 DEG C in 20min;
Two, methane gas is passed into, the gas flow controlling argon gas is 5sccm, the gas flow controlling methane gas is 50sccm, then vacuum pumping rate is regulated to be controlled by pressure in plasma enhanced chemical vapor deposition vacuum plant as 500Pa, then depositing system radio-frequency power be 175W, pressure deposits under be 500Pa and temperature being 500 DEG C of conditions, sedimentation time is 10min;
Three, after deposition terminates, close radio-frequency power supply and heating power supply, stopping passing into methane gas, under an argon atmosphere, is 5 DEG C/s with cooling rate, cool to room temperature, namely obtains amorphous carbon/vertical graphene combination electrode material.
Surface described in step one has the collector material of vertical Graphene specifically to prepare according to the following steps: electrode material is placed in plasma enhanced chemical vapor deposition vacuum plant, be evacuated to below 5Pa, pass into argon gas and methane gas, the gas flow regulating methane gas is 15sccm, the gas flow regulating argon gas is 75sccm, pressure in plasma enhanced chemical vapor deposition vacuum plant is regulated to be 500Pa, then radio-frequency power be 175W, temperature deposits under be 650 DEG C and pressure being the condition of 500Pa, sedimentation time is 40min;
Described collector material is metallic nickel.
Fig. 1 is the scanning electron microscope (SEM) photograph of amorphous carbon/vertical graphene combination electrode material prepared by embodiment one; As seen from the figure, amorphous carbon is evenly distributed on graphene film.
Concentration is the angle of wetting on amorphous carbon/vertical graphene combination electrode material of preparing at the present embodiment of the KOH electrolyte of 6 mol/L is 75 °, and amorphous carbon/vertical graphene combination electrode material prepared by the present embodiment is the ratio capacitance value in the KOH electrolyte of 6 mol/L in concentration is 525 μ F/cm
2.
Claims (10)
1. a preparation method for amorphous carbon/vertical graphene combination electrode material, is characterized in that it carries out according to following steps:
One, the collector material of vertical Graphene is had on surface to be placed in plasma enhanced chemical vapor deposition vacuum plant, being evacuated to pressure is 5Pa, be that 20sccm ~ 40sccm passes into argon gas with gas flow, vacuum pumping rate is regulated to be controlled by pressure in plasma enhanced chemical vapor deposition vacuum plant as 200Pa ~ 400Pa, and under pressure is 200Pa ~ 400Pa and argon gas atmosphere, by temperature most 200 DEG C ~ 600 DEG C in 10min ~ 30min;
Two, methane gas is passed into, the gas flow controlling argon gas is 1sccm ~ 10sccm, the gas flow controlling methane gas is 5sccm ~ 50sccm, then vacuum pumping rate is regulated to be controlled by pressure in plasma enhanced chemical vapor deposition vacuum plant as 400Pa ~ 800Pa, then depositing system radio-frequency power be 50W ~ 200W, pressure deposits under be 400Pa ~ 800Pa and temperature being 200 DEG C ~ 600 DEG C conditions, sedimentation time is 1min ~ 10min;
Three, after deposition terminates, close radio-frequency power supply and heating power supply, stop passing into methane gas, under an argon atmosphere, with cooling rate be 5 DEG C/s ~ 10 DEG C/s, cool to room temperature, namely obtains amorphous carbon/vertical graphene combination electrode material.
2. the preparation method of a kind of amorphous carbon according to claim 1/vertical graphene combination electrode material, it is characterized in that the surface described in step one has the collector material of vertical Graphene specifically to prepare according to the following steps: electrode material is placed in plasma enhanced chemical vapor deposition vacuum plant, be evacuated to below 5Pa, pass into argon gas and methane gas, the gas flow regulating methane gas is 5sccm ~ 20sccm, the gas flow regulating argon gas is 50sccm ~ 100sccm, pressure in plasma enhanced chemical vapor deposition vacuum plant is regulated to be 200Pa ~ 900Pa, then be 50W ~ 200W at radio-frequency power, temperature is 500 DEG C ~ 800 DEG C and pressure is deposit under the condition of 200Pa ~ 900Pa, sedimentation time is 5min ~ 60min,
Described collector material is metallic nickel, nickel foam, metal platinum, stainless steel substrates or graphite paper.
3. the preparation method of a kind of amorphous carbon according to claim 1/vertical graphene combination electrode material, the gas flow that it is characterized in that controlling in step 2 argon gas is 5sccm ~ 10sccm.
4. the preparation method of a kind of amorphous carbon according to claim 1/vertical graphene combination electrode material, the gas flow that it is characterized in that controlling in step 2 methane gas is 10sccm ~ 50sccm.
5. the preparation method of a kind of amorphous carbon according to claim 1/vertical graphene combination electrode material, is characterized in that then regulating vacuum pumping rate to control pressure in plasma enhanced chemical vapor deposition vacuum plant for 400Pa ~ 700Pa in step 2.
6. the preparation method of a kind of amorphous carbon according to claim 1/vertical graphene combination electrode material, to it is characterized in that in step 2 then depositing system radio-frequency power be 100W ~ 175W, pressure deposits under be 400Pa ~ 800Pa and temperature being 200 DEG C ~ 600 DEG C conditions, sedimentation time is 1min ~ 10min.
7. the preparation method of a kind of amorphous carbon according to claim 1/vertical graphene combination electrode material, to it is characterized in that in step 2 then depositing system radio-frequency power be 50W ~ 200W, pressure deposits under be 400Pa ~ 800Pa and temperature being 200 DEG C ~ 600 DEG C conditions, sedimentation time is 2min ~ 10min.
8. the preparation method of a kind of amorphous carbon according to claim 1/vertical graphene combination electrode material, to is characterized in that temperature most 300 DEG C in step one in 10min ~ 30min.
9. the preparation method of a kind of amorphous carbon according to claim 1/vertical graphene combination electrode material, to is characterized in that temperature most 500 DEG C in step one in 10min ~ 30min.
10. the preparation method of a kind of amorphous carbon according to claim 1/vertical graphene combination electrode material, to is characterized in that temperature most 310 DEG C ~ 490 DEG C in step one in 10min ~ 30min.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101831633A (en) * | 2010-04-21 | 2010-09-15 | 清华大学 | Method for preparing composite film of graphene and amorphous carbon |
| CN103183344A (en) * | 2013-04-24 | 2013-07-03 | 哈尔滨工业大学 | Method for low-temperature and efficient preparation of large-size graphene |
| CN103613094A (en) * | 2013-11-28 | 2014-03-05 | 华中科技大学 | Method for preparing graphene and porous amorphous carbon films simultaneously |
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| CN101831633A (en) * | 2010-04-21 | 2010-09-15 | 清华大学 | Method for preparing composite film of graphene and amorphous carbon |
| CN103183344A (en) * | 2013-04-24 | 2013-07-03 | 哈尔滨工业大学 | Method for low-temperature and efficient preparation of large-size graphene |
| CN103613094A (en) * | 2013-11-28 | 2014-03-05 | 华中科技大学 | Method for preparing graphene and porous amorphous carbon films simultaneously |
| CN104064378A (en) * | 2014-07-16 | 2014-09-24 | 哈尔滨工业大学 | Method for manufacturing low-cost three-dimensional-structure graphene-aluminum supercapacitor composite electrode material |
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