CN104576083A - Preparation method for supercapacitor made of graphene nanoscrolls - Google Patents
Preparation method for supercapacitor made of graphene nanoscrolls Download PDFInfo
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- CN104576083A CN104576083A CN201510006310.9A CN201510006310A CN104576083A CN 104576083 A CN104576083 A CN 104576083A CN 201510006310 A CN201510006310 A CN 201510006310A CN 104576083 A CN104576083 A CN 104576083A
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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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- 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
- H01G11/36—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
- 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 invention discloses a preparation method for a supercapacitor made of graphene nanoscrolls. The method includes the following steps that 1, oxidized graphene raw materials are dissolved in water to obtain oxidized graphene solutions with the mass fraction of 0%-1%; 2, the oxidized graphene solutions are reduced to be black through a chemical reduction method and uniformly dispersed; 3, the reduced oxidized graphene solutions are transferred into a freeze dryer to be freeze-dried after being quickly frozen through liquid nitrogen or liquid ammonia to be solidified; 4, deep reduction is conducted on a freeze-dried sample through a chemical reduction method or a high-temperature heat treatment method to obtain the graphene nanoscrolls; 5, the graphene nanoscrolls serve as two electrodes of the capacitor and are combined into the frequently-used dual-electrode capacitor. A high conversion rate and large-scale preparation of the graphene nanoscrolls can be achieved, operation is simple and convenient, cost is low, user-friendliness is achieved, specific capacitance and energy density of the supercapacitor are high, the supercapacitor has good crushing resistance, and the method can be used in the fields of high-energy density energy storage materials, devices and the like.
Description
Technical field
The present invention relates to the preparation method of a kind of graphene nano volume ultracapacitor.
Background technology
Graphene nano volume is a kind of new carbon with one dimension open tubular topological structure.Its structure can regard the 1-dimention nano pipe with helical structure that two-dimensional graphene sheet is formed through continuous crisping as.This structure differing from carbon nano-tube gives the character that graphene nano rolls up some uniquenesses, as guest molecule load capacity, high mechanical properties, high conductivity and thermal conductivity etc.Therefore, graphene nano twists in hydrogen storage material, there is broad prospect of application energy storage material, sensor aspect.
The research of graphene nano volume is still in the starting stage at present, prepares the research puzzle that graphene nano volume remains academia, only has after can successfully preparing in a large number, really could realize its application how in a large number, high conversion.
Ultracapacitor, also known as electrochemical capacitor, becomes both another significant energy storing modes after lithium rechargeable battery with the energy density of its superelevation, power density, cyclical stability.The energy storage mechnism of ultracapacitor is generally divided into two kinds: electric double layer capacitance and fake capacitance.Electric double layer capacitance produced by electrode/electrolyte interface accumulation of electrostatic charge, and therefore the size of electric double layer capacitance depends on the electrode surface area size being conducive to electrolyte ion and entering; Fake capacitance by the electroactive material of tool on electrode, reversible faradaic electrochemical reaction occurs to produce, and both depended on the theoretical electric capacity of active material itself, also depended on surface topography and the conductivity degree of electrode.Graphene nano volume, as material with carbon element, while the electric double layer capacitance with common material with carbon element, owing to having unique hatch frame, is easy to other object particles of load, can increases the fake capacitance of material.
Summary of the invention
The object of the invention is to overcome the deficiencies in the prior art, provide graphene nano to roll up the preparation method of ultracapacitor, improve the chemical property of ultracapacitor.
The object of the invention is to be achieved through the following technical solutions: a kind of preparation method of graphene nano volume ultracapacitor, step is as follows:
(1) area is greater than 0.01 μm
2graphene oxide is water-soluble, obtains the graphene oxide solution that mass fraction is 0.005 ~ 1%;
(2) with chemical reduction method above-mentioned graphene oxide solution be reduced to black and be uniformly dispersed;
(3) the graphene solution liquid nitrogen after step 2 being reduced or cryotherapy with liquid nitrogen, to after solidifying, are transferred to freeze-drying in freeze drier;
(4) by chemical reduction method or high-temperature heat treatment method, the product after step 3 freeze-drying is fully reduced, obtain graphene nano volume;
(5) using graphene nano volume as capacitor the two poles of the earth, bipolar electrode capacitor is assembled into.
Further, chemical reduction method in described step 4 is specially: be the graphene oxide 1-24 hour after the reducibility gas reduction freeze-drying of 50-160 DEG C by temperature, described reducibility gas comprises hydrazine hydrate steam, hydroiodic acid/acetic acid steam, hydroiodic acid/trifluoroacetic acid steam.
Further, the high-temperature heat treatment in described step 4 is specially: with the graphene oxide 1-12 hour of nitrogen, argon gas or hydrogen/argon gas mist after 800-1300 DEG C of reduction freeze-drying.
Disclosure sets forth a kind of preparation method of novel graphite alkene nanometer roll ultracapacitor.This graphene nano volume ultracapacitor, owing to having the one dimension tubular structure of the high-ratio surface sum carbon nano-tube of Graphene simultaneously, therefore while possessing the high specific capacitance due to carbon nano-tube, has again the compressive property and high rate performance that are better than Graphene.In addition it is easy to be combined with object particle, can improve ratio capacitance and the energy density of capacitor by introducing fake capacitance further.
Accompanying drawing explanation
Fig. 1 is the electron scanning micrograph of graphene nano volume;
Fig. 2 is the transmission electron microscope photo of graphene nano volume;
Fig. 3 is the cyclic voltammetry curve that embodiment 1 prepares graphene nano volume;
Fig. 4 is the constant current charge-discharge curve that embodiment 1 prepares graphene nano volume;
Fig. 5 is the cyclic voltammetry curve that embodiment 2 prepares graphene nano volume;
Fig. 6 is the constant current charge-discharge curve that embodiment 2 prepares graphene nano volume.
Embodiment
The step of the preparation method of graphene nano volume ultracapacitor is as follows:
(1) by water-soluble for graphene oxide raw material and stir, the graphene oxide solution of mass percentage below 1% is obtained; Wherein, graphene oxide sheet is of a size of 0.01 μm
2above arbitrary size, graphene oxide solution concentration is any concentration of mass percentage below 1%.
(2) with existing chemical reduction method, above-mentioned graphene oxide solution is reduced, obtain partial reduction graphene solution; Wherein, reducing agent can be the solution that hydrazine hydrate solution, hydroiodic acid solution, sodium ascorbate solution etc. have reproducibility.The concentration of recovery time, reduction temperature and reducing agent is determined by the reducing degree of graphene oxide solution, when graphene oxide solution be reduced to black but can dispersed, can stop without during some visual precipitation.
(3), after partial reduction graphene solution snap frozen extremely all being solidified, freeze-drying in freeze drier is transferred to; Cooling means is the freezing mode such as liquid nitrogen snap frozen, liquefied ammonia snap frozen;
(4) by chemical reduction method or high-temperature heat treatment method, the sample after freeze-drying is carried out drastic reduction, obtain graphene nano volume; Fully reducing the graphene oxide of freeze-drying with chemical reduction method is prior art, and chemical reducing agent can be the reproducibility steam such as hydrazine hydrate steam, hydroiodic acid/acetic acid steam, hydroiodic acid/trifluoroacetic acid steam; Wherein in hydroiodic acid/acetic acid steam, hydroiodic acid/trifluoroacetic acid steam, the proportionate relationship of hydroiodic acid and acetic acid and hydroiodic acid can be any ratio with the proportionate relationship of trifluoroacetic acid, and known from institute, the concentration of hydroiodic acid in mist is larger, reproducibility is stronger, and namely the recovery time is shorter.Reduction temperature is generally 50-160 DEG C, and the recovery time is generally 1-24 hour; Equally, the graphene oxide also existing technological means in capable territory of freeze-drying is fully reduced by high-temperature heat treatment method, such as, the graphene oxide 1-12 hour of nitrogen, argon gas, hydrogen/argon gas mist after 800-1300 DEG C of reduction freeze-drying can be used, wherein hydrogen/argon gas mist is commercial gas, and volume ratio is between the two generally hydrogen/argon gas=5/95.
(5) using graphene nano volume as capacitor the two poles of the earth, bipolar electrode capacitor is assembled into.Electrolyte wherein can be aqueous phase electrolyte, organic bath, ionic liquid etc.; Such as potassium hydroxide solution, sulfuric acid solution; Concentration can be any concentration.
Below by embodiment, the present invention is specifically described; the present embodiment is only for the present invention is described further; limiting the scope of the invention can not be interpreted as; those skilled in the art's content according to the present invention makes some nonessential change and adjustment, all belongs to protection scope of the present invention.
embodiment 1:
1) it is 100 μm by lamella average-size
2graphene oxide raw material is water-soluble and stir, and obtains the graphene oxide solution that mass percentage is 0.008%;
2) above-mentioned graphene oxide solution is placed in 60
oc oil bath, add 10 μ L mass fractions be 85% hydrazine hydrate solution be reduced to black, and be uniformly dispersed, the precipitation that is invisible to the naked eye (about 30min), stops reduction, obtains partial reduction graphene solution;
3) partial reduction graphene solution is immersed liquid nitrogen snap frozen and be transferred to freeze-drying in freeze drier after all solidifying;
4) by the sample after freeze-drying in 100
oc hydroiodic acid/acetic acid steam (V/V=1:1) reduces 12h, obtains graphene nano volume; As depicted in figs. 1 and 2, graphene nano volume has open coil structure, and nanometer roll diameter is at about 200nm, and length is not at several microns to hundreds of micron etc.
5) using graphene nano volume as capacitor the two poles of the earth, 1mol/L sulfuric acid solution is electrolyte, is assembled into bipolar electrode capacitor.
As shown in Figure 3, the ratio capacitance that this ultracapacitor utilizes cyclic voltammetry to calculate under 10mV/s sweep speed is 70F/g, and energy density is 1.6 Wh/kg, is 47% by the capacity retention of 10mV/s to 1000mV/s; As shown in Figure 4, the ratio capacitance utilizing constant current charge-discharge method to calculate under 0.5A/g current density is 64.5F/g, and energy density is 1.4 Wh/kg, is 71% by the capacity retention of 0.5A/g to 10A/g.
embodiment 2:
1) it is 10000 μm by lamella average-size
2graphene oxide raw material is water-soluble and stir, and obtains the graphene oxide solution that mass percentage is 0.01%;
2) above-mentioned graphene oxide solution is placed in 70
oc oil bath, adds 50 μ L hydroiodic acid solution (mass fraction is 15%) and is reduced to black, and be uniformly dispersed, the precipitation that is invisible to the naked eye (about 20min), stops reduction, obtains partial reduction graphene solution;
3) partial reduction graphene solution is immersed liquid nitrogen snap frozen and be transferred to freeze-drying in freeze drier after all solidifying;
4) by the sample after freeze-drying in 90
oc hydrazine hydrate steam reduction 24h, obtains graphene nano volume;
5) using graphene nano volume as capacitor the two poles of the earth, 6mol/L potassium hydroxide solution is electrolyte, is assembled into bipolar electrode capacitor.
As shown in Figure 5, the ratio capacitance that this ultracapacitor utilizes cyclic voltammetry to calculate under 10mV/s sweep speed is 73F/g, and energy density is 1.6 Wh/kg, is 47% by the capacity retention of 10mV/s to 1000mV/s; As shown in Figure 6, the ratio capacitance utilizing constant current charge-discharge method to calculate under 0.5A/g current density is 64 F/g, and energy density is 1.4 Wh/kg, is 73% by the capacity retention of 0.5A/g to 10A/g.
embodiment 3:
1) it is 0.1 μm by lamella average-size
2graphene oxide raw material is water-soluble and stir, and obtains the graphene oxide solution that mass percentage is 0.9%;
2) above-mentioned graphene oxide solution is placed in 70
oc oil bath, adds 60 μ L sodium ascorbate solutions (mass fraction is 15%) and is reduced to black, and be uniformly dispersed, the precipitation that is invisible to the naked eye (about 25min), stops reduction, obtains partial reduction graphene solution;
3) partial reduction graphene solution is immersed liquefied ammonia snap frozen and be transferred to freeze-drying in freeze drier after all solidifying;
4) by the sample after freeze-drying in 160
oc hydroiodic acid/trifluoroacetic acid steam (V/V=2:1) reduces 1h, obtains graphene nano volume;
5) using graphene nano volume as capacitor the two poles of the earth, 4mol/L potassium hydroxide solution is electrolyte, is assembled into bipolar electrode capacitor.
The ratio capacitance that this ultracapacitor utilizes cyclic voltammetry to calculate under 10mV/s sweep speed is 64F/g, and energy density is 1.5Wh/kg, is 54% by the capacity retention of 10mV/s to 1000mV/s; The ratio capacitance utilizing constant current charge-discharge method to calculate under 0.5A/g current density is 60F/g, and energy density is 1.5Wh/kg, is 76% by the capacity retention of 0.5A/g to 10A/g.
embodiment 4:
1) it is 10 μm by lamella average-size
2graphene oxide raw material is water-soluble and stir, and obtains the graphene oxide solution that mass percentage is 0.1%;
2) above-mentioned graphene oxide solution is placed in 70
oc oil bath, adds 60 μ L hydroiodic acid solution (mass fraction is 25%) and is reduced to black, and be uniformly dispersed, the precipitation that is invisible to the naked eye (about 5min), stops reduction, obtains partial reduction graphene solution;
3) partial reduction graphene solution is immersed liquefied ammonia snap frozen and be transferred to freeze-drying in freeze drier after all solidifying;
4) by the sample after freeze-drying in 50
oc hydroiodic acid/acetic acid steam (V/V=1:2) reductase 12 4h, obtains graphene nano volume;
5) using graphene nano volume as capacitor the two poles of the earth, 1mol/L sulfuric acid solution is electrolyte, is assembled into bipolar electrode capacitor.
The ratio capacitance that this ultracapacitor utilizes cyclic voltammetry to calculate under 10mV/s sweep speed is 57.4F/g, and energy density is 1.6Wh/kg, is 57% by the capacity retention of 10mV/s to 1000mV/s; The ratio capacitance utilizing constant current charge-discharge method to calculate under 0.5A/g current density is 62F/g, and energy density is 1.6Wh/kg, is 74% by the capacity retention of 0.5A/g to 10A/g.
embodiment 5:
1) it is 10000 μm by lamella average-size
2graphene oxide raw material is water-soluble and stir, and obtains the graphene oxide solution that mass percentage is 0.005%;
2) above-mentioned graphene oxide solution is placed in 60
oc oil bath, add 20 μ L concentration be 85% hydrazine hydrate solution be reduced to black, and be uniformly dispersed, the precipitation that is invisible to the naked eye (about 30min), stops reduction, obtains partial reduction graphene solution;
3) partial reduction graphene solution is immersed liquid nitrogen snap frozen and be transferred to freeze-drying in freeze drier after all solidifying;
4) by the sample after freeze-drying under hydrogen/argon gas mixed atmosphere 1300
oc reduces 1h, obtains graphene nano volume;
5) using graphene nano volume as capacitor the two poles of the earth, 1mol/L sulfuric acid solution is electrolyte, is assembled into bipolar electrode capacitor.
The ratio capacitance that this ultracapacitor utilizes cyclic voltammetry to calculate under 10mV/s sweep speed is 96F/g, and energy density is 2.1 Wh/kg, is 55% by the capacity retention of 10mV/s to 1000mV/s; The ratio capacitance utilizing constant current charge-discharge method to calculate under 1A/g current density is 78.6 F/g, and energy density is 1.7 Wh/kg, is 96% by the capacity retention of 0.5A/g to 10A/g.
embodiment 6:
1) it is 50 μm by lamella average-size
2graphene oxide raw material is water-soluble and stir, and obtains the graphene oxide solution that mass percentage is 0.05%;
2) above-mentioned graphene oxide solution is placed in 60
oc oil bath, add 20 μ L concentration be 85% hydrazine hydrate solution be reduced to black, and be uniformly dispersed, the precipitation that is invisible to the naked eye (about 30min), stops reduction, obtains partial reduction graphene solution;
3) partial reduction graphene solution is immersed liquid nitrogen snap frozen and be transferred to freeze-drying in freeze drier after all solidifying;
4) by the sample after freeze-drying in nitrogen 800
oc reduces 12h, obtains graphene nano volume;
5) using graphene nano volume as capacitor the two poles of the earth, 1mol/L sulfuric acid solution is electrolyte, is assembled into bipolar electrode capacitor.
The ratio capacitance that this ultracapacitor utilizes cyclic voltammetry to calculate under 10mV/s sweep speed is 96F/g, and energy density is 2.1 Wh/kg, is 55% by the capacity retention of 10mV/s to 1000mV/s; The ratio capacitance utilizing constant current charge-discharge method to calculate under 1A/g current density is 78.6 F/g, and energy density is 1.7 Wh/kg, is 96% by the capacity retention of 0.5A/g to 10A/g.
embodiment 7:
1) it is 0.25 μm by lamella average-size
2graphene oxide raw material is water-soluble and stir, and obtains the graphene oxide solution that mass percentage is 0.005%;
2) above-mentioned graphene oxide solution is placed in 70
oc oil bath, 20 μ L mass fractions be 85% hydrazine hydrate solution be reduced to black, and be uniformly dispersed, the precipitation that is invisible to the naked eye (about 45min), stops reduction, obtains partial reduction graphene solution;
3) partial reduction graphene solution is immersed liquid nitrogen snap frozen and be transferred to freeze-drying in freeze drier after all solidifying;
4) by the sample after freeze-drying in 90
oc hydroiodic acid/acetic acid steam reduction 12h, then in 120
oc vacuumize 12h obtains graphene nano volume;
5) using graphene nano volume as capacitor the two poles of the earth, 1mol/L sulfuric acid solution is electrolyte, is assembled into bipolar electrode capacitor.
The ratio capacitance that this ultracapacitor utilizes cyclic voltammetry to calculate under 10mV/s sweep speed is 78F/g, and energy density is 1.7 Wh/kg, is 31% by the capacity retention of 10mV/s to 1000mV/s; The ratio capacitance utilizing constant current charge-discharge method to calculate under 0.5A/g current density is 68.3 F/g, and energy density is 1.5 Wh/kg, is 62% by the capacity retention of 0.5A/g to 10A/g.
Claims (3)
1. a preparation method for graphene nano volume ultracapacitor, it is characterized in that, its step is as follows:
(1) area is greater than 0.01 μm
2graphene oxide is water-soluble, obtains the graphene oxide solution that mass fraction is 0.005 ~ 1%;
(2) be reduced to black by the graphene oxide solution that step 1 obtains by chemical reduction method and be uniformly dispersed;
(3) the graphene solution liquid nitrogen after step 2 being reduced or cryotherapy with liquid nitrogen, to after solidifying, are transferred to freeze-drying in freeze drier;
(4) by chemical reduction method or high-temperature heat treatment method, the product after step 3 freeze-drying is fully reduced, obtain graphene nano volume;
(5) using graphene nano volume as capacitor the two poles of the earth, bipolar electrode capacitor is assembled into.
2. preparation method according to claim 1, it is characterized in that, chemical reduction method in described step 4 is specially: be the graphene oxide 1-24 hour after the reducibility gas reduction freeze-drying of 50-160 DEG C by temperature, described reducibility gas is selected from hydrazine hydrate steam, hydroiodic acid/acetic acid steam, hydroiodic acid/trifluoroacetic acid steam.
3. preparation method according to claim 1, is characterized in that, the high-temperature heat treatment in described step 4 is specially: with the graphene oxide 1-12 hour of nitrogen, argon gas or hydrogen/argon gas mist after 800-1300 DEG C of reduction freeze-drying.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106698403A (en) * | 2017-01-06 | 2017-05-24 | 南京工业大学 | Method of preparing graphene roll in large area |
| CN106744899A (en) * | 2017-01-09 | 2017-05-31 | 南京工业大学 | A kind of preparation method of two-dimensional material nanometer roll |
| CN113697798A (en) * | 2021-08-11 | 2021-11-26 | 哈尔滨工业大学 | Preparation method of magnetic graphene nano wave absorbing material |
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| CN102976316A (en) * | 2012-12-19 | 2013-03-20 | 中国科学院宁波材料技术与工程研究所 | Preparation method of graphene roll |
| CN104140096A (en) * | 2014-07-25 | 2014-11-12 | 同济大学 | Method for manufacturing graphene roll |
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| CN102976316A (en) * | 2012-12-19 | 2013-03-20 | 中国科学院宁波材料技术与工程研究所 | Preparation method of graphene roll |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106698403A (en) * | 2017-01-06 | 2017-05-24 | 南京工业大学 | Method of preparing graphene roll in large area |
| CN106698403B (en) * | 2017-01-06 | 2019-01-18 | 南京工业大学 | A kind of method of large area preparation graphene roll |
| CN106744899A (en) * | 2017-01-09 | 2017-05-31 | 南京工业大学 | A kind of preparation method of two-dimensional material nanometer roll |
| CN113697798A (en) * | 2021-08-11 | 2021-11-26 | 哈尔滨工业大学 | Preparation method of magnetic graphene nano wave absorbing material |
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Application publication date: 20150429 |