CN107316750A - A kind of graphene-based electrode material for super capacitor of high conductivity and preparation method thereof - Google Patents
A kind of graphene-based electrode material for super capacitor of high conductivity and preparation method thereof Download PDFInfo
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- CN107316750A CN107316750A CN201710686087.6A CN201710686087A CN107316750A CN 107316750 A CN107316750 A CN 107316750A CN 201710686087 A CN201710686087 A CN 201710686087A CN 107316750 A CN107316750 A CN 107316750A
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- graphene
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- electrode 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
- H01G11/24—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 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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- 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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- 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 the graphene-based electrode material for super capacitor and preparation method of a kind of high conductivity, it is prepared from by the raw material of following parts by weight:3 ~ 5 parts of activated carbon, 1 ~ 3 point of titania nanotube, 2 ~ 5 parts of graphene, 4 ~ 6 parts of diisostearoyl ethylene titanate, 40 ~ 50 parts of ethyl acetate, 0.2 ~ 0.6 part of polyacrylonitrile, 10 ~ 15 parts of dimethylformamide.Electrode for super capacitor material produced by the present invention has good chemical stability and electrical conductivity, specific capacitance and energy density are higher simultaneously, activated carbon and titania nanotube and graphene after processing have good dispersiveness and adhesiveness, make full use of the loose structure of graphene, improve the utilization of specific surface area, the electrical conductivity of activated carbon and graphene is fully improved, improves the surface wettability of graphene, is a kind of good electrode material of combination property.
Description
Technical field
The present invention relates to the graphene-based ultracapacitor of electrochemical material preparation field, more particularly to a kind of high conductivity
Electrode material and preparation method thereof.
Background technology
Ultracapacitor is a kind of energy storaging product of the great market competitiveness, it is possible to achieve quick charge, heavy-current discharge,
And with the charge lifetimes of more than 100,000 times, occupy epochmaking status in some needs applications of high-multiplying power discharge in short-term.
Electrode is the core component of ultracapacitor, and electrode material directly influences the performance of ultracapacitor, mesh
Preceding conventional electrode material is activated carbon.
With the development of nano material, the two-dimensional graphene material with lamellar structure causes electrochemical material field
Extensive concern.A variety of researchs are found, it is combined with electrode material, the performance of ultracapacitor can be lifted.But due to graphite
The two-dimensional nano lamellar structure of alkene makes it easily reunite together, and the performance advantage of graphene is difficult to be given full play of.Cause
This, often shows relatively low electrical conductivity and surface wettability, to a certain degree by graphene for the capacitor electrode material of main material
On limit application of the graphene in electrode material for super capacitor.
The content of the invention
In view of the shortcomings of the prior art, the invention provides a kind of high conductivity and good capacitive graphene-based super electricity
Container electrode material and preparation method thereof.
Solve the technical scheme that uses of above-mentioned technical problem for:A kind of graphene-based electrode of super capacitor of high conductivity
Material, is prepared from by the raw material of following parts by weight:3 ~ 5 parts of activated carbon, 1 ~ 3 point of titania nanotube, graphene 2 ~ 5
Part, 4 ~ 6 parts of diisostearoyl ethylene titanate, 40 ~ 50 parts of ethyl acetate, 0.2 ~ 0.6 part of polyacrylonitrile, dimethylformamide
10 ~ 15 parts.
Preferably, a kind of graphene-based electrode material for super capacitor of described high conductivity, by following parts by weight
Several raw materials are prepared from:4 parts of activated carbon, 2 points of titania nanotube, 3 parts of graphene, diisostearoyl ethylene titanate
5 parts, 45 parts of ethyl acetate, 0.4 part of polyacrylonitrile, 12 parts of dimethylformamide.
A kind of preparation method of the graphene-based electrode material for super capacitor of described high conductivity, including following step
Suddenly:
(1)It is placed in after activated carbon and titania nanotube are mixed in the acid solution of 10 ~ 15 times of amounts, 10 ~ 20min of sonic oscillation
After be warming up to 8 ~ 10h of insulated and stirred after 60 ~ 70 DEG C, obtain mixed liquor, add the deionized waters of 2 ~ 3 times of mixing liquid measures and stand 8 ~
It is washed with deionized after 10h, filtering to neutrality, drying process obtains mixture one;
(2)By step(1)The mixture one of gained is placed in the mixed solution of diisostearoyl ethylene titanate and ethyl acetate
In, 6 ~ 8h is stood after 1 ~ 2h of stirring, filters and dries solids, 1 ~ 2h is ground, 200 mesh sieves is crossed, obtains mixture two;
(3)Will under polyacrylonitrile and dimethylformamide normal temperature be well mixed, be then heated to 50 ~ 60 DEG C and add graphene surpass
30 ~ 60min of sound, then 1 ~ 2h of insulated and stirred, filters and removes solvent after being dried at 110 ~ 120 DEG C to constant weight, obtain modified graphite
Alkene;
(4)Strong step(2)The mixture two and step of gained(3)The modified graphene of gained is placed in mortar, and 2 ~ 4h of grinding is extremely
Uniformly, it is subsequently poured into mould, is heated to 120 ~ 130 DEG C, mould is positioned on electric tablet machine, it is hot under 10MPa pressure
Press after 30 ~ 40min, cooling and demolding, polished smooth the electrode obtained material with sand paper.
Further, step(1)Described in acid solution be the concentrated sulfuric acid and concentrated nitric acid mixed liquor, the concentrated sulfuric acid and concentrated nitric acid
Volume ratio is 2:1.
Compared with prior art, what the present invention possessed has the beneficial effect that:
Electrode for super capacitor material produced by the present invention has good chemical stability and electrical conductivity, at the same specific capacitance and
Energy density is higher, and the activated carbon and titania nanotube and graphene after processing have good dispersed and adhesion
Property, the loose structure of graphene is made full use of, the utilization of specific surface area is improved, the conductance of activated carbon and graphene is fully improved
Rate, improves the surface wettability of graphene, is a kind of good electrode material of combination property.
Embodiment
With reference to specific embodiment, the present invention is described further.Following examples are simply described to the present invention
The explanation of property, it is impossible to which protection scope of the present invention is limited with this.
Moreover, the raw material used in the present invention, is conventional commercially available prod unless otherwise required;Likewise, being made
Method is conventional production method unless otherwise required.
Embodiment 1:The graphene-based electrode material for super capacitor of a kind of high conductivity, by the raw material of following parts by weight
It is prepared from:4 parts of activated carbon, 2 points of titania nanotube, 3 parts of graphene, 5 parts of diisostearoyl ethylene titanate, acetic acid
45 parts of ethyl ester, 0.4 part of polyacrylonitrile, 12 parts of dimethylformamide.
A kind of preparation method of the graphene-based electrode material for super capacitor of described high conductivity, including following step
Suddenly:
(1)It is placed in the acid solution of 12 times of amounts, is heated up after sonic oscillation 15min after activated carbon and titania nanotube are mixed
Insulated and stirred 9h after to 65 DEG C, obtains mixed liquor, adds the deionized water of 2 times of mixing liquid measures and stands 9h, deionization is used after filtering
Water washing is to neutrality, and drying process obtains mixture one;
(2)By step(1)The mixture one of gained is placed in the mixed solution of diisostearoyl ethylene titanate and ethyl acetate
In, 7h is stood after stirring 1h, filters and dries solids, 2h is ground, 200 mesh sieves is crossed, obtains mixture two;
(3)It will be well mixed under polyacrylonitrile and dimethylformamide normal temperature, be then heated to 55 DEG C and add graphene ultrasound
45min, then insulated and stirred 2h, filters and removes solvent after being dried at 115 DEG C to constant weight, obtain modified graphene;
(4)Strong step(2)The mixture two and step of gained(3)The modified graphene of gained is placed in mortar, and 3h is to equal for grinding
It is even, it is subsequently poured into mould, is heated to 125 DEG C, mould is positioned on electric tablet machine, the hot pressing under 10MPa pressure
After 35min, cooling and demolding, the electrode obtained material is polished smooth with sand paper.
Further, step(1)Described in acid solution be the concentrated sulfuric acid and concentrated nitric acid mixed liquor, the concentrated sulfuric acid and concentrated nitric acid
Volume ratio is 2:1.
Embodiment 2:The graphene-based electrode material for super capacitor of a kind of high conductivity, by the raw material of following parts by weight
It is prepared from:3 parts of activated carbon, 1 point of titania nanotube, 2 parts of graphene, 4 parts of diisostearoyl ethylene titanate, acetic acid
40 parts of ethyl ester, 0. part of polyacrylonitrile, 10 parts of dimethylformamide.
A kind of preparation method of the graphene-based electrode material for super capacitor of described high conductivity, including following step
Suddenly:
(1)It is placed in the acid solution of 10 times of amounts, is heated up after sonic oscillation 10min after activated carbon and titania nanotube are mixed
Insulated and stirred 8h after to 60 DEG C, obtains mixed liquor, adds the deionized water of 2 times of mixing liquid measures and stands 8h, deionization is used after filtering
Water washing is to neutrality, and drying process obtains mixture one;
(2)By step(1)The mixture one of gained is placed in the mixed solution of diisostearoyl ethylene titanate and ethyl acetate
In, 6h is stood after stirring 1h, filters and dries solids, 1h is ground, 200 mesh sieves is crossed, obtains mixture two;
(3)It will be well mixed under polyacrylonitrile and dimethylformamide normal temperature, be then heated to 50 DEG C and add graphene ultrasound
30min, then insulated and stirred 1h, filters and removes solvent after being dried at 110 DEG C to constant weight, obtain modified graphene;
(4)Strong step(2)The mixture two and step of gained(3)The modified graphene of gained is placed in mortar, and 2h is to equal for grinding
It is even, it is subsequently poured into mould, is heated to 120 DEG C, mould is positioned on electric tablet machine, the hot pressing under 10MPa pressure
After 30min, cooling and demolding, the electrode obtained material is polished smooth with sand paper.
Further, step(1)Described in acid solution be the concentrated sulfuric acid and concentrated nitric acid mixed liquor, the concentrated sulfuric acid and concentrated nitric acid
Volume ratio is 2:1.
Embodiment 3:The graphene-based electrode material for super capacitor of a kind of high conductivity, by the raw material of following parts by weight
It is prepared from:5 parts of activity, 3 points of titania nanotube, 5 parts of graphene, 6 parts of diisostearoyl ethylene titanate, acetic acid second
50 parts of ester, 0.6 part of polyacrylonitrile, 15 parts of dimethylformamide.
A kind of preparation method of the graphene-based electrode material for super capacitor of described high conductivity, including following step
Suddenly:
(1)It is placed in the acid solution of 15 times of amounts, is heated up after sonic oscillation 20min after activated carbon and titania nanotube are mixed
Insulated and stirred 10h after to 70 DEG C, obtains mixed liquor, and the deionized water for adding 3 times of mixing liquid measures simultaneously stands 10h, spent after filtering from
Sub- water washing is to neutrality, and drying process obtains mixture one;
(2)By step(1)The mixture one of gained is placed in the mixed solution of diisostearoyl ethylene titanate and ethyl acetate
In, 8h is stood after stirring 2h, filters and dries solids, 2h is ground, 200 mesh sieves is crossed, obtains mixture two;
(3)It will be well mixed under polyacrylonitrile and dimethylformamide normal temperature, be then heated to 60 DEG C and add graphene ultrasound
60min, then insulated and stirred 2h, filters and removes solvent after being dried at 120 DEG C to constant weight, obtain modified graphene;
(4)Strong step(2)The mixture two and step of gained(3)The modified graphene of gained is placed in mortar, and 4h is to equal for grinding
It is even, it is subsequently poured into mould, is heated to 130 DEG C, mould is positioned on electric tablet machine, the hot pressing under 10MPa pressure
After 40min, cooling and demolding, the electrode obtained material is polished smooth with sand paper.
Further, step(1)Described in acid solution be the concentrated sulfuric acid and concentrated nitric acid mixed liquor, the concentrated sulfuric acid and concentrated nitric acid
Volume ratio is 2:1.
Embodiment 4:The graphene-based electrode material for super capacitor of a kind of high conductivity, by the raw material of following parts by weight
It is prepared from:3 parts of activated carbon, 3 points of titania nanotube, 2 parts of graphene, 6 parts of diisostearoyl ethylene titanate, acetic acid
40 parts of ethyl ester, 0.6 part of polyacrylonitrile, 10 parts of dimethylformamide.
A kind of preparation method of the graphene-based electrode material for super capacitor of described high conductivity, phase specific steps are same
Embodiment 1.
Embodiment 5:The graphene-based electrode material for super capacitor of a kind of high conductivity, by the raw material of following parts by weight
It is prepared from:4 parts of activated carbon, 1 point of titania nanotube, 5 parts of graphene, 5 parts of diisostearoyl ethylene titanate, poly- third
0.5 part of alkene nitrile, 13 parts of dimethylformamide.
A kind of preparation method of the graphene-based electrode material for super capacitor of described high conductivity, phase specific steps are same
Embodiment 1.
Have higher electrical conductivity, energy density and power close using ultracapacitor made from the electrode material of the present invention
Degree, while chemical stability is good, with more superior performance.
Should be it is again noted that content described in above-described embodiment be only presently preferred embodiments of the present invention, it is impossible to be considered as
Practical range for limiting the present invention.All equivalent changes made according to the present patent application scope or improvement, all should still be belonged to
Within protection scope of the present invention.
Claims (4)
1. a kind of graphene-based electrode material for super capacitor of high conductivity, it is characterised in that:By the original of following parts by weight
Material is prepared from:3 ~ 5 parts of activated carbon, 1 ~ 3 point of titania nanotube, 2 ~ 5 parts of graphene, diisostearoyl ethylene titanate
4 ~ 6 parts, 40 ~ 50 parts of ethyl acetate, 0.2 ~ 0.6 part of polyacrylonitrile, 10 ~ 15 parts of dimethylformamide.
2. a kind of graphene-based electrode material for super capacitor of high conductivity according to claim 1, it is characterised in that:
It is prepared from by the raw material of following parts by weight:4 parts of activated carbon, 2 points of titania nanotube, 3 parts of graphene, two isostearoyls
5 parts of base metatitanic acid second diester, 45 parts of ethyl acetate, 0.4 part of polyacrylonitrile, 12 parts of dimethylformamide.
3. a kind of preparation method of the graphene-based electrode material for super capacitor of high conductivity described in claim 1 or 2, its
It is characterised by, comprises the following steps:
(1)It is placed in after activated carbon and titania nanotube are mixed in the acid solution of 10 ~ 15 times of amounts, 10 ~ 20min of sonic oscillation
After be warming up to 8 ~ 10h of insulated and stirred after 60 ~ 70 DEG C, obtain mixed liquor, add the deionized waters of 2 ~ 3 times of mixing liquid measures and stand 8 ~
It is washed with deionized after 10h, filtering to neutrality, drying process obtains mixture one;
(2)By step(1)The mixture one of gained is placed in the mixed solution of diisostearoyl ethylene titanate and ethyl acetate
In, 6 ~ 8h is stood after 1 ~ 2h of stirring, filters and dries solids, 1 ~ 2h is ground, 200 mesh sieves is crossed, obtains mixture two;
(3)Will under polyacrylonitrile and dimethylformamide normal temperature be well mixed, be then heated to 50 ~ 60 DEG C and add graphene surpass
30 ~ 60min of sound, then 1 ~ 2h of insulated and stirred, filters and removes solvent after being dried at 110 ~ 120 DEG C to constant weight, obtain modified graphite
Alkene;
(4)Strong step(2)The mixture two and step of gained(3)The modified graphene of gained is placed in mortar, and 2 ~ 4h of grinding is extremely
Uniformly, it is subsequently poured into mould, is heated to 120 ~ 130 DEG C, mould is positioned on electric tablet machine, it is hot under 10MPa pressure
Press after 30 ~ 40min, cooling and demolding, polished smooth the electrode obtained material with sand paper.
4. a kind of preparation method of the graphene-based electrode material for super capacitor of high conductivity according to claim 3,
It is characterized in that:Step(1)Described in acid solution be the concentrated sulfuric acid and concentrated nitric acid mixed liquor, the volume ratio of the concentrated sulfuric acid and concentrated nitric acid
For 2:1.
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
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CN109741963A (en) * | 2019-02-15 | 2019-05-10 | 铜陵市启动电子制造有限责任公司 | A kind of high power density recombiner condenser electrode and preparation method thereof |
CN114743800A (en) * | 2022-04-25 | 2022-07-12 | 武夷学院 | Preparation method of polyacrylic acid/graphene-based flexible electrode material |
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CN106252089A (en) * | 2016-08-03 | 2016-12-21 | 代长华 | A kind of electrode material for super capacitor and preparation method thereof |
CN106486290A (en) * | 2016-11-08 | 2017-03-08 | 铜陵市启动电子制造有限责任公司 | A kind of titanium manganese blending modification shitosan polypyrrole charcoal combination electrode material |
CN106683897A (en) * | 2016-12-10 | 2017-05-17 | 宁国市大荣电器有限公司 | Modified graphene supercapacitor electrode material |
CN106783212A (en) * | 2016-11-22 | 2017-05-31 | 张家港智电芳华蓄电研究所有限公司 | A kind of preparation method of porous carbon electrode |
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Patent Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
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CN106252089A (en) * | 2016-08-03 | 2016-12-21 | 代长华 | A kind of electrode material for super capacitor and preparation method thereof |
CN106486290A (en) * | 2016-11-08 | 2017-03-08 | 铜陵市启动电子制造有限责任公司 | A kind of titanium manganese blending modification shitosan polypyrrole charcoal combination electrode material |
CN106783212A (en) * | 2016-11-22 | 2017-05-31 | 张家港智电芳华蓄电研究所有限公司 | A kind of preparation method of porous carbon electrode |
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Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
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CN109741963A (en) * | 2019-02-15 | 2019-05-10 | 铜陵市启动电子制造有限责任公司 | A kind of high power density recombiner condenser electrode and preparation method thereof |
CN114743800A (en) * | 2022-04-25 | 2022-07-12 | 武夷学院 | Preparation method of polyacrylic acid/graphene-based flexible electrode material |
CN114743800B (en) * | 2022-04-25 | 2023-07-21 | 武夷学院 | Preparation method of polyacrylic acid/graphene-based flexible electrode material |
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