CN103258658B - A kind of preparation method based on functional form Graphene electrode of super capacitor - Google Patents
A kind of preparation method based on functional form Graphene electrode of super capacitor Download PDFInfo
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- CN103258658B CN103258658B CN201310203648.4A CN201310203648A CN103258658B CN 103258658 B CN103258658 B CN 103258658B CN 201310203648 A CN201310203648 A CN 201310203648A CN 103258658 B CN103258658 B CN 103258658B
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- nickel foam
- graphite oxide
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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 kind of preparation method based on functional form Graphene electrode of super capacitor, first the method passes through Hummer legal system for graphite oxide slurry, then graphite oxide slurry is evenly coated in nickel foam, graphite oxide is made to enter in the silk screen micropore of nickel foam, the direct microwave heating expansion graphite oxide functional form Graphene being peeled off and reduce in atmospheric conditions after drying, and be embedded in the silk screen of nickel foam, the nickel foam being inlaid with functional form Graphene is pressed into sheet, namely obtains electrode of super capacitor after cropped; This method technique is simple, and can realize extensive preparation, prepared functional form Graphene is embedded in the micropore of nickel foam, it can be used as electrode of super capacitor to have high specific capacity.
Description
Technical field
The present invention relates to a kind of preparation method based on functional form Graphene electrode of super capacitor, belong to new energy field.
Technical background
Graphene is by sp
2the cellular planar structure of hexagonal of the carbon atom formation of hydridization, due to the structure that it is special, unique chemical property and using value potential in a large number cause the extensive concern of countries in the world scientist.2004, first Geim and Novoselov peeled off the method for highly oriented pyrolytic graphite repeatedly by adhesive tape, obtain single-layer graphene.Subsequently, optics, the electricity and thermal property etc. of the excellence of Graphene are all excavated out, and the specific area of such as Graphene is up to 2600m
2/ g, application prospect is very wide, as using the electrode material of Graphene as ultracapacitor.Therefore prepare Graphene how efficiently, in a large number and become our the primary problem solved.At present, along with the development of science and technology, the preparation of Graphene has developed multiple method, mainly comprises mechanical stripping method, chemical stripping method, chemical vapour deposition technique (CVD), epitaxial growth method, high-temperature heat expansion method etc.
The place that these methods all come with some shortcomings, such as mechanical stripping legal system yields poorly for Graphene, and area is little, not easy to operate etc.; Epitaxial growth method is generally growing graphene on the monocrystalline such as Ru, because the strict growth conditions such as costliness and high temperature of single crystalline substrate limits the method large-scale production Graphene; Oxidation-reduction method causes the defect of Graphene many due to graphite after strong oxidation and reduction, easily reunites in reduction process between graphene sheet layer simultaneously, and not thoroughly, the reaction time is long in reduction; CVD prepares Graphene, high to the requirement of equipment, yields poorly, condition is harsh etc. prepared by the method Graphene is more difficult and cost is high.Hot soarfing for preparing Graphene provides an extraordinary approach fast, can prepare high-quality graphene from graphite oxide method fast on a large scale.Traditional hot stripping means needs high temperature, the fast rate of heat addition, condition of high vacuum degree and low temperature hydrogen environment.Along with the development of electric automobile, require more and more higher to novel energy-storing materials and devices; Graphene is sent to great expectations as the energy storage material of novelty in the application of electrode of super capacitor, and the preparation method based on Graphene electrodes therefore seeking simple and convenient seems particularly important.Traditional electrode of super capacitor needs electrode material and conductive agent and binding agent to be mixed with to form, and binding agent to be generally insulator non-conductive, thus increase the internal resistance of capacitor, reduce the capacity of capacitor, therefore the specific capacity how improved based on Graphene electrode for capacitors becomes urgent problem.
Summary of the invention
The object of this invention is to provide a kind of preparation method based on functional form Graphene electrode of super capacitor, solve the environment that traditional dilatometry prepares excessive temperature that Graphene requires and high vacuum.Applicant finds graphite oxide generation thermal expansion just can be made to peel off by microwave heating a period of time in atmospheric conditions, make the functional form Graphene of preparation be embedded in nickel foam silk screen simultaneously, take full advantage of nickel foam surface area, improve the ability of Graphene electrodes adion, eliminate the process mixed with binding agent, reduce the internal resistance of capacitor, improve specific capacity.
A kind of preparation method based on functional form Graphene electrode of super capacitor provided by the invention comprises the steps:
1) first alkali cleaning is carried out on nickel foam surface, then carry out pickling, the oxide on removing surface, finally carries out cleaning and drying with clear water;
2) by Hummers legal system for graphite oxide slurry, then graphite oxide slurry is evenly coated in the nickel foam of cleaning, drying, and dries in vacuum drying chamber;
3) in atmospheric conditions, the nickel foam scribbling graphite oxide is put into microwave oven, microwave heating makes the graphite oxide in foam nickel screen be reduced into the Graphene be embedded in nickel foam silk screen;
4) the power 800 ~ 1600W of microwave; Time 30s ~ the 8min of microwave;
5) nickel foam being inlaid with functional form Graphene is pressed into sheet, namely obtains electrode of super capacitor after cropped.
Step 2) in, described in vacuum drying chamber with 45 DEG C of dry 48h.
In step 3), microwave heating is under Ar gas shielded environment.
In step 5), described nickel foam 10Mpa on tablet press machine is pressed into sheet.
beneficial effect of the present invention:
Compared with the traditional process required, condition is simple, and easily realize, energy consumption is low.And the electrode of the ultracapacitor of the functional form Graphene prepared compare traditional electrode preparation method-Graphene, binding agent, conductive agent mixing coating prepared by electrode have larger ratio capacitance.
Embodiment
embodiment 1
(1) adopt the Hummers legal system improved for graphite oxide.First, in 500ml conical flask, add the 115ml concentrated sulfuric acid, and conical flask is put into cryostat, temperature is controlled at about 0 DEG C.Add in advance with the natural flake graphite powder 5g of watery hydrochloric acid process, then add 2.5gNaNO
3, more slowly add 15gKMNO
4, after stirring reaction 2h.Moved into by conical flask in the constant water bath box of 35 DEG C, continue stirring reaction 2 hours, now solution is in purple green.Then slowly add 230ml deionized water, heating-up temperature is elevated to 95 DEG C, continue to stir a period of time.Slowly add appropriate hydrogen peroxide, now solution becomes golden yellow, filters while hot, and with mass fraction be 5% hydrochloric acid and deionized water cyclic washing until sulfate radical-free ion in filtrate.Finally the graphite oxide paste obtained after filtration is evenly coated in nickel foam, graphite oxide paste is fully entered in the micropore of nickel foam.
(2) nickel foam scribbling graphite oxide paste that step (1) obtains to be placed in vacuum drying chamber dry 48h in 45 DEG C of environment, then directly put into microwave oven under air ambient, 1600W microwave heating 30s can obtain the nickel foam being inlaid with functional form Graphene.
(3) electrode for super capacitor can be obtained after compressing tablet and cutting.Electrochemical workstation and constant current charge-discharge instrument carry out electrochemical property test respectively.Test result shows, the electrode ratio capacitance of ultracapacitor when charging and discharging currents density is 1A/g is up to 248F/g; When sweep speed is 1mV/s, ratio capacitance is up to 245F/g.
embodiment 2
(1) nickel foam scribbling graphite oxide paste prepared in example 1 to be placed in vacuum drying chamber dry 48h in 45 DEG C of environment, then directly put into microwave oven under air ambient, 1600W microwave heating 1min can obtain the nickel foam being inlaid with functional form Graphene.
(2) electrode for super capacitor can be obtained after compressing tablet and cutting.Electrochemical workstation and constant current charge-discharge instrument carry out electrochemical property test respectively.Test result shows, the electrode ratio capacitance of ultracapacitor when charging and discharging currents density is 1A/g is up to 227F/g, and when sweep speed is 1mV/s, ratio capacitance is up to 223F/g.
embodiment 3
(1) nickel foam scribbling graphite oxide paste prepared in example 1 to be placed in vacuum drying chamber dry 48h in 45 DEG C of environment; then directly put into microwave oven (Ar gas shielded) under air ambient, 800W microwave heating 2min can obtain the nickel foam being inlaid with functional form Graphene.
(2) electrode for super capacitor can be obtained after compressing tablet and cutting.Electrochemical workstation and constant current charge-discharge instrument do electrochemical property test respectively.Test result shows, the electrode ratio capacitance of ultracapacitor when charging and discharging currents density is 1A/g is up to 236F/g, and when sweep speed is 1mV/s, ratio capacitance is up to 232F/g.
embodiment 4
(1) nickel foam scribbling graphite oxide paste prepared in example 1 to be placed in vacuum drying chamber dry 48h in 45 DEG C of environment; then directly put into microwave oven (Ar gas shielded) under air ambient, 1200W microwave heating 2min can obtain the nickel foam being inlaid with functional form Graphene.
(2) electrode for super capacitor can be obtained after compressing tablet and cutting.Electrochemical workstation and constant current charge-discharge instrument do electrochemical property test respectively.Test result shows, the electrode ratio capacitance of ultracapacitor when charging and discharging currents density is 1A/g is up to 217F/g, and when sweep speed is 1mV/s, ratio capacitance is up to 212F/g.
embodiment 5
(1) nickel foam scribbling graphite oxide paste prepared in example 1 to be placed in vacuum drying chamber dry 48h in 45 DEG C of environment; then directly put into microwave oven (Ar gas shielded) under air ambient, 1600W microwave heating 2min can obtain the nickel foam being inlaid with functional form Graphene.
(2) electrode for super capacitor can be obtained after compressing tablet and cutting.Electrochemical workstation and constant current charge-discharge instrument do electrochemical property test respectively.Test result shows, the electrode ratio capacitance of ultracapacitor when charging and discharging currents density is 1A/g is up to 204F/g, and when sweep speed is 1mV/s, ratio capacitance is up to 201F/g.
embodiment 6
(1) graphite oxide paste prepared in example 1 to be placed in vacuum drying chamber dry 48h in 45 DEG C, then put into microwave oven (Ar gas shielded), 1600W microwave heating 2min, the black powder obtained after expansion pyrolysis is functional form Graphene.
(2), after the functional form Graphene obtained, acetylene black, PTFE being mixed according to the ratio uniform of mass ratio 8:1:1, be coated in nickel foam, after the cutting of drying compressing tablet, make electrode.Then on electrochemical workstation and constant current charge-discharge instrument, electrochemical property test is carried out respectively.Test result shows, the electrode ratio capacitance of ultracapacitor when charging and discharging currents density is 1A/g is up to 189F/g, and when sweep speed is 1mV/s, ratio capacitance is up to 181F/g.
embodiment 7
(1) nickel foam scribbling graphite oxide paste prepared in example 1 to be placed in vacuum drying chamber dry 48h in 45 DEG C of environment; then directly put into microwave oven (Ar gas shielded) under air ambient, 1600W microwave heating 4min can obtain the nickel foam being inlaid with functional form Graphene.
(2) electrode for super capacitor can be obtained after compressing tablet and cutting.Electrochemical workstation and constant current charge-discharge instrument do electrochemical property test respectively.Test result shows, the electrode ratio capacitance of ultracapacitor when charging and discharging currents density is 1A/g is up to 177F/g, and when sweep speed is 1mV/s, ratio capacitance is up to 170F/g.
embodiment 8
(1) nickel foam scribbling graphite oxide paste prepared in example 1 to be placed in vacuum drying chamber dry 48h in 45 DEG C of environment; then directly put into microwave oven (Ar gas shielded) under air ambient, 1600W microwave heating 8min can obtain the nickel foam being inlaid with functional form Graphene.
(2) electrode for super capacitor can be obtained after compressing tablet and cutting.Electrochemical workstation and constant current charge-discharge instrument do electrochemical property test respectively.Test result shows, the electrode ratio capacitance of ultracapacitor when charging and discharging currents density is 1A/g is up to 163F/g, and when sweep speed is 1mV/s, ratio capacitance is up to 158F/g.
Claims (1)
1., based on a preparation method for functional form Graphene electrode of super capacitor, it is characterized in that comprising the steps:
1) first alkali cleaning is carried out on nickel foam surface, then carry out pickling, the oxide on removing surface, finally carries out cleaning and drying with clear water;
2) by Hummers legal system for graphite oxide slurry, then graphite oxide slurry is evenly coated in the nickel foam of cleaning, drying, and dries in vacuum drying chamber;
3) in atmospheric conditions, the nickel foam scribbling graphite oxide is put into microwave oven, microwave heating makes the graphite oxide in foam nickel screen be reduced into the Graphene be embedded in nickel foam silk screen;
4) the power 800 ~ 1600W of microwave; Time 30s ~ the 8min of microwave;
5) nickel foam being inlaid with functional form Graphene is pressed into sheet, namely obtains electrode of super capacitor after cropped;
Step 2) in, described in vacuum drying chamber with 45 DEG C of dry 48h;
In step 3), microwave heating is under Ar gas shielded environment;
In step 5), described nickel foam 10Mpa on tablet press machine is pressed into sheet.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103545121B (en) * | 2013-10-23 | 2016-12-07 | 南京大学 | A kind of electrode material for super capacitor preparation method based on three-dimensional grapheme |
| CN103903880A (en) * | 2014-03-03 | 2014-07-02 | 广东工业大学 | Method for in-situ preparation of graphene supercapacitor electrode based on nickel foam |
| CN104021946B (en) * | 2014-06-12 | 2017-02-01 | 吉林大学 | Super capacitor based on graphene material and manufacturing method of super capacitor |
| CN104291324A (en) * | 2014-09-09 | 2015-01-21 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method of graphene foams |
| CN105914056B (en) * | 2016-04-20 | 2018-04-20 | 青岛华高墨烯科技股份有限公司 | A kind of preparation method of graphene/nickel foam composite electrode |
| CN106630685B (en) * | 2016-12-27 | 2020-05-19 | 东南大学 | Preparation method of carbon-coated optical fiber |
| CN115798946B (en) * | 2023-01-30 | 2023-05-12 | 昆山美淼新材料科技有限公司 | Production process of metal graphene multi-element composite electrode |
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| CN101831622B (en) * | 2010-05-20 | 2011-12-21 | 中国科学院化学研究所 | Grapheme foam and preparation method thereof |
| CN101948107A (en) * | 2010-09-15 | 2011-01-19 | 天津大学 | Method for preparing and purifying graphene by microwave radiation under vacuum |
| CN102496480B (en) * | 2011-12-16 | 2013-09-18 | 江南大学 | Preparation method of graphene/nickel-aluminum bi-metal hydroxide composite material and application thereof |
| CN102646518B (en) * | 2012-05-08 | 2014-03-05 | 同济大学 | Method for fabricating graphene electrode materials through pulsed laser deposition and application thereof |
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