CN109659165A - The preparation method of the polyaniline laminated nanocomposite of supercapacitor graphene - Google Patents
The preparation method of the polyaniline laminated nanocomposite of supercapacitor graphene Download PDFInfo
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- CN109659165A CN109659165A CN201811319662.XA CN201811319662A CN109659165A CN 109659165 A CN109659165 A CN 109659165A CN 201811319662 A CN201811319662 A CN 201811319662A CN 109659165 A CN109659165 A CN 109659165A
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 168
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 145
- 229920000767 polyaniline Polymers 0.000 title claims abstract description 100
- 238000002360 preparation method Methods 0.000 title claims abstract description 31
- 239000002114 nanocomposite Substances 0.000 title claims abstract description 13
- 238000000034 method Methods 0.000 claims abstract description 58
- 239000002131 composite material Substances 0.000 claims abstract description 46
- 238000006116 polymerization reaction Methods 0.000 claims abstract description 28
- 239000007788 liquid Substances 0.000 claims abstract description 27
- 238000004519 manufacturing process Methods 0.000 claims abstract description 11
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 10
- 239000010439 graphite Substances 0.000 claims abstract description 10
- 239000003990 capacitor Substances 0.000 claims abstract description 9
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 176
- 229910052759 nickel Inorganic materials 0.000 claims description 89
- 239000000243 solution Substances 0.000 claims description 87
- PAYRUJLWNCNPSJ-UHFFFAOYSA-N Aniline Chemical compound NC1=CC=CC=C1 PAYRUJLWNCNPSJ-UHFFFAOYSA-N 0.000 claims description 74
- 239000006260 foam Substances 0.000 claims description 52
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 42
- VZGDMQKNWNREIO-UHFFFAOYSA-N tetrachloromethane Chemical compound ClC(Cl)(Cl)Cl VZGDMQKNWNREIO-UHFFFAOYSA-N 0.000 claims description 36
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 claims description 34
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 claims description 34
- 239000008367 deionised water Substances 0.000 claims description 33
- 229910021641 deionized water Inorganic materials 0.000 claims description 33
- 238000003756 stirring Methods 0.000 claims description 30
- 238000001035 drying Methods 0.000 claims description 26
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 22
- 239000011521 glass Substances 0.000 claims description 21
- 239000004033 plastic Substances 0.000 claims description 19
- 229920003023 plastic Polymers 0.000 claims description 19
- 239000002002 slurry Substances 0.000 claims description 18
- 239000011668 ascorbic acid Substances 0.000 claims description 17
- 229960005070 ascorbic acid Drugs 0.000 claims description 17
- 235000010323 ascorbic acid Nutrition 0.000 claims description 17
- 239000000463 material Substances 0.000 claims description 17
- 239000000843 powder Substances 0.000 claims description 17
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 12
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims description 12
- 238000006243 chemical reaction Methods 0.000 claims description 12
- 230000001590 oxidative effect Effects 0.000 claims description 12
- 239000012528 membrane Substances 0.000 claims description 11
- 239000003792 electrolyte Substances 0.000 claims description 10
- 239000003822 epoxy resin Substances 0.000 claims description 10
- 239000003365 glass fiber Substances 0.000 claims description 10
- 229920000647 polyepoxide Polymers 0.000 claims description 10
- 229920006267 polyester film Polymers 0.000 claims description 10
- 239000000945 filler Substances 0.000 claims description 9
- 239000004570 mortar (masonry) Substances 0.000 claims description 9
- 238000007789 sealing Methods 0.000 claims description 9
- BFKJFAAPBSQJPD-UHFFFAOYSA-N tetrafluoroethene Chemical compound FC(F)=C(F)F BFKJFAAPBSQJPD-UHFFFAOYSA-N 0.000 claims description 9
- 238000005406 washing Methods 0.000 claims description 9
- 229920000049 Carbon (fiber) Polymers 0.000 claims description 6
- 238000013019 agitation Methods 0.000 claims description 6
- 229910001870 ammonium persulfate Inorganic materials 0.000 claims description 6
- 230000009172 bursting Effects 0.000 claims description 6
- 239000004917 carbon fiber Substances 0.000 claims description 6
- 238000010790 dilution Methods 0.000 claims description 6
- 239000012895 dilution Substances 0.000 claims description 6
- 229910021397 glassy carbon Inorganic materials 0.000 claims description 6
- 238000005303 weighing Methods 0.000 claims description 6
- 238000005119 centrifugation Methods 0.000 claims description 4
- 239000006185 dispersion Substances 0.000 claims description 4
- 230000005611 electricity Effects 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 4
- 239000000284 extract Substances 0.000 claims description 3
- 239000011259 mixed solution Substances 0.000 claims description 3
- 239000012286 potassium permanganate Substances 0.000 claims description 3
- GDSOZVZXVXTJMI-SNAWJCMRSA-N (e)-1-methylbut-1-ene-1,2,4-tricarboxylic acid Chemical compound OC(=O)C(/C)=C(C(O)=O)\CCC(O)=O GDSOZVZXVXTJMI-SNAWJCMRSA-N 0.000 claims 1
- 229920002472 Starch Polymers 0.000 claims 1
- 229910052799 carbon Inorganic materials 0.000 claims 1
- 238000005538 encapsulation Methods 0.000 claims 1
- -1 graphite Alkene Chemical class 0.000 claims 1
- 239000008107 starch Substances 0.000 claims 1
- 235000019698 starch Nutrition 0.000 claims 1
- 239000011345 viscous material Substances 0.000 claims 1
- 239000000126 substance Substances 0.000 abstract description 9
- 230000005764 inhibitory process Effects 0.000 abstract description 5
- 238000009826 distribution Methods 0.000 abstract description 3
- 241000446313 Lamella Species 0.000 abstract description 2
- 230000009286 beneficial effect Effects 0.000 abstract description 2
- 150000001412 amines Chemical class 0.000 description 7
- 235000019441 ethanol Nutrition 0.000 description 7
- 229920006389 polyphenyl polymer Polymers 0.000 description 7
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 description 6
- 239000002033 PVDF binder Substances 0.000 description 5
- 230000008901 benefit Effects 0.000 description 5
- 238000000227 grinding Methods 0.000 description 5
- 229920002981 polyvinylidene fluoride Polymers 0.000 description 5
- 150000004040 pyrrolidinones Chemical class 0.000 description 5
- 150000001336 alkenes Chemical class 0.000 description 4
- 229920002239 polyacrylonitrile Polymers 0.000 description 4
- 229960000935 dehydrated alcohol Drugs 0.000 description 2
- 238000010041 electrostatic spinning Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 238000009987 spinning Methods 0.000 description 2
- 239000007848 Bronsted acid Substances 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000002041 carbon nanotube Substances 0.000 description 1
- 229910021393 carbon nanotube Inorganic materials 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 239000008151 electrolyte solution Substances 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 229960004756 ethanol Drugs 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- 239000002121 nanofiber Substances 0.000 description 1
- 239000002070 nanowire Substances 0.000 description 1
- 239000007800 oxidant agent Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000011946 reduction process Methods 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 238000001291 vacuum drying Methods 0.000 description 1
- 239000002023 wood Substances 0.000 description 1
Classifications
-
- 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
-
- 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
-
- 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
- H01G11/30—Electrodes characterised by their material
-
- 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
- H01G11/30—Electrodes characterised by their material
- H01G11/32—Carbon-based
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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
- H01G11/30—Electrodes characterised by their material
- H01G11/48—Conductive polymers
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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
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- Engineering & Computer Science (AREA)
- Power Engineering (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Chemical & Material Sciences (AREA)
- Materials Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Carbon And Carbon Compounds (AREA)
Abstract
The method of ultracapacitor the invention discloses a kind of preparation method of polyaniline laminated nanocomposite of supercapacitor graphene and using composite material preparation, using polyaniline as the base stock of N doping, polyaniline nano-line is deposited on the dilute lamella of graphite using liquid level polymerization, the more uniform tiny distribution of polyaniline, so that the electric current inhibition of graphene polyaniline composite material is small, the electric conductivity of capacitor pole piece is stronger.Compared with prior art, the beneficial effects of the present invention are: the graphene polyaniline composite material of the method preparation of liquid level polymerization has very strong chemical combination key active force between graphene polyaniline since polymerization reaction occurs, it is a whole substance, there is very strong binding force.Using the condenser plate of the graphene polyaniline composite material production of the method preparation of liquid level of the present invention polymerization, the electric current inhibition of graphene polyaniline composite material is small, and the electric conductivity of pole piece is stronger.
Description
Technical field
The present invention relates to material processing and preparation technical field more particularly to a kind of supercapacitor graphene polyanilines
The method of the preparation method of laminated nano composition and the ultracapacitor using composite material preparation.
Background technique
Supercapacitor has become one of the hot spot of whole world new energy or new material research, and electrode material is system
The about key of chemical property raising.But the chemical property of homogenous material is unable to satisfy modern society to the need of energy storage device
It asks, the design of composite material and constructs and can preferably solve this problem, to prepare with high-energy density and power
The supercapacitor of density.
The preparation method of graphene mainly has 1. mechanical stripping methods at present: the graphene film scale that this method obtains can be with
Reach 100 μm or so.It is simple process that this method, which prepares advantage, and cost is relatively low, and obtained product remains more perfect crystal
Structure, defect are less.Disadvantage is long preparation period, and the efficiency for generating graphene is lower, is not suitable for large-scale industry
Production.2. epitaxial growth method: graphene made from the method can control graphene sheet layer thickness by changing temperature, obtain
Graphene film electron mobility with higher, therefore have a good application prospect.But the graphene of this method production
Piece is influenced bigger by SiC substrate, and often graphene film is in uneven thickness, while the interaction meeting between product and matrix
Influence the characteristic of graphene.3. chemical vapour deposition technique: required equipment is sufficiently expensive, and reaction condition requires relatively
Height constrains large-scale application of this method in actual production.4. cutting carbon nanotubes method: this method is to laboratory apparatus
And experimental implementation difficulty has larger requirement, is not able to satisfy the needs of common laboratory scientific research.5. reduction-oxidation graphite method: oxidation stone
The electric conductivity of ink is very poor.Graphene oxide may not be able to restore completely in reduction process, lead to some physics, chemistry etc.
Performance loss, especially electric conductivity, but it is this method is simple and low in cost, large scale preparation graphite may be implemented
Alkene.
The synthetic method of polyaniline mainly has 1. chemical oxidative polymerizations: by the type and concentration of oxidant, Bronsted acid
Acidity (pH value), the influence of temperature of the concentration of aniline monomer and reaction system etc..2. electrochemical polymerization method: the electricity of polyaniline
Chemical polymerization is carried out in the electrolyte solution of aniline, and oxidative polymerization occurs for anode, is deposited into electrode surface poly-
Aniline Films.The preparation method of conductive polyaniline nanometer structure mainly has template, template-free method etc..
Application No. is 201610010126.6 patent documents to disclose a kind of magnetic graphene polyaniline nano composite wood
Material and preparation method thereof: by being ultrasonically treated after mixing graphite oxide and solvent, graphene oxide solution is obtained；Described
The hydrochloric acid solution containing aniline is added in graphene oxide solution and stirs evenly, obtains mixed liquor；(NH will be contained4)2S2O8Hydrochloric acid
Solution, which is added in the mixed liquor, to be reacted, and obtains grapheme/polyaniline composite material after reaction.The invention system
Standby magnetic graphene polyaniline nano-composite material has stable chemical performance, and large specific surface area, absorption property is strong, overcomes
The disadvantage that graphene sheet layer easily stacks and simple polyaniline is easy to reunite, advantage easy to operate.
Application No. is 201610017331.5 patent documents to disclose a kind of preparation of graphene polyaniline composite material
Method, by the way that graphene to be dissolved in dehydrated alcohol and n,N-Dimethylformamide composite solution, graphite is made in ultrasonic disperse
Alkene solution；Polyacrylonitrile powder is added in n,N-Dimethylformamide solution, it is molten to obtain polyacrylonitrile for heating stirring dissolution
Liquid；Polyaniline is added in solvent, stirring and dissolving, polyaniline solutions are made；Graphene solution and polyaniline solutions are instilled
It in polyacrylonitrile solution, is sufficiently stirred, electrostatic spinning precursor liquid is obtained after standing and defoaming, above-mentioned spinning solution is added to electrostatic
Electrostatic spinning is carried out in device for spinning, and graphene polyaniline composite nanofiber membrane is prepared after vacuum drying.Invention benefit
With the preferable fibre forming property of polyacrylonitrile, the content of polyaniline in composite material is improved.Preparation method is easy to operate, at low cost
It is honest and clean；The composite material of preparation has many advantages, such as conductivity height, large specific surface area.
The above invention has the advantages that its is fine, but graphene polyaniline composite material is all absorbent-type, cannot be fine
Combination, polyaniline is unevenly distributed on the surface of graphene, big to the inhibition of electric current.
Summary of the invention
The present invention provides a kind of preparation method of polyaniline laminated nanocomposite of supercapacitor graphene with
And the method for the ultracapacitor using composite material preparation, it is poly- using liquid level using polyaniline as the base stock of N doping
Polyaniline nano-line is deposited on the dilute lamella of graphite by conjunction method, the more uniform tiny distribution of polyaniline, so that graphene is poly-
The electric current inhibition of aniline composite material is small, and the electric conductivity of capacitor pole piece is stronger.
To achieve the above object, the present invention is implemented with the following technical solutions:
The preparation method of the polyaniline laminated nanocomposite of supercapacitor graphene,
Graphene oxide is prepared using Hummer oxidizing process first, by KMnO4It is added to dense H2SO4With P2O5, graphite powder stirs
It in the mixed solution mixed, and keeps the temperature, addition deionized water makes reaction terminating after deionized water stirring is added；It is with mass concentration
After 20%~36% hydrochloric acid and water are washed according to the HCL that the volume ratio of 1:10 is prepared, deionized water continues washing to being in neutrality,
It dilutes and stirs and be allowed to evenly dispersed；
Secondly graphene polyaniline composite material is prepared using method of liquid level polymerization, by the graphene oxide prepared and
Ascorbic acid mixing is put into the stirring of beaker 1 and is completely dissolved to ascorbic acid, and carbon tetrachloride solution and aniline solution are put into beaker 2
It is mixed, 1 solution of beaker is drained to beaker 2, aniline and graphene oxide are respectively placed in up and down in two-phase system, allow benzene
Amine and graphene oxide extract carbon tetrachloride solution out after sealing a period of time in the interface of two-phase generation polymerization reaction, and will
It is dry after the centrifugation of aniline graphene solution, obtain graphene polyaniline composite material.
It is described graphene oxide to be prepared using Hummer oxidizing process the specific method is as follows:
1) taking 115-120mL mass concentration is 98% dense H2SO4It is added in the beaker of 1L, weighs the P of 2-4g2O5And
Dense H is added in the graphite powder of 4-6g2SO4In, 2-3h is stirred with magnetic stirrer, set temperature is 4-6 DEG C；
2) KMnO of 10-15g is added in the solution being stirred4, it is slowly added to prevent heat release is too fast from bursting beaker, keeps
The temperature of solution is lower than 20 DEG C, is heated to 32-36 DEG C, keeps the temperature 1.5-2.5h；
3) plus deionized water 225-235mL, control temperature stir 12-17min at 96-99 DEG C；
4) 0.5-0.9L deionized water is added by reaction terminating, meanwhile, the H of 11-15mL is added2O2；
5) HCL that the hydrochloric acid for being 20%~36% with mass concentration and water are prepared according to the volume ratio of 1:10 is by acquired solution
It is washed in centrifuge twice, uses deionized water instead and continue washing until solution is in neutrality；
6) acquired solution is poured into beaker and deionized water 225-235mL dilution is added, be placed in ultrasonic agitation case, be allowed to
It is evenly dispersed.
The method using liquid level polymerization prepares graphene polyaniline composite material, and the specific method is as follows:
1) each 45-55ml of graphene oxide for weighing the ammonium persulfate solution of 0.5-1.5mol/L and preparing pours into beaker
It in 1, then weighs 0.5-1.5g ascorbic acid and is put into beaker 1, stirred ten minutes with glass bar, be completely dissolved ascorbic acid；
2) it weighs the carbon tetrachloride solution of 45-55ml and 1-3mL aniline solution pours into beaker 2, stir 5~10 minutes；
3) liquid in beaker 1 is poured into beaker 2 in such a way that glass drains, sealing is placed 45-50 hours, benzene
Amine and graphene oxide are in the interface of two-phase generation polymerization reaction；
4) carbon tetrachloride solution to be extracted out, remaining graphene polyaniline solutions pour into 3 centrifuge tubes, it is centrifuged 3-6 times,
It is put into thermostatic drying chamber later 34-38 hours dry.
The graphene prepared using the preparation method of the polyaniline laminated nanocomposite of supercapacitor graphene is poly-
The method that aniline composite material prepares supercapacitor,
A) production of condenser plate: claying into power the graphene polyaniline composite material after drying shape with mortar, will
Graphene polyaniline powder and conductive black be mixed evenly be ground to it is thick, together with N-Methyl pyrrolidone (NMP)
Beaker 3 is poured into, stirring a period of time, nickel foam is placed on tetrafluoroethene plate, takes a small amount of graphene polyphenyl with glass bar is viscous
Amine slurry is uniformly applied to the end surface of nickel foam, and the nickel foam for being coated with graphene polyaniline slurry is put into thermostatic drying chamber
Middle drying, tabletting, nickel foam pole piece are successful；
B) production of supercapacitor: the identical plastic plate with holes of two sizes and a nickel bar are taken, uses alcohol respectively
Wiping, nickel bar is penetrated from the hole of plastic plate, in the nickel bar for taking two nickel foam pole pieces identical in quality being just placed through respectively,
Nickel bar is not allowed to expose；The two face-to-face modes of nickel foam pole piece are superimposed together, and centre is separated with glass fiber membrane, to avoid
Two electric pole short circuits；The vitreous carbon fibers film central filler KOH electrolyte of two nickel foam pole pieces and with polyester film and epoxy
Resin is packaged capacitor.
The specific method is as follows:
1) the graphene polyaniline composite material after drying is clayed into power shape with mortar；
2) in graphene polyaniline powder: conductive black: Kynoar=85:10:5 ratio weighs graphene polyphenyl
Amine powder, conductive black and Kynoar (PVDF), load weighted material is put into beaker 3, grinding is mixed evenly
It is extremely thick, N- first is weighed with graduated cylinder in the ratio that mixed material and N-Methyl pyrrolidone (NMP) quality and volume ratio are 1:5
Base pyrrolidones (NMP), and N-Methyl pyrrolidone (NMP) is poured into beaker 3, with 3 hours of magnetic stirrer；
3) it takes the nickel foam of 2 × 2cm to be placed on tetrafluoroethene plate, takes graphene obtained in step 2) poly- with glass bar is viscous
Aniline slurry is uniformly applied to the end surface of nickel foam, application area 1cm2；
4) nickel foam for being coated with graphene polyaniline slurry is put into thermostatic drying chamber, under conditions of 78-82 DEG C, is done
Dry 5 hours, tabletting, nickel foam pole piece are successful；
5) the identical plastic plate with holes of two sizes and a nickel bar are taken, respectively with alcohol wipe and by nickel bar from plastics
The hole of plate penetrates 0.5-1.5cm；
6) in the nickel bar for taking two nickel foam pole pieces identical in quality being just placed through respectively, nickel bar is not allowed to expose；
7) piece face-to-face mode in the two poles of the earth is superimposed together, centre is separated with glass fiber membrane, short to avoid two electrodes
Road, the vitreous carbon fibers film central filler KOH electrolyte of two nickel foam pole pieces and with polyester film and epoxy resin to electricity
Container is packaged.
Compared with prior art, the beneficial effects of the present invention are:
1) present invention prepares graphene polyaniline composite material using the method for liquid level polymerization, and polyaniline is slowly in two phase boundaries
Polymerization reaction occurs between face, the uniform vertical-growth of polyaniline nano spot is in graphene film layer surface.And multi-layer graphene
Still keep its original sheet-shaped.Nano-wire array is vertically coated on the surface of graphene sheet layer.Polyaniline is more uniform thin
Small distribution.
2) the graphene polyaniline composite material of the method preparation of liquid level polymerization, since polymerization reaction occurs, graphene is poly-
There is very strong chemical combination key active force between aniline, is a whole substance, there is very strong binding force.
3) condenser plate made of the graphene polyaniline composite material of the method preparation of liquid level of the present invention polymerization,
The electric current inhibition of graphene polyaniline composite material is small, and the electric conductivity of pole piece is stronger.
Detailed description of the invention
Fig. 1 is graphene polyaniline constant current charge-discharge curve graph.
Fig. 2 is the manufacturing process figure of supercapacitor.
In figure: 1- nickel foam pole piece；2- nickel bar；3- graphene polyaniline slurry；4- glass fiber membrane；5- fills KOH
The position of electrolyte, polyester film and epoxy resin；Plastic plate 6- with holes.
Specific embodiment
It elaborates below with reference to embodiment to the present invention, but practical range of the invention is not limited only to following realities
Apply example.
The preparation method of the polyaniline laminated nanocomposite of supercapacitor graphene,
Graphene oxide is prepared using Hummer oxidizing process first, by KMnO4It is added to dense H2SO4With P2O5, graphite powder stirs
It in the mixed solution mixed, and keeps the temperature, addition deionized water makes reaction terminating after deionized water stirring is added；It is with mass concentration
After 20%~36% hydrochloric acid and water are washed according to the HCL that the volume ratio of 1:10 is prepared, deionized water continues washing to being in neutrality,
It dilutes and stirs and be allowed to evenly dispersed；
Secondly graphene polyaniline composite material is prepared using method of liquid level polymerization, by the graphene oxide prepared and
Ascorbic acid mixing is put into the stirring of beaker 1 and is completely dissolved to ascorbic acid, and carbon tetrachloride solution and aniline solution are put into beaker 2
It is mixed, 1 solution of beaker is drained to beaker 2, aniline and graphene oxide are respectively placed in up and down in two-phase system, allow benzene
Amine and graphene oxide extract carbon tetrachloride solution out after sealing a period of time in the interface of two-phase generation polymerization reaction, and will
It is dry after the centrifugation of aniline graphene solution, obtain graphene polyaniline composite material.
It is described graphene oxide to be prepared using Hummer oxidizing process the specific method is as follows:
1) taking 115-120mL mass concentration is 98% dense H2SO4It is added in the beaker of 1L, weighs the P of 2-4g2O5And
Dense H is added in the graphite powder of 4-6g2SO4In, 2-3h is stirred with magnetic stirrer, set temperature is 4-6 DEG C；
2) KMnO of 10-15g is added in the solution being stirred4, it is slowly added to prevent heat release is too fast from bursting beaker, keeps
The temperature of solution is lower than 20 DEG C, is heated to 32-36 DEG C, keeps the temperature 1.5-2.5h；
3) plus deionized water 225-235mL, control temperature stir 12-17min at 96-99 DEG C；
4) 0.5-0.9L deionized water is added by reaction terminating, meanwhile, the H of 11-15mL is added2O2；
5) HCL that the hydrochloric acid for being 20%~36% with mass concentration and water are prepared according to the volume ratio of 1:10 is by acquired solution
It is washed in centrifuge twice, uses deionized water instead and continue washing until solution is in neutrality；
6) acquired solution is poured into beaker and deionized water 225-235mL dilution is added, be placed in ultrasonic agitation case, be allowed to
It is evenly dispersed.
The method using liquid level polymerization prepares graphene polyaniline composite material, and the specific method is as follows:
1) each 45-55ml of graphene oxide for weighing the ammonium persulfate solution of 0.5-1.5mol/L and preparing pours into beaker
It in 1, then weighs 0.5-1.5g ascorbic acid and is put into beaker 1, stirred ten minutes with glass bar, be completely dissolved ascorbic acid；
2) weigh 45-55ml carbon tetrachloride solution and 1-3mL aniline solution (solution that aniline and ethyl alcohol mix,
Aniline solution concentration is 1000ug/mL in dehydrated alcohol) it pours into beaker 2, it stirs 5~10 minutes；
3) liquid in beaker 1 is poured into beaker 2 in such a way that glass drains, sealing is placed 45-50 hours, benzene
Amine and graphene oxide are in the interface of two-phase generation polymerization reaction；
4) carbon tetrachloride solution to be extracted out, remaining graphene polyaniline solutions pour into 3 centrifuge tubes, it is centrifuged 3-6 times,
It is put into thermostatic drying chamber later 34-38 hours dry.
The graphene prepared using the preparation method of the polyaniline laminated nanocomposite of supercapacitor graphene is poly-
The method that aniline composite material prepares supercapacitor,
A) production of condenser plate: claying into power the graphene polyaniline composite material after drying shape with mortar, will
Graphene polyaniline powder and conductive black be mixed evenly be ground to it is thick, together with N-Methyl pyrrolidone (NMP)
Beaker 3 is poured into, stirring a period of time, nickel foam is placed on tetrafluoroethene plate, takes a small amount of graphene polyphenyl with glass bar is viscous
Amine slurry is uniformly applied to the end surface of nickel foam, and the nickel foam for being coated with graphene polyaniline slurry is put into thermostatic drying chamber
Middle drying, tabletting, nickel foam pole piece are successful；
B) production of supercapacitor: the identical plastic plate 6 with holes of two sizes and a nickel bar 2 are taken, uses wine respectively
Essence wiping, nickel bar 2 is penetrated from the hole of plastic plate, the nickel for taking two nickel foam pole pieces 1 identical in quality being just placed through respectively
On item 2, nickel bar 2 not allowed to be exposed；The face-to-face mode of two nickel foam pole piece 1 is superimposed together, centre with glass fiber membrane 4 every
It opens, to avoid two electric pole short circuits；The 4 central filler KOH electrolyte of vitreous carbon fibers film of two nickel foam pole pieces 1 simultaneously uses polyester
Film and epoxy resin are packaged capacitor.(as shown in Figure 2)
The specific method is as follows:
1) the graphene polyaniline composite material after drying is clayed into power shape with mortar；
2) in graphene polyaniline powder: conductive black: Kynoar=85:10:5 ratio weighs graphene polyphenyl
Amine powder, conductive black and Kynoar (PVDF), load weighted material is put into beaker 3, grinding is mixed evenly
It is extremely thick, N- first is weighed with graduated cylinder in the ratio that mixed material and N-Methyl pyrrolidone (NMP) quality and volume ratio are 1:5
Base pyrrolidones (NMP), and N-Methyl pyrrolidone (NMP) is poured into beaker 3, with 3 hours of magnetic stirrer；
3) it takes the nickel foam of 2 × 2cm to be placed on tetrafluoroethene plate, takes graphene obtained in step 2) poly- with glass bar is viscous
Aniline slurry is uniformly applied to the end surface of nickel foam, application area 1cm2；
4) nickel foam for being coated with graphene polyaniline slurry is put into thermostatic drying chamber, under conditions of 78-82 DEG C, is done
Dry 5 hours, tabletting, nickel foam pole piece are successful；
5) the identical plastic plate with holes of two sizes and a nickel bar are taken, respectively with alcohol wipe and by nickel bar from plastics
The hole of plate penetrates 0.5-1.5cm；
6) in the nickel bar for taking two nickel foam pole pieces identical in quality being just placed through respectively, nickel bar is not allowed to expose；
7) piece face-to-face mode in the two poles of the earth is superimposed together, centre is separated with glass fiber membrane, short to avoid two electrodes
Road, the vitreous carbon fibers film central filler KOH electrolyte of two nickel foam pole pieces and with polyester film and epoxy resin to electricity
Container is packaged.
Fig. 1 is the constant current charge-discharge of Graphene electrodes and aniline graphene combination electrode under -1.5V-1.5V voltage window
Curve graph, the test all carried out in the case where current density is 1A/g, 2A/g, 5A/g, 10A/g.
All charging and discharging curves all symmetrical triangles are distributed, and show that preferable capacitance behavior, composite material can be subjected to
One than wider current density range.Current density is bigger, and the charge and discharge time is shorter.
Embodiment 1:
Graphene oxide is prepared using Hummer oxidizing process:
1) taking 120mL concentration is 98% dense H2SO4It is added in the beaker of 1L, weighs the P of 2g2O5And the graphite powder of 5g
Dense H is added2SO4In, 2.5h is stirred with magnetic stirrer, set temperature is 5 DEG C；
2) KMnO of 13g is added in the solution being stirred4, it is slowly added to prevent heat release is too fast from bursting beaker, keeps molten
The temperature of liquid is lower than 20 DEG C, is heated to 34 DEG C, keeps the temperature 2h；
3) plus deionized water 230mL, control temperature stir 15min at 98 DEG C；
4) 0.7L deionized water is added by reaction terminating, meanwhile, the H of 13mL is added2O2；
5) acquired solution is being centrifuged by the hydrochloric acid for being 20% with mass concentration and water according to the HCL that the volume ratio of 1:10 is prepared
It is washed in machine twice, uses deionized water instead and continue washing until solution is in neutrality；
6) acquired solution is poured into beaker and the dilution of 230mL deionized water is added, be placed in ultrasonic agitation case, be allowed to uniform
Dispersion.
Graphene polyaniline composite material is prepared using the method that liquid level polymerize:
1) each 50ml of graphene oxide for weighing the ammonium persulfate solution of 1mol/L and preparing is poured into beaker 1, then is claimed
Amount 1g ascorbic acid is put into beaker 1, is stirred ten minutes with glass bar, is completely dissolved ascorbic acid；
2) it weighs the carbon tetrachloride solution of 50ml and 2ml aniline solution pours into beaker 2, stir 5 minutes；
3) liquid in beaker 1 is poured into beaker 2 in such a way that glass drains, sealing is placed 48 hours, aniline
Polymerization reaction occurs in the interface of two-phase with graphene oxide；
4) carbon tetrachloride solution to be extracted out, remaining graphene polyaniline solutions pour into 3 centrifuge tubes, it is centrifuged 4 times, it
After be put into thermostatic drying chamber it is 36 hours dry.
Prepare supercapacitor:
1) the graphene polyaniline composite material after drying is clayed into power shape with mortar；
2) in graphene polyaniline powder: conductive black: Kynoar=85:10:5 ratio weighs graphene polyphenyl
Amine powder, conductive black and Kynoar (PVDF), load weighted material is put into beaker 3, grinding is mixed evenly
It is extremely thick, N- first is weighed with graduated cylinder in the ratio that mixed material and N-Methyl pyrrolidone (NMP) quality and volume ratio are 1:5
Base pyrrolidones (NMP), and N-Methyl pyrrolidone (NMP) is poured into beaker 3, with 3 hours of magnetic stirrer；
3) it takes the nickel foam (weighed quality) of 2 × 2cm to be placed on tetrafluoroethene plate, takes a small amount of graphite with glass bar is viscous
Alkene polyaniline slurry is uniformly applied to the end surface of nickel foam, application area 1cm2；
4) nickel foam for being coated with graphene polyaniline slurry is put into thermostatic drying chamber, under conditions of 80 DEG C, dry 5
A hour, tabletting weigh quality, and pole piece is successful；
5) the identical plastic plate with holes of two sizes and a nickel bar are taken, respectively with alcohol wipe and by nickel bar from plastics
The hole of plate penetrates 1cm；
6) in the nickel bar for taking nickel foam pole piece similar in two quality being just placed through respectively, nickel bar is not allowed to expose；
7) piece face-to-face mode in the two poles of the earth is superimposed together, centre is separated with glass fiber membrane, short to avoid two electrodes
Road, central filler KOH electrolyte are simultaneously packaged capacitor with polyester film and epoxy resin.
Embodiment 2:
Hummer oxidizing process prepares graphene oxide:
1) taking 115mL concentration is 98% dense H2SO4It is added in the beaker of 1L, weighs the P of 3g2O5And the graphite powder of 6g
Dense H is added2SO4In, 3h is stirred with magnetic stirrer, set temperature is 6 DEG C；
2) KMnO of 10g is added in the solution being stirred4, it is slowly added to prevent heat release is too fast from bursting beaker, keeps molten
The temperature of liquid is lower than 20 DEG C, is heated to 32 DEG C, keeps the temperature 1.5h；
3) plus deionized water 235mL, control temperature stir 17min at 96 DEG C；
4) 0.7L deionized water is added by reaction terminating, meanwhile, the H of 15mL is added2O2；
5) HCL that the hydrochloric acid for being 20%~36% with mass concentration and water are prepared according to the volume ratio of 1:10 is by acquired solution
It is washed in centrifuge twice, uses deionized water instead and continue washing until solution is in neutrality；
6) acquired solution is poured into beaker and deionized water 235mL dilution is added, be placed in ultrasonic agitation case, be allowed to uniform
Dispersion.
Graphene polyaniline composite material is prepared using the method that liquid level polymerize:
1) each 55ml of graphene oxide for weighing the ammonium persulfate solution of 1mol/L and preparing is poured into beaker 1, then is claimed
Amount 1g ascorbic acid is put into beaker 1, is stirred ten minutes with glass bar, is completely dissolved ascorbic acid；
2) it weighs the carbon tetrachloride solution of 55ml and 3ml aniline solution pours into beaker 2, stir 5 minutes；
3) liquid in beaker 1 is poured into beaker 2 in such a way that glass drains, sealing is placed 50 hours, aniline
Polymerization reaction occurs in the interface of two-phase with graphene oxide；
4) carbon tetrachloride solution to be extracted out, remaining graphene polyaniline solutions pour into 3 centrifuge tubes, it is centrifuged 5 times, it
After be put into thermostatic drying chamber it is 38 hours dry.
Prepare supercapacitor:
1) the graphene polyaniline composite material after drying is clayed into power shape with mortar；
2) in graphene polyaniline powder: conductive black: Kynoar=85:10:5 ratio weighs graphene polyphenyl
Amine powder, conductive black and Kynoar (PVDF), load weighted material is put into beaker 3, grinding is mixed evenly
It is extremely thick, N- first is weighed with graduated cylinder in the ratio that mixed material and N-Methyl pyrrolidone (NMP) quality and volume ratio are 1:5
Base pyrrolidones (NMP), and N-Methyl pyrrolidone (NMP) is poured into beaker 3, with 3 hours of magnetic stirrer；
3) it takes the nickel foam (weighed quality) of 2 × 2cm to be placed on tetrafluoroethene plate, takes a small amount of graphite with glass bar is viscous
Alkene polyaniline slurry is uniformly applied to the end surface of nickel foam, application area 1cm2；
4) nickel foam for being coated with graphene polyaniline slurry is put into thermostatic drying chamber, under conditions of 82 DEG C, dry 5
A hour, tabletting weigh quality, and pole piece is successful；
5) the identical plastic plate with holes of two sizes and a nickel bar are taken, respectively with alcohol wipe and by nickel bar from plastics
The hole of plate penetrates 1.5cm；
6) in the nickel bar for taking nickel foam pole piece similar in two quality being just placed through respectively, nickel bar is not allowed to expose；
7) piece face-to-face mode in the two poles of the earth is superimposed together, centre is separated with glass fiber membrane, short to avoid two electrodes
Road, central filler KOH electrolyte are simultaneously packaged capacitor with polyester film and epoxy resin.
Embodiment 3:
Graphene oxide is prepared using Hummer oxidizing process:
1) taking 115mL concentration is 98% dense H2SO4It is added in the beaker of 1L, weighs the P of 2g2O5And the graphite powder of 4g
Dense H is added2SO4In, 2h is stirred with magnetic stirrer, set temperature is 4 DEG C；
2) KMnO of 14g is added in the solution being stirred4, it is slowly added to prevent heat release is too fast from bursting beaker, keeps molten
The temperature of liquid is lower than 20 DEG C, is heated to 34 DEG C, keeps the temperature 2.5h；
3) plus deionized water 225mL, control temperature stir 12min at 96 DEG C；
4) 0.5L deionized water is added by reaction terminating, meanwhile, the H of 15mL is added2O2；
5) acquired solution is being centrifuged by the hydrochloric acid for being 36% with mass concentration and water according to the HCL that the volume ratio of 1:10 is prepared
It is washed in machine twice, uses deionized water instead and continue washing until solution is in neutrality；
6) acquired solution is poured into beaker and deionized water 225mL dilution is added, be placed in ultrasonic agitation case, be allowed to uniform
Dispersion.
Graphene polyaniline composite material is prepared using the method that liquid level polymerize:
1) each 45ml of graphene oxide for weighing the ammonium persulfate solution of 1mol/L and preparing is poured into beaker 1, then is claimed
Amount 1g ascorbic acid is put into beaker 1, is stirred ten minutes with glass bar, is completely dissolved ascorbic acid；
2) it weighs the carbon tetrachloride solution of 50ml and 1ml aniline solution pours into beaker 2, stir 5 minutes；
3) liquid in beaker 1 is poured into beaker 2 in such a way that glass drains, sealing is placed 46 hours, aniline
Polymerization reaction occurs in the interface of two-phase with graphene oxide；
4) carbon tetrachloride solution to be extracted out, remaining graphene polyaniline solutions pour into 3 centrifuge tubes, it is centrifuged 3 times, it
After be put into thermostatic drying chamber it is 34 hours dry.
Prepare supercapacitor:
The specific method is as follows:
1) the graphene polyaniline composite material after drying is clayed into power shape with mortar；
2) in graphene polyaniline powder: conductive black: Kynoar=85:10:5 ratio weighs graphene polyphenyl
Amine powder, conductive black and Kynoar (PVDF), load weighted material is put into beaker 3, grinding is mixed evenly
It is extremely thick, N- first is weighed with graduated cylinder in the ratio that mixed material and N-Methyl pyrrolidone (NMP) quality and volume ratio are 1:5
Base pyrrolidones (NMP), and N-Methyl pyrrolidone (NMP) is poured into beaker 3, with 3 hours of magnetic stirrer；
3) it takes the nickel foam of 2 × 2cm to be placed on tetrafluoroethene plate, takes a small amount of graphene polyaniline slurry with glass bar is viscous
Uniformly it is applied to the end surface of nickel foam, application area 1cm2；
4) nickel foam for being coated with graphene polyaniline slurry is put into thermostatic drying chamber, under conditions of 78 DEG C, dry 5
A hour, tabletting weigh quality, and pole piece is successful；
5) the identical plastic plate with holes of two sizes and a nickel bar are taken, respectively with alcohol wipe and by nickel bar from plastics
The hole of plate penetrates 1cm；
6) in the nickel bar for taking nickel foam pole piece similar in two quality being just placed through respectively, nickel bar is not allowed to expose；
7) piece face-to-face mode in the two poles of the earth is superimposed together, centre is separated with glass fiber membrane, short to avoid two electrodes
Road, central filler KOH electrolyte are simultaneously packaged capacitor with polyester film and epoxy resin.
Claims (5)
1. the preparation method of the polyaniline laminated nanocomposite of supercapacitor graphene, which is characterized in that
Graphene oxide is prepared using Hummer oxidizing process first, by KMnO4It is added to dense H2SO4With P2O5, graphite powder is stirred
Mixed solution in, and keep the temperature, be added after deionized water stirring and deionized water is added makes reaction terminating；It is 20% with mass concentration
After~36% hydrochloric acid and water is washed according to the HCL that the volume ratio of 1:10 is prepared, deionized water continues washing to being in neutrality, and dilutes
And it stirs and is allowed to evenly dispersed；
Secondly graphene polyaniline composite material is prepared using method of liquid level polymerization, by the graphene oxide prepared and anti-bad
Hematic acid mixing is put into the stirring of beaker 1 and is completely dissolved to ascorbic acid, and carbon tetrachloride solution and aniline solution are put into beaker 2 and mixed
Stirring, is drained to beaker 2 for 1 solution of beaker, and aniline and graphene oxide are respectively placed in up and down in two-phase system, allow aniline and
In the interface of two-phase polymerization reaction occurs for graphene oxide, extracts carbon tetrachloride solution out after sealing a period of time, and by aniline
It is dry after graphene solution centrifugation, obtain graphene polyaniline composite material.
2. the preparation method of the polyaniline laminated nanocomposite of supercapacitor graphene according to claim 1,
Graphene oxide prepared it is characterized in that, described using Hummer oxidizing process the specific method is as follows:
1) taking 115-120mL mass concentration is 98% dense H2SO4It is added in the beaker of 1L, weighs the P of 2-4g2O5And 4-6g
Dense H is added in graphite powder2SO4In, 2-3h is stirred with magnetic stirrer, set temperature is 4-6 DEG C；
2) KMnO of 10-15g is added in the solution being stirred4, it is slowly added to prevent heat release is too fast from bursting beaker, keeps solution
Temperature be lower than 20 DEG C, be heated to 32-36 DEG C, keep the temperature 1.5-2.5h；
3) plus deionized water 225-235mL, control temperature stir 12-17min at 96-99 DEG C；
4) 0.5-0.9L deionized water is added by reaction terminating, meanwhile, the H of 11-15mL is added2O2；
5) with mass concentration be 20%~36% hydrochloric acid and water according to 1:10 volume ratio prepare HCL by acquired solution from
It is washed in scheming twice, uses deionized water instead and continue washing until solution is in neutrality；
6) acquired solution is poured into beaker and deionized water 225-235mL dilution is added, be placed in ultrasonic agitation case, be allowed to uniform
Dispersion.
3. the preparation method of the polyaniline laminated nanocomposite of supercapacitor graphene according to claim 1,
It is characterized in that, the method using liquid level polymerization prepares graphene polyaniline composite material, the specific method is as follows:
1) each 45-55ml of graphene oxide for weighing the ammonium persulfate solution of 0.5-1.5mol/L and preparing is poured into beaker 1,
0.5-1.5g ascorbic acid is weighed again to be put into beaker 1, is stirred ten minutes with glass bar, is completely dissolved ascorbic acid；
2) it weighs the carbon tetrachloride solution of 45-55ml and 1-3mL aniline solution pours into beaker 2, stir 5~10 minutes；
3) by the liquid in beaker 1 glass drain by way of pour into beaker 2, sealing place 45-50 hour, aniline with
In the interface of two-phase polymerization reaction occurs for graphene oxide；
4) carbon tetrachloride solution is extracted out, remaining graphene polyaniline solutions pour into 3 centrifuge tubes, centrifugation 3-6 times, later
It is put into thermostatic drying chamber 34-38 hours dry.
4. being prepared using the preparation method of supercapacitor described in claim 1 graphene polyaniline laminated composite material
The method of graphene polyaniline composite material preparation supercapacitor, which is characterized in that
A) production of condenser plate: the graphene polyaniline composite material after drying is clayed into power shape with mortar, by graphite
Alkene polyaniline powder and conductive black, which are mixed evenly, to be ground to thick, is poured into together with N-Methyl pyrrolidone (NMP)
Beaker 3, nickel foam is placed on tetrafluoroethene plate stirring a period of time, takes a small amount of graphene polyaniline to starch with glass bar is viscous
Material is uniformly applied to the end surface of nickel foam, and the nickel foam for being coated with graphene polyaniline slurry is put into thermostatic drying chamber and is done
Dry, tabletting, nickel foam pole piece is successful；
B) production of supercapacitor: taking the identical plastic plate with holes of two sizes and a nickel bar, uses alcohol wipe respectively,
Nickel bar is penetrated from the hole of plastic plate, it, should not in the nickel bar for taking two nickel foam pole pieces identical in quality being just placed through respectively
Nickel bar is allowed to expose；The two face-to-face modes of nickel foam pole piece are superimposed together, and centre is separated with glass fiber membrane, to avoid two electricity
Extremely short road；The vitreous carbon fibers film central filler KOH electrolyte of two nickel foam pole pieces and with polyester film and epoxy resin
Capacitor is packaged.
5. the method for preparation supercapacitor according to claim 4, which is characterized in that the specific method is as follows:
1) the graphene polyaniline composite material after drying is clayed into power shape with mortar；
2) in graphene polyaniline powder: conductive black: Kynoar=85:10:5 ratio weighs graphene polyaniline powder
End, conductive black and Kynoar, load weighted material is put into beaker 3, is mixed evenly and is ground to thick, presses
The ratio that mixed material and N-Methyl pyrrolidone quality and volume ratio are 1:5 weighs N-Methyl pyrrolidone with graduated cylinder, and will
N-Methyl pyrrolidone pours into beaker 3, with 3 hours of magnetic stirrer；
3) it takes the nickel foam of 2 × 2cm to be placed on tetrafluoroethene plate, takes graphene polyaniline obtained in step 2) with glass bar is viscous
Slurry is uniformly applied to the end surface of nickel foam, application area 1cm2；
4) nickel foam for being coated with graphene polyaniline slurry is put into thermostatic drying chamber, under conditions of 78-82 DEG C, dry 5
A hour, tabletting, nickel foam pole piece are successful；
5) the identical plastic plate with holes of two sizes and a nickel bar are taken, respectively with alcohol wipe and by nickel bar from plastic plate
Hole penetrates 0.5-1.5cm；
6) in the nickel bar for taking two nickel foam pole pieces identical in quality being just placed through respectively, nickel bar is not allowed to expose；
7) piece face-to-face mode in the two poles of the earth being superimposed together, centre is separated with glass fiber membrane, to avoid two electric pole short circuits, two
The vitreous carbon fibers film central filler KOH electrolyte of a nickel foam pole piece and with polyester film and epoxy resin to capacitor into
Row encapsulation.
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| CN117165130A (en) * | 2023-09-05 | 2023-12-05 | 无锡固山紧固件有限公司 | Processing technology of high-strength nut |
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| CN101281820A (en) * | 2007-04-04 | 2008-10-08 | 深圳市正宇能源科技有限公司 | Cascade type super capacitor and method for fabricating the same |
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| CN104119529A (en) * | 2014-08-02 | 2014-10-29 | 桂林理工大学 | Preparation method of polyaniline/graphene composite material with nano tubular structure |
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| CN117165130A (en) * | 2023-09-05 | 2023-12-05 | 无锡固山紧固件有限公司 | Processing technology of high-strength nut |
| CN117165130B (en) * | 2023-09-05 | 2024-01-26 | 无锡固山紧固件有限公司 | Processing technology of high-strength nut |
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