CN108376618A - Polyaniline/phytic acid conductive hydrogel and preparation method thereof and flexible super capacitor - Google Patents
Polyaniline/phytic acid conductive hydrogel and preparation method thereof and flexible super capacitor Download PDFInfo
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- CN108376618A CN108376618A CN201810258794.XA CN201810258794A CN108376618A CN 108376618 A CN108376618 A CN 108376618A CN 201810258794 A CN201810258794 A CN 201810258794A CN 108376618 A CN108376618 A CN 108376618A
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- Prior art keywords
- polyaniline
- phytic acid
- conductive hydrogel
- electrode
- preparation
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- IMQLKJBTEOYOSI-GPIVLXJGSA-N Inositol-hexakisphosphate Chemical compound OP(O)(=O)O[C@H]1[C@H](OP(O)(O)=O)[C@@H](OP(O)(O)=O)[C@H](OP(O)(O)=O)[C@H](OP(O)(O)=O)[C@@H]1OP(O)(O)=O IMQLKJBTEOYOSI-GPIVLXJGSA-N 0.000 title claims abstract description 68
- IMQLKJBTEOYOSI-UHFFFAOYSA-N Phytic acid Natural products OP(O)(=O)OC1C(OP(O)(O)=O)C(OP(O)(O)=O)C(OP(O)(O)=O)C(OP(O)(O)=O)C1OP(O)(O)=O IMQLKJBTEOYOSI-UHFFFAOYSA-N 0.000 title claims abstract description 68
- 235000002949 phytic acid Nutrition 0.000 title claims abstract description 68
- 239000000467 phytic acid Substances 0.000 title claims abstract description 68
- 229940068041 phytic acid Drugs 0.000 title claims abstract description 68
- 239000000017 hydrogel Substances 0.000 title claims abstract description 61
- 229920000767 polyaniline Polymers 0.000 title claims abstract description 59
- 239000003990 capacitor Substances 0.000 title claims abstract description 48
- 238000002360 preparation method Methods 0.000 title claims abstract description 34
- 238000000034 method Methods 0.000 claims abstract description 24
- PAYRUJLWNCNPSJ-UHFFFAOYSA-N Aniline Chemical compound NC1=CC=CC=C1 PAYRUJLWNCNPSJ-UHFFFAOYSA-N 0.000 claims description 54
- 229910052751 metal Inorganic materials 0.000 claims description 32
- 239000002184 metal Substances 0.000 claims description 32
- 239000000243 solution Substances 0.000 claims description 25
- 239000000758 substrate Substances 0.000 claims description 22
- -1 polyethylene terephthalate Polymers 0.000 claims description 20
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 18
- 239000011245 gel electrolyte Substances 0.000 claims description 15
- 239000008367 deionised water Substances 0.000 claims description 14
- 229910021641 deionized water Inorganic materials 0.000 claims description 14
- 239000011259 mixed solution Substances 0.000 claims description 13
- 239000003792 electrolyte Substances 0.000 claims description 11
- 239000000178 monomer Substances 0.000 claims description 11
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 10
- 239000010931 gold Substances 0.000 claims description 10
- 239000002253 acid Substances 0.000 claims description 9
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims description 9
- 229910052737 gold Inorganic materials 0.000 claims description 9
- 239000004698 Polyethylene Substances 0.000 claims description 8
- 239000002270 dispersing agent Substances 0.000 claims description 8
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 8
- 229920000573 polyethylene Polymers 0.000 claims description 8
- 229920000139 polyethylene terephthalate Polymers 0.000 claims description 8
- 239000005020 polyethylene terephthalate Substances 0.000 claims description 8
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 6
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 6
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 6
- 239000004743 Polypropylene Substances 0.000 claims description 6
- 238000000151 deposition Methods 0.000 claims description 6
- 230000008021 deposition Effects 0.000 claims description 6
- VLTRZXGMWDSKGL-UHFFFAOYSA-N perchloric acid Chemical compound OCl(=O)(=O)=O VLTRZXGMWDSKGL-UHFFFAOYSA-N 0.000 claims description 6
- 229920001155 polypropylene Polymers 0.000 claims description 6
- 238000001755 magnetron sputter deposition Methods 0.000 claims description 5
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 4
- 229910052802 copper Inorganic materials 0.000 claims description 4
- 239000010949 copper Substances 0.000 claims description 4
- 229910052697 platinum Inorganic materials 0.000 claims description 4
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 3
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 3
- 229910017052 cobalt Inorganic materials 0.000 claims description 3
- 239000010941 cobalt Substances 0.000 claims description 3
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims description 3
- 239000003822 epoxy resin Substances 0.000 claims description 3
- 229910052742 iron Inorganic materials 0.000 claims description 3
- 239000007769 metal material Substances 0.000 claims description 3
- 229910052759 nickel Inorganic materials 0.000 claims description 3
- 229920000647 polyepoxide Polymers 0.000 claims description 3
- 229920002635 polyurethane Polymers 0.000 claims description 3
- 239000004814 polyurethane Substances 0.000 claims description 3
- 229920000915 polyvinyl chloride Polymers 0.000 claims description 3
- 239000004800 polyvinyl chloride Substances 0.000 claims description 3
- 229910052709 silver Inorganic materials 0.000 claims description 3
- 239000004332 silver Substances 0.000 claims description 3
- 238000007738 vacuum evaporation Methods 0.000 claims description 3
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 claims description 2
- 239000004793 Polystyrene Substances 0.000 claims description 2
- 230000008859 change Effects 0.000 claims description 2
- 229910052748 manganese Inorganic materials 0.000 claims description 2
- 239000011572 manganese Substances 0.000 claims description 2
- 229920002223 polystyrene Polymers 0.000 claims description 2
- QQONPFPTGQHPMA-UHFFFAOYSA-N propylene Natural products CC=C QQONPFPTGQHPMA-UHFFFAOYSA-N 0.000 claims 1
- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 claims 1
- 229920005989 resin Polymers 0.000 claims 1
- 239000011347 resin Substances 0.000 claims 1
- 238000001947 vapour-phase growth Methods 0.000 claims 1
- 239000000463 material Substances 0.000 abstract description 14
- 238000006243 chemical reaction Methods 0.000 abstract description 12
- 238000006116 polymerization reaction Methods 0.000 abstract description 10
- 239000003999 initiator Substances 0.000 abstract description 6
- 238000004140 cleaning Methods 0.000 abstract description 5
- 230000000694 effects Effects 0.000 abstract description 4
- 230000008569 process Effects 0.000 abstract description 3
- 239000000126 substance Substances 0.000 abstract description 3
- 238000011065 in-situ storage Methods 0.000 abstract description 2
- 239000004372 Polyvinyl alcohol Substances 0.000 description 18
- 229920002451 polyvinyl alcohol Polymers 0.000 description 18
- 238000012360 testing method Methods 0.000 description 14
- 239000007772 electrode material Substances 0.000 description 13
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 12
- 229920002799 BoPET Polymers 0.000 description 11
- 230000005611 electricity Effects 0.000 description 9
- 238000005452 bending Methods 0.000 description 6
- 238000001035 drying Methods 0.000 description 6
- 239000011149 active material Substances 0.000 description 4
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 description 4
- 239000003431 cross linking reagent Substances 0.000 description 4
- 238000007747 plating Methods 0.000 description 4
- 238000000627 alternating current impedance spectroscopy Methods 0.000 description 3
- 238000002484 cyclic voltammetry Methods 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- 229920000178 Acrylic resin Polymers 0.000 description 2
- 239000004925 Acrylic resin Substances 0.000 description 2
- KKEYFWRCBNTPAC-UHFFFAOYSA-N Terephthalic acid Chemical compound OC(=O)C1=CC=C(C(O)=O)C=C1 KKEYFWRCBNTPAC-UHFFFAOYSA-N 0.000 description 2
- 239000000654 additive Substances 0.000 description 2
- 230000000996 additive effect Effects 0.000 description 2
- 229910001870 ammonium persulfate Inorganic materials 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 230000006870 function Effects 0.000 description 2
- 239000000499 gel Substances 0.000 description 2
- 230000003760 hair shine Effects 0.000 description 2
- QWPPOHNGKGFGJK-UHFFFAOYSA-N hypochlorous acid Chemical compound ClO QWPPOHNGKGFGJK-UHFFFAOYSA-N 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 230000014759 maintenance of location Effects 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 238000004626 scanning electron microscopy Methods 0.000 description 2
- 238000002604 ultrasonography Methods 0.000 description 2
- 239000003643 water by type Substances 0.000 description 2
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 1
- IMROMDMJAWUWLK-UHFFFAOYSA-N Ethenol Chemical compound OC=C IMROMDMJAWUWLK-UHFFFAOYSA-N 0.000 description 1
- 239000005977 Ethylene Substances 0.000 description 1
- 239000002033 PVDF binder Substances 0.000 description 1
- 238000013019 agitation Methods 0.000 description 1
- 150000001336 alkenes Chemical class 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- SVPXDRXYRYOSEX-UHFFFAOYSA-N bentoquatam Chemical compound O.O=[Si]=O.O=[Al]O[Al]=O SVPXDRXYRYOSEX-UHFFFAOYSA-N 0.000 description 1
- RUOKPLVTMFHRJE-UHFFFAOYSA-N benzene-1,2,3-triamine Chemical compound NC1=CC=CC(N)=C1N RUOKPLVTMFHRJE-UHFFFAOYSA-N 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 description 1
- 239000004327 boric acid Substances 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 239000006229 carbon black Substances 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000006258 conductive agent Substances 0.000 description 1
- 125000004122 cyclic group Chemical group 0.000 description 1
- 125000000118 dimethyl group Chemical group [H]C([H])([H])* 0.000 description 1
- 238000010528 free radical solution polymerization reaction Methods 0.000 description 1
- 238000001453 impedance spectrum Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000001764 infiltration Methods 0.000 description 1
- 230000008595 infiltration Effects 0.000 description 1
- 239000011244 liquid electrolyte Substances 0.000 description 1
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 229920001596 poly (chlorostyrenes) Polymers 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 229920006389 polyphenyl polymer Polymers 0.000 description 1
- 239000004810 polytetrafluoroethylene Substances 0.000 description 1
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 1
- 229920002981 polyvinylidene fluoride Polymers 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000008439 repair process Effects 0.000 description 1
- 229920005573 silicon-containing polymer Polymers 0.000 description 1
- 238000004544 sputter deposition Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 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
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
- H01G11/48—Conductive polymers
-
- 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
-
- 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
Landscapes
- Engineering & Computer Science (AREA)
- Power Engineering (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Chemical & Material Sciences (AREA)
- Materials Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Macromolecular Compounds Obtained By Forming Nitrogen-Containing Linkages In General (AREA)
Abstract
The present invention relates to Material Fields, in particular to a kind of polyaniline/phytic acid conductive hydrogel and preparation method thereof and flexible super capacitor.Polyaniline/phytic acid conductive hydrogel is prepared using electrochemical polymerization, the use of initiator can be effectively prevented from, and saves subsequent tedious cleaning process, greatly saves material preparation cost and time.This method can realize the growth in situ of material, and the homogeneity of the material prepared is good, thus device repeatability and have good stability.This method can regulate and control the load capacity of electroactive substance by controlling the concentration of each component in polymerization time or reaction solution, further achieve the effect that control flexible super capacitor capacity.
Description
Technical field
The present invention relates to Material Fields, in particular to a kind of polyaniline/phytic acid conductive hydrogel and preparation method thereof
And flexible super capacitor.
Background technology
Some in the prior art, the preparation method of layer/polyaniline conductive hydrogel is mainly (poly- by aniline monomer, framework material
Vinyl alcohol), the components such as crosslinking agent (phytic acid, triaminobenzene boric acid) be mixed with to obtain aqueous solution according to a certain percentage, then
Initiator (ammonium persulfate etc.) initiated polymerization is added, to obtain conductive hydrogel.Some separately having in the prior art, are gathered
The synthesis generally use solution polymerization process of aniline based aquagel：Aniline monomer, crosslinking agent and framework material are dissolved in water
Then middle formation mixed solution is added the initiators such as ammonium persulfate and causes monomer polymerization, ultimately forms aquogel system.
But or the product that these methods need that initiator is added or obtain needs to be placed on a large amount of deionized waters
Middle cleaning 24 hours or more, to remove initiator, by-product and excess ions.Complicated for operation, effect is poor.
The device architecture of flexible super capacitor is usually support substrate layer, current collector layers, anode layer, diaphragm+solid-state electricity
Matter (diaphragm+liquid electrolyte) layer, negative electrode layer, current collector layers are solved, classical architecture is the sandwich of electrode-electric solution liquid-electrode
Structure.
But the electrode of existing flexible super capacitor usually contains additive, as conductive agent carbon black, binder PTFE or
Person PVDF etc. so that flexible super capacitor is complicated, and the usual thickness of device is larger, it is difficult to which device is made very thin.
Invention content
The first object of the present invention is to provide a kind of preparation method of polyaniline/phytic acid conductive hydrogel, provides one kind
The new method for preparing polyaniline/phytic acid conductive hydrogel.
The second object of the present invention is to provide a kind of polyaniline/phytic acid conductive hydrogel.
The third object of the present invention is to provide a kind of flexible super capacitor, which is free of additive, the device
It retention property can stablize under the conditions ofs bending, folding etc., can be applied to flexible display and wearable electronic device.
To achieve the goals above, technical solution used in the embodiment of the present invention is as follows：
A kind of preparation method of polyaniline/phytic acid conductive hydrogel, including：Metal collector electricity is prepared on a flexible substrate
Pole；Prepare aniline/phytic acid mixed solution；By metal collector electrode assembling at three-electrode structure, metal collector electrode is soaked
Enter aniline/phytic acid mixed solution, voltage is applied to metal collector electrode, polyaniline/plant is deposited on metal collector electrode
Sour conductive hydrogel.
A kind of polyaniline/phytic acid conductive hydrogel electrode material, using above-mentioned polyaniline/phytic acid conductive hydrogel electrode
The preparation method of material is prepared.
A kind of flexible super capacitor, including basal electrode are deposited on basal electrode and are led just like above-mentioned polyaniline/phytic acid
Electric hydrogel；And PVA/H2SO4Gel electrolyte；PVA/H2SO4Gel electrolyte is cast in polyaniline/phytic acid conduction water-setting
The surface of gel electrode material.Wherein, PVA/H2SO4Gel electrolyte is to be add to deionized water electrolyte, PVA,
80-90 degrees Celsius of stirring is made；The mass ratio of electrolyte, PVA and deionized water is 1:1:10.
The beneficial effects of the invention are as follows：
A kind of preparation method of polyaniline/phytic acid conductive hydrogel provided by the invention, prepares metal on a flexible substrate
Collector electrode；Prepare aniline/phytic acid mixed solution；By metal collector electrode assembling at three-electrode structure, by metal afflux
Body electrode immerses aniline/phytic acid mixed solution, applies voltage to metal collector electrode, is deposited on metal collector electrode poly-
Aniline/phytic acid conductive hydrogel.Layer/polyaniline conductive hydrogel electrode material, Neng Gouyou are prepared using this electrochemical polymerization
The use of initiator is avoided to effect, and saves subsequent tedious cleaning process, greatly saves material preparation cost and time.
This method can realize the growth in situ of material, and the homogeneity of the material prepared is good, thus device is repeatable
Property and have good stability.This method can regulate and control electrification by controlling the concentration of each component in polymerization time or reaction solution
The load capacity for learning active material further achievees the effect that control flexible super capacitor capacity.
A kind of polyaniline/phytic acid conductive hydrogel provided by the invention, using above-mentioned polyaniline/phytic acid conductive hydrogel
Preparation method be prepared, which can be used in preparing flexible super electrode.
A kind of flexible super capacitor provided by the invention, including basal electrode and PVA/H2SO4Gel electrolyte.Base
Deposition has polyaniline/phytic acid conductive hydrogel on hearth electrode.PVA/H2SO4Gel electrolyte is cast in polyaniline/phytic acid conductivity water
The surface of gel electrode material.Wherein, PVA/H2SO4Gel electrolyte is to be add to deionized water electrolyte, PVA,
It stirs and is made at 80-90 degrees Celsius；The mass ratio of electrolyte, PVA and deionized water is 1:1:10.Flexible super electricity
Container breaks through the larger drawback of conventional flex ultracapacitor thickness, the flexible super capacitor for the PET film support prepared
Integral thickness be only 200-300 μm, effective work area be 0.813cm2, this device quality is light, thickness is thin, flexible,
It is easily achieved the Surface Mounting Technology function of flexible capacitor.The flexible super capacitor has good mechanical flexibility, in bending, turns round
Under the states such as song, the performance of device still is able to keep stablizing, this characteristic makes it be expected to become flexible display device, wearable electricity
The energy source of sub- device.The flexible super capacitor can also be designed by further series and parallel structure, to realize difference
Power and energy output, meet the different demands in practical application.
Description of the drawings
In order to illustrate the technical solution of the embodiments of the present invention more clearly, below will be to needed in the embodiment attached
Figure is briefly described, it should be understood that the following drawings illustrates only certain embodiments of the present invention, therefore is not construed as pair
The restriction of range for those of ordinary skill in the art without creative efforts, can also be according to this
A little attached drawings obtain other relevant attached drawings.
Fig. 1 is that scanning electron microscopy of the polyaniline provided in an embodiment of the present invention/phytic acid hydrogel under the first multiple shines
Piece；
Fig. 2 is that scanning electron microscopy of the polyaniline provided in an embodiment of the present invention/phytic acid hydrogel under the second multiple shines
Piece；
Fig. 3 is flexible super capacitor lateral flexibility test result provided in an embodiment of the present invention；
Fig. 4 is flexible super capacitor longitudinal flexible test result provided in an embodiment of the present invention；
Fig. 5 is the cycle under bending, distortion, undeformed state of flexible super capacitor provided in an embodiment of the present invention
Volt-ampere curve；
Fig. 6 is cyclic voltammetry curve of the flexible super capacitor provided in an embodiment of the present invention under different scanning rates
Figure；
Fig. 7 is constant current charge-discharge curve of the flexible super capacitor provided in an embodiment of the present invention under different current densities
Figure；
Fig. 8 is the AC impedance spectroscopy of flexible super capacitor provided in an embodiment of the present invention；
Fig. 9 is two cascaded structure schematic diagrames of flexible super capacitor provided in an embodiment of the present invention；
Figure 10 is three cascaded structure schematic diagrames of flexible super capacitor provided in an embodiment of the present invention；
Figure 11 is the constant current charge-discharge number and capacity retention ratio of flexible super capacitor provided in an embodiment of the present invention
Schematic diagram.
Specific implementation mode
Embodiment of the present invention is described in detail below in conjunction with embodiment, but those skilled in the art will
Understand, the following example is merely to illustrate the present invention, and is not construed as limiting the scope of the invention.It is not specified in embodiment specific
Condition person carries out according to conventional conditions or manufacturer's recommended conditions.Reagents or instruments used without specified manufacturer is
The conventional products that can be obtained by commercially available purchase.
In the description of the present invention, it should be noted that term " first ", " second " etc. are only used for distinguishing description, without
It can be interpreted as indicating or implying relative importance.
Below to the polyaniline of the embodiment of the present invention/phytic acid conductive hydrogel and preparation method thereof and flexible super capacitance
Device is specifically described.
A kind of preparation method of polyaniline/phytic acid conductive hydrogel provided in an embodiment of the present invention, including：
S1, metal collector electrode is prepared on a flexible substrate.
Further, flexible substrates are selected from polyethylene terephthalate, polyethylene, polypropylene, polyvinyl chloride, polyphenyl
Any one in ethylene, acrylic resin, epoxy resin or polyurethane.
Further, metal collector electrode is selected from least one of gold, platinum, silver, copper, nickel, cobalt, manganese or iron.
Still optionally further, above-mentioned metal collector electrode selection gold.Flexible substrates select poly terephthalic acid second two
Alcohol ester.
Further, it is by the way that metal material is used magnetron sputtering to prepare metal collector electrode on a flexible substrate
Method, vacuum evaporation, chemical meteorology deposition or solwution method are deposited to flexible substrates.
Still optionally further, selection by metal material by using magnetic when preparing metal collector electrode on a flexible substrate
Control sputtering method is deposited to flexible substrates.
Further, it is to prepare interdigital electrode on a flexible substrate to prepare metal collector electrode on a flexible substrate.
Specifically, polyethylene terephthalate (PET) film that thickness is 30-200 μm is chosen, is cut into rectangular
Shape is cleaned by ultrasonic several times with deionized water and acetone, and drying is for use.Interdigital structure is processed using ultraviolet laser cold processing technique
Mask plate.Stick mask plate in clean PET film, then by magnetron sputtering technique in PET film plated with gold (Au)
Interdigital electrode.
It should be noted that the finger spacing selection of interdigital electrode obtained above is more than 0.4mm, so as to effectively keep away
Exempt from two electric pole short circuits.The finger beam of interdigital electrode obtained above can be according to actual demand unrestricted choice.
S2, aniline/phytic acid mixed solution is prepared.
Further, aniline/phytic acid mixed solution is that plant acid solution, aniline monomer and dispersant are prepared.
Optionally, above-mentioned dispersant is selected from least one of sulfuric acid, phosphoric acid or perchloric acid.
It should be noted that in other optional embodiments of the invention, above-mentioned dispersant can select water.
When further, by plant acid solution, aniline monomer and dispersant, the concentration of each raw material can be as needed
Selection.Aniline/phytic acid mixed solution concentration is smaller, and the quality of the active material deposited in the unit interval is fewer, and aniline/phytic acid is mixed
The quality for closing the active material that solution concentration is bigger, is deposited in the unit interval is more.
S3, by metal collector electrode assembling at three-electrode structure, metal collector electrode is immersed into aniline/phytic acid and is mixed
Solution applies voltage to metal collector electrode, makes layer/polyaniline conductive hydrogel deposit electrode material in metal collector electrode
On.
Specifically, the PET film for plating gold electrode is assembled in three-electrode structure, and interdigital electrode part is immersed instead
It answers in solution, applies certain constant voltage to electrode on electrochemical workstation, certain voltage stabling control is set, you can pitching
Refer to the upper polyaniline/phytic acid conductive hydrogel electrode material of deposition on electrode.
It should be noted that above-mentioned apply certain constant voltage on electrochemical workstation to electrode, it can be according to reality
Border needs to select suitable voltage range.In the present embodiment, optionally, above-mentioned constant voltage selects 0.3-1.0V.It is above-mentioned
On electrochemical workstation, certain voltage stabling control is set, suitable voltage stabling control range can also be selected according to actual needs.
In the present embodiment, optionally, above-mentioned voltage stabling control range selects 60-900s.Polymerization time is longer, deposits on a current collector
Electrochemical active material it is more.
It is above-mentioned when preparing aniline mixed solution, it can select aniline monomer and crosslinking agent and dispersant being prepared instead
Precursor solution is answered, then hydrogel is formed using the method for electrochemical polymerization.Above-mentioned crosslinking agent can select this field other
Common material applicatory.Above-mentioned dispersant can select other common materials applicatory of this field.
Some embodiments of the present invention also provide a kind of polyaniline/phytic acid conductive hydrogel, using above-mentioned polyaniline/
The preparation method of phytic acid conductive hydrogel is prepared.
Some embodiments of the present invention also provide a kind of flexible super capacitor, including basal electrode and PVA/H2SO4
Gel electrolyte.Deposition has polyaniline/phytic acid conductive hydrogel on basal electrode. PVA/H2SO4Gel electrolyte is cast in poly-
The surface of aniline/phytic acid conductive hydrogel electrode material.Wherein, PVA/H2SO4Gel electrolyte is to add electrolyte, PVA
Enter into deionized water, stirs and be made at 80-90 degrees Celsius；The mass ratio of electrolyte, PVA and deionized water is 1:
1:10。
The flexible super capacitor breaks through the larger drawback of conventional flex ultracapacitor thickness, the PET film prepared
The integral thickness of the flexible super capacitor of support is only 200-300 μm, and effective work area is 0.813cm2, this device matter
Amount is light, thickness is thin, flexible, it is easy to accomplish the Surface Mounting Technology function of flexible capacitor.The flexible super capacitor has good
Mechanical flexibility, under the states such as bending, distortion, the performance of device still is able to keep stablizing, this characteristic makes it be expected to become soft
Property display equipment, wearable electronic device energy source.The flexible super capacitor can also pass through further connection in series-parallel knot
Structure designs, and to realize different power and energy output, meets the different demands in practical application.
The feature and performance of the present invention are described in further detail with reference to embodiments：
Embodiment 1
A kind of polyaniline/phytic acid conductive hydrogel provided in this embodiment, preparation method are as follows：
Polyethylene terephthalate (PET) film that thickness is 50 μm is chosen, the rectangle of 2 × 3 cm is cut into,
It is cleaned by ultrasonic several times with deionized water and acetone, drying is for use.Covering for interdigital structure is processed using ultraviolet laser cold processing technique
Film version.Stick mask plate in clean PET film, then by magnetron sputtering technique in PET film the interdigital electricity of plated with gold
The finger beam of pole, interdigital electrode is 1 mm, and it is 0.8mm to refer to spacing.2.21mL (2.4mmol) 50wt% plant acid solutions are measured,
1.10mL (12mmol) aniline monomer is added in the sulfuric acid of 60mL 1mol/L, obtains reaction solution.Gold electrode will be plated
PET film is assembled in three-electrode structure, and interdigital electrode part is immersed in reaction solution, to electricity on electrochemical workstation
Pole applies the constant voltage of 0.8V, and setting voltage stabling control is 300s, you can deposits upper polyaniline/phytic acid in interdigital electrode and leads
Electric hydrogel electrode material.
Embodiment 2
A kind of polyaniline/phytic acid conductive hydrogel provided in this embodiment, preparation method are as follows：
The polyethylene film that thickness is 30 μm is chosen, the rectangle of 2 × 3cm is cut into, with deionized water and acetone ultrasound
Several times, drying is for use for cleaning.The mask plate of interdigital structure is processed using ultraviolet laser cold processing technique.It is thin in clean polyethylene
Mask plate is sticked on film, then plates platinum interdigital electrode on polyethylene film by vacuum evaporation, and the finger beam of interdigital electrode is
1mm, it is 0.5mm to refer to spacing.2.21mL (2.4mmol) 50wt% plant acid solutions are measured, 1.10mL (12mmol) aniline monomer adds
Enter the H to 60mL 1mol/L3PO4In, obtain reaction solution.The polyethylene film for plating platinum electrode is assembled in three-electrode structure
In, and interdigital electrode part is immersed in reaction solution, apply the constant voltage of 0.5V to electrode on electrochemical workstation, if
It is 60s to set voltage stabling control, you can upper polyaniline/phytic acid conductive hydrogel electrode material is deposited in interdigital electrode.
Embodiment 3
A kind of polyaniline/phytic acid conductive hydrogel provided in this embodiment, preparation method are as follows：
The polyvinyl chloride film that thickness is 100 μm is chosen, the rectangle of 2 × 3cm is cut into, it is super with deionized water and acetone
Sound cleans several times, and drying is for use.The mask plate of interdigital structure is processed using ultraviolet laser cold processing technique.In clean polychlorostyrene second
Mask plate is sticked on alkene film, and plated with copper interdigital electrode on polypropylene film is then deposited on by solwution method, interdigital electrode
Finger beam is 1mm, and it is 0.9mm to refer to spacing.Measure 2.21mL (2.4mmol) 50wt% plant acid solutions, 1.10mL (12mmol) benzene
Amine monomers are added to the HClO of 60mL 1mol/L4In, obtain reaction solution.The polyethylene film for plating copper electrode is assembled in
In three-electrode structure, and interdigital electrode part is immersed in reaction solution, applies 0.3V's to electrode on electrochemical workstation
Constant voltage, setting voltage stabling control are 500s, you can upper polyaniline/phytic acid conductive hydrogel electrode material is deposited in interdigital electrode
Material.
Embodiment 4
A kind of polyaniline/phytic acid conductive hydrogel provided in this embodiment, preparation method are as follows：
The polypropylene film that thickness is 200 μm is chosen, the rectangle of 2 × 3cm is cut into, with deionized water and acetone ultrasound
Several times, drying is for use for cleaning.The mask plate of interdigital structure is processed using ultraviolet laser cold processing technique.It is thin in clean polypropylene
Mask plate is sticked on film, then plates silver-colored interdigital electrode, the finger of interdigital electrode on polypropylene film by chemical meteorology deposition
Width is 1mm, and it is 0.6 mm to refer to spacing.Measure 2.21mL (2.4mmol) 50wt% plant acid solutions, 1.10mL (12mmol) aniline list
Body is added to the HClO of 60mL 1mol/L4In, obtain reaction solution.The polyethylene film for plating silver electrode is assembled in three electricity
In the structure of pole, and interdigital electrode part is immersed in reaction solution, applies the constant of 1.0V to electrode on electrochemical workstation
Voltage, setting voltage stabling control are 900s, you can upper polyaniline/phytic acid conductive hydrogel electrode material is deposited in interdigital electrode.
Embodiment 5
A kind of polyaniline/phytic acid conductive hydrogel provided in this embodiment, the basic step phase of preparation method and embodiment 1
Together, institute the difference is that, metal collector electrode in the present embodiment selects nickel, flexible substrates to select polystyrene.
Embodiment 6
A kind of polyaniline/phytic acid conductive hydrogel provided in this embodiment, the basic step phase of preparation method and embodiment 1
Together, institute the difference is that, metal collector electrode in the present embodiment selects cobalt, flexible substrates to select acrylic resin.
Embodiment 7
A kind of polyaniline/phytic acid conductive hydrogel provided in this embodiment, the basic step phase of preparation method and embodiment 1
Together, institute the difference is that, metal collector electrode in the present embodiment selects manganese, flexible substrates to select epoxy resin.
Embodiment 8
A kind of polyaniline/phytic acid conductive hydrogel provided in this embodiment, the basic step phase of preparation method and embodiment 1
Together, institute the difference is that, metal collector electrode in the present embodiment selects iron, flexible substrates to select polyurethane.
Embodiment 9
A kind of flexible super capacitor provided in this embodiment, preparation method are as follows：
Polyethylene terephthalate (PET) film that thickness is 50 μm is chosen, the rectangle of 2 × 3 cm is cut into,
It is cleaned by ultrasonic several times with deionized water and acetone, drying is for use.Covering for interdigital structure is processed using ultraviolet laser cold processing technique
Film version.Stick mask plate in clean PET film, then by magnetron sputtering technique in PET film the interdigital electricity of plated with gold
The finger beam of pole, interdigital electrode is 1 mm, and it is 0.8mm to refer to spacing.2.21mL (2.4mmol) 50wt% plant acid solutions are measured,
1.10mL (12mmol) aniline monomer is added in the sulfuric acid of 60mL 1mol/L, obtains reaction solution.Gold electrode will be plated
PET film is assembled in three-electrode structure, and interdigital electrode part is immersed in reaction solution, to electricity on electrochemical workstation
Pole applies the constant voltage of 0.8V, and setting voltage stabling control is 300s, you can deposits upper polyaniline/phytic acid in interdigital electrode and leads
Electric hydrogel electrode material.
5g polyvinyl alcohol (PVA) particle is weighed, the 5g concentrated sulfuric acids are added in 50g deionized waters, 85 C water baths'
Under the conditions of magnetic agitation two hours, obtain the PVA/H of clear2SO4Gel electrolyte.
Using gel electrolyte placingJi Shu, the PVA/H that will be prepared2SO4Gel electrolyte is cast in interdigital electrode table
Face, outermost layer are packaged with dimethyl silicone polymer (PDMS) again, you can obtain being based on electrochemical polymerization polyaniline hydrogel
Flexible interdigital flexible super capacitor.
Embodiment 10
A kind of flexible super capacitor provided in this embodiment, preparation method is identical as the basic step of embodiment 9, and institute is not
It is with place, the electrolyte in the present embodiment selects phosphoric acid, bath temperature to select 80 degrees Celsius.
Embodiment 11
A kind of flexible super capacitor provided in this embodiment, preparation method is identical as the basic step of embodiment 9, and institute is not
It is with place, the electrolyte in the present embodiment selects perchloric acid, bath temperature to select 90 degrees Celsius.
The performance for polyaniline/phytic acid conductive hydrogel that embodiment 1-8 is provided is investigated with reference to test example.
Test example 1
The structure of the polyaniline that embodiment 1-8 is prepared using scanning electron microscope/phytic acid conductive hydrogel is detected.
Testing result is as depicted in figs. 1 and 2.
As can be seen that polyaniline/phytic acid hydrogel that electrochemical polymerization prepares is in three-dimensional network shape from SEM photograph
Structure, material body are cross-linked with each other the cross-linked structure formed by nano level microballoon, and this structure is conducive to electrolyte
Infiltration and ion transmission.
Test example 2
The flexibility of the embodiment 9-11 flexible super capacitors provided is tested, test result is shown in Fig. 3 and Fig. 4.
From figure 3, it can be seen that flexible super capacitor has good flexibility, it can be with transverse curvature.It can be with from Fig. 4
Find out, flexible super capacitor has good flexibility, can be with buckling.
Further, Fig. 5, the shape of cyclic voltammetry curve of the flexible super capacitor under bending, twisted state are please referred to
The shape of shape and the test curve under undeformed state is consistent substantially, this illustrates that device can be in states such as bending, distortions
Lower its electrochemical stability of holding.
Test example 3
Cyclic voltammetric and constant current charge-discharge are investigated to the flexible super capacitor that embodiment 9-11 is provided, as a result see Fig. 6 and
Fig. 7.
Such as Fig. 6, in cyclic voltammetry curve, it can clearly be seen that the distinctive redox peaks of a pair of conductive high polymer, and
And the shape of CV curves is held essentially constant under different sweep speeds, illustrates that device has good high rate performance.Such as figure
7, in constant current charge-discharge curve, charging curve and discharge curve are in symmetrical triangular shaped, illustrate the coulombic efficiency of device
It is very high.
Test example 4
Ac impedance spectroscopy is investigated to the flexible super capacitor that embodiment 9-11 is provided, as a result sees Fig. 8.
It is 0.01-100000Hz in the test frequency of ac impedance spectroscopy, in the low frequency range of impedance spectrum, EIS curves almost hang down
Directly, illustrate that double capacitive properties of device are preferable, in high frequency region, the intercept of EIS and horizontal axis is 5.2, illustrates the equivalent series of device
Resistance very little, only 5.2 Ω or so.
Test example 5
Two series connection, three concatenated structures can be designed to the embodiment 9-11 flexible super capacitors provided.As a result
See Fig. 9 and Figure 10.
Test example 6
Cyclical stability is investigated to the flexible super capacitor that embodiment 9-11 is provided.
Test result shows that flexible super capacitor shows up to 562mFcm-2Face capacitance and 311Fg-1's
Quality specific capacitance.Further, as shown in figure 11, flexible super capacitor its appearance after 3000 constant current charge-discharges recycle
It is about 83% to measure conservation rate, illustrates that the cyclical stability of device is good.
The foregoing is only a preferred embodiment of the present invention, is not intended to restrict the invention, for the skill of this field
For art personnel, the invention may be variously modified and varied.All within the spirits and principles of the present invention, any made by repair
Change, equivalent replacement, improvement etc., should all be included in the protection scope of the present invention.
Claims (10)
1. a kind of preparation method of polyaniline/phytic acid conductive hydrogel, which is characterized in that including：
Metal collector electrode is prepared on a flexible substrate；
Prepare aniline/phytic acid mixed solution；
By the metal collector electrode assembling at three-electrode structure, the metal collector electrode is immersed into the aniline/plant
Sour mixed solution applies voltage to the metal collector electrode, polyaniline/phytic acid is deposited on the metal collector electrode
Conductive hydrogel.
2. the preparation method of polyaniline as described in claim 1/phytic acid conductive hydrogel, which is characterized in that
The flexible substrates are selected from polyethylene terephthalate, polyethylene, polypropylene, polyvinyl chloride, polystyrene, propylene
Any one in acid resin, epoxy resin or polyurethane.
3. the preparation method of polyaniline as described in claim 1/phytic acid conductive hydrogel, which is characterized in that
The metal collector electrode is selected from least one of gold, platinum, silver, copper, nickel, cobalt, manganese or iron.
4. the preparation method of polyaniline as described in any one of claims 1-3/phytic acid conductive hydrogel, which is characterized in that
The aniline/phytic acid mixed solution is that plant acid solution, aniline monomer and dispersant are prepared.
5. the preparation method of polyaniline as claimed in claim 4/phytic acid conductive hydrogel, which is characterized in that
The dispersant is selected from least one of sulfuric acid, phosphoric acid or perchloric acid.
6. the preparation method of polyaniline as described in claim 1/phytic acid conductive hydrogel, which is characterized in that
It is by the way that metal material is used magnetron sputtering method, vacuum evaporation, change to prepare metal collector electrode on a flexible substrate
It learns vapor phase deposition or solwution method is deposited to the flexible substrates.
7. the preparation method of polyaniline as claimed in claim 6/phytic acid conductive hydrogel, which is characterized in that
It is to prepare interdigital electrode in the flexible substrates to prepare metal collector electrode on a flexible substrate.
8. a kind of polyaniline/phytic acid conductive hydrogel, which is characterized in that led using polyaniline/phytic acid as described in claim 1
The preparation method of electric hydrogel is prepared.
9. a kind of flexible super capacitor, which is characterized in that the flexible super capacitor includes：
Basal electrode, deposition has polyaniline as described in claim 1/phytic acid conductive hydrogel on the basal electrode；And
PVA/H2SO4Gel electrolyte；The PVA/H2SO4Gel electrolyte is cast in the polyaniline/phytic acid conductive hydrogel
The surface of electrode.
10. flexible super capacitor as claimed in claim 9, which is characterized in that
The PVA/H2SO4Gel electrolyte is to be add to deionized water electrolyte, PVA, is stirred at 80-90 degrees Celsius
Mixing obtains；The mass ratio of the electrolyte, the PVA and the deionized water is 1:1:10.
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