CN110415857A - A kind of Nitrogen-rich porous carbon is the electrochemical actuator and preparation method thereof of electrode - Google Patents
A kind of Nitrogen-rich porous carbon is the electrochemical actuator and preparation method thereof of electrode Download PDFInfo
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- CN110415857A CN110415857A CN201910667088.5A CN201910667088A CN110415857A CN 110415857 A CN110415857 A CN 110415857A CN 201910667088 A CN201910667088 A CN 201910667088A CN 110415857 A CN110415857 A CN 110415857A
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- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 title claims abstract description 166
- 229910052757 nitrogen Inorganic materials 0.000 title claims abstract description 84
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 48
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 45
- 238000002360 preparation method Methods 0.000 title claims abstract description 37
- 239000003575 carbonaceous material Substances 0.000 claims abstract description 40
- -1 zeolite imidazole ester Chemical class 0.000 claims abstract description 30
- RAXXELZNTBOGNW-UHFFFAOYSA-N imidazole Natural products C1=CNC=N1 RAXXELZNTBOGNW-UHFFFAOYSA-N 0.000 claims abstract description 24
- 239000002608 ionic liquid Substances 0.000 claims abstract description 24
- 239000003792 electrolyte Substances 0.000 claims abstract description 15
- 229910021536 Zeolite Inorganic materials 0.000 claims abstract description 11
- 229920002521 macromolecule Polymers 0.000 claims abstract description 11
- 239000010457 zeolite Substances 0.000 claims abstract description 11
- 239000011159 matrix material Substances 0.000 claims abstract description 10
- 239000002322 conducting polymer Substances 0.000 claims abstract description 7
- 229920001940 conductive polymer Polymers 0.000 claims abstract description 7
- 239000000853 adhesive Substances 0.000 claims abstract description 5
- 230000001070 adhesive effect Effects 0.000 claims abstract description 5
- 239000013153 zeolitic imidazolate framework Substances 0.000 claims description 48
- 239000000243 solution Substances 0.000 claims description 25
- 229920000144 PEDOT:PSS Polymers 0.000 claims description 23
- 239000000463 material Substances 0.000 claims description 22
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 16
- 238000007731 hot pressing Methods 0.000 claims description 15
- 229910052751 metal Inorganic materials 0.000 claims description 13
- 239000002184 metal Substances 0.000 claims description 13
- 239000006185 dispersion Substances 0.000 claims description 12
- 239000007788 liquid Substances 0.000 claims description 12
- 238000000034 method Methods 0.000 claims description 12
- 239000004814 polyurethane Substances 0.000 claims description 10
- 229920002635 polyurethane Polymers 0.000 claims description 10
- IBZJNLWLRUHZIX-UHFFFAOYSA-N 1-ethyl-3-methyl-2h-imidazole Chemical compound CCN1CN(C)C=C1 IBZJNLWLRUHZIX-UHFFFAOYSA-N 0.000 claims description 9
- 239000007864 aqueous solution Substances 0.000 claims description 9
- 150000003839 salts Chemical class 0.000 claims description 8
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 6
- 239000003960 organic solvent Substances 0.000 claims description 5
- 230000001681 protective effect Effects 0.000 claims description 5
- 238000005245 sintering Methods 0.000 claims description 5
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 4
- 229920001661 Chitosan Polymers 0.000 claims description 4
- 150000001868 cobalt Chemical class 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 4
- 150000003751 zinc Chemical class 0.000 claims description 4
- ONDPHDOFVYQSGI-UHFFFAOYSA-N zinc nitrate Chemical compound [Zn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O ONDPHDOFVYQSGI-UHFFFAOYSA-N 0.000 claims description 4
- 238000004090 dissolution Methods 0.000 claims description 3
- 238000003837 high-temperature calcination Methods 0.000 claims description 3
- 229920000172 poly(styrenesulfonic acid) Polymers 0.000 claims description 3
- 238000000197 pyrolysis Methods 0.000 claims description 3
- MCTWTZJPVLRJOU-UHFFFAOYSA-N 1-methyl-1H-imidazole Chemical compound CN1C=CN=C1 MCTWTZJPVLRJOU-UHFFFAOYSA-N 0.000 claims description 2
- GKWLILHTTGWKLQ-UHFFFAOYSA-N 2,3-dihydrothieno[3,4-b][1,4]dioxine Chemical compound O1CCOC2=CSC=C21 GKWLILHTTGWKLQ-UHFFFAOYSA-N 0.000 claims description 2
- LXBGSDVWAMZHDD-UHFFFAOYSA-N 2-methyl-1h-imidazole Chemical compound CC1=NC=CN1 LXBGSDVWAMZHDD-UHFFFAOYSA-N 0.000 claims description 2
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 claims description 2
- ZOIORXHNWRGPMV-UHFFFAOYSA-N acetic acid;zinc Chemical compound [Zn].CC(O)=O.CC(O)=O ZOIORXHNWRGPMV-UHFFFAOYSA-N 0.000 claims description 2
- 229910052786 argon Inorganic materials 0.000 claims description 2
- GVPFVAHMJGGAJG-UHFFFAOYSA-L cobalt dichloride Chemical compound [Cl-].[Cl-].[Co+2] GVPFVAHMJGGAJG-UHFFFAOYSA-L 0.000 claims description 2
- UFMZWBIQTDUYBN-UHFFFAOYSA-N cobalt dinitrate Chemical compound [Co+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O UFMZWBIQTDUYBN-UHFFFAOYSA-N 0.000 claims description 2
- 229910001981 cobalt nitrate Inorganic materials 0.000 claims description 2
- 239000007789 gas Substances 0.000 claims description 2
- 150000002500 ions Chemical class 0.000 claims description 2
- 239000000203 mixture Substances 0.000 claims description 2
- 239000013174 zeolitic imidazolate framework-10 Substances 0.000 claims description 2
- 239000013175 zeolitic imidazolate framework-11 Substances 0.000 claims description 2
- 239000013176 zeolitic imidazolate framework-12 Substances 0.000 claims description 2
- 239000013154 zeolitic imidazolate framework-8 Substances 0.000 claims description 2
- 239000004246 zinc acetate Substances 0.000 claims description 2
- NWONKYPBYAMBJT-UHFFFAOYSA-L zinc sulfate Chemical compound [Zn+2].[O-]S([O-])(=O)=O NWONKYPBYAMBJT-UHFFFAOYSA-L 0.000 claims description 2
- 229960001763 zinc sulfate Drugs 0.000 claims description 2
- 229910000368 zinc sulfate Inorganic materials 0.000 claims description 2
- MFLKDEMTKSVIBK-UHFFFAOYSA-N zinc;2-methylimidazol-3-ide Chemical compound [Zn+2].CC1=NC=C[N-]1.CC1=NC=C[N-]1 MFLKDEMTKSVIBK-UHFFFAOYSA-N 0.000 claims description 2
- ZHNUHDYFZUAESO-UHFFFAOYSA-N Formamide Chemical compound NC=O ZHNUHDYFZUAESO-UHFFFAOYSA-N 0.000 claims 2
- 150000004676 glycans Chemical class 0.000 claims 1
- 150000002460 imidazoles Chemical class 0.000 claims 1
- 239000012621 metal-organic framework Substances 0.000 abstract description 9
- 239000011664 nicotinic acid Substances 0.000 abstract description 2
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 description 18
- 238000006073 displacement reaction Methods 0.000 description 17
- 229920000642 polymer Polymers 0.000 description 8
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 8
- 239000004810 polytetrafluoroethylene Substances 0.000 description 8
- 239000004809 Teflon Substances 0.000 description 6
- 229920006362 Teflon® Polymers 0.000 description 6
- 229920001746 electroactive polymer Polymers 0.000 description 6
- 239000000126 substance Substances 0.000 description 6
- 238000002484 cyclic voltammetry Methods 0.000 description 5
- 229920000867 polyelectrolyte Polymers 0.000 description 5
- 239000002904 solvent Substances 0.000 description 5
- 230000005611 electricity Effects 0.000 description 4
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 3
- 230000005540 biological transmission Effects 0.000 description 3
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 description 3
- 230000005518 electrochemistry Effects 0.000 description 3
- 239000006260 foam Substances 0.000 description 3
- 229920000831 ionic polymer Polymers 0.000 description 3
- 239000002905 metal composite material Substances 0.000 description 3
- 229910052755 nonmetal Inorganic materials 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- 239000010936 titanium Substances 0.000 description 3
- 229910052719 titanium Inorganic materials 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical group CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- YTPLMLYBLZKORZ-UHFFFAOYSA-N Thiophene Chemical compound C=1C=CSC=1 YTPLMLYBLZKORZ-UHFFFAOYSA-N 0.000 description 2
- 238000004833 X-ray photoelectron spectroscopy Methods 0.000 description 2
- 239000002041 carbon nanotube Substances 0.000 description 2
- 229910021393 carbon nanotube Inorganic materials 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 230000005012 migration Effects 0.000 description 2
- 238000013508 migration Methods 0.000 description 2
- 229910000510 noble metal Inorganic materials 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- UINDRJHZBAGQFD-UHFFFAOYSA-N 2-ethyl-1-methylimidazole Chemical compound CCC1=NC=CN1C UINDRJHZBAGQFD-UHFFFAOYSA-N 0.000 description 1
- 150000008614 2-methylimidazoles Chemical class 0.000 description 1
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 1
- 241000790917 Dioxys <bee> Species 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 1
- ISRUGXGCCGIOQO-UHFFFAOYSA-N Rhoden Chemical compound CNC(=O)OC1=CC=CC=C1OC(C)C ISRUGXGCCGIOQO-UHFFFAOYSA-N 0.000 description 1
- CKUAXEQHGKSLHN-UHFFFAOYSA-N [C].[N] Chemical compound [C].[N] CKUAXEQHGKSLHN-UHFFFAOYSA-N 0.000 description 1
- 125000003342 alkenyl group Chemical group 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052796 boron Inorganic materials 0.000 description 1
- 239000003990 capacitor Substances 0.000 description 1
- 238000003763 carbonization Methods 0.000 description 1
- 238000005266 casting Methods 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 229910021389 graphene Inorganic materials 0.000 description 1
- 238000003760 magnetic stirring Methods 0.000 description 1
- 230000010534 mechanism of action Effects 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 235000001968 nicotinic acid Nutrition 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 238000007747 plating Methods 0.000 description 1
- 239000002861 polymer material Substances 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000010408 sweeping Methods 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 229930192474 thiophene Natural products 0.000 description 1
- JGPSMWXKRPZZRG-UHFFFAOYSA-N zinc;dinitrate;hexahydrate Chemical class O.O.O.O.O.O.[Zn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O JGPSMWXKRPZZRG-UHFFFAOYSA-N 0.000 description 1
Classifications
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
- H01B1/04—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors mainly consisting of carbon-silicon compounds, carbon or silicon
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
- H01B1/06—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors mainly consisting of other non-metallic substances
- H01B1/12—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors mainly consisting of other non-metallic substances organic substances
- H01B1/124—Intrinsically conductive polymers
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
- H01B1/06—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors mainly consisting of other non-metallic substances
- H01B1/12—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors mainly consisting of other non-metallic substances organic substances
- H01B1/124—Intrinsically conductive polymers
- H01B1/127—Intrinsically conductive polymers comprising five-membered aromatic rings in the main chain, e.g. polypyrroles, polythiophenes
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B13/00—Apparatus or processes specially adapted for manufacturing conductors or cables
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- H—ELECTRICITY
- H02—GENERATION; CONVERSION OR DISTRIBUTION OF ELECTRIC POWER
- H02N—ELECTRIC MACHINES NOT OTHERWISE PROVIDED FOR
- H02N11/00—Generators or motors not provided for elsewhere; Alleged perpetua mobilia obtained by electric or magnetic means
- H02N11/006—Motors
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- Physics & Mathematics (AREA)
- Spectroscopy & Molecular Physics (AREA)
- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Battery Electrode And Active Subsutance (AREA)
- Carbon And Carbon Compounds (AREA)
Abstract
The invention discloses the electrochemical actuators that a kind of Nitrogen-rich porous carbon is electrode, belong to electrochemical actuator technical field, electrochemical actuator of the invention includes first electrode layer, electrolyte layer and the second electrode lay three-decker；The electrolyte layer upper and lower surface adhesive electrodes layer；The electrode layer includes the Nitrogen-rich porous carbon material and conducting polymer of zeolite imidazole ester metal-organic framework, and the electrolyte layer includes ionic liquid and macromolecule matrix material.The invention also discloses the preparation methods of this electrochemical actuator, and the preparation method is simple, and the electrochemical actuator electromechanical of preparation is had excellent performance, the fields such as artificial-muscle, bionic soft robot with good application prospect.
Description
Technical field
The invention belongs to electrochemical actuator technical field, specifically a kind of Nitrogen-rich porous carbon is that the electrochemistry of electrode drives
Device and preparation method thereof.
Background technique
Electroactive polymer (Electro-active polymer, EAP) is a kind of intellectual material, has special machine
Electric conversion properties.Electroactive polymer it is most common using it first is that the exploitation of artificial-muscle in robotics.Therefore, electric
Living polymer is also commonly used as the synonym of artificial-muscle.According to the difference of the mechanism of action, electroactive polymer is broadly divided into
Electron type and ionic two major classes.Wherein, ionic electroactive polymer include ionic polymer metal composite material, it is conductive poly-
Close (the progress of Wang Lan, Zhao Shujin, Wang Haiyan, Dang Zhimin electroactive polymer such as object, polymer gel, carbon nanotube
Rare Metals Materials and engineering, 2005,34,728-733).Ionic electroactive polymer material is led to based on electrochemical principle
It crosses electrochemical machinery effect and causes macroscopic deformation caused by the migration of ion, be also generally referred to as electrochemical actuator.
Ionic polymer metal composite material (Ionic polymer metal composite, IPMC) is this kind of classical
Electrochemical actuator mainly be combined by amberplex and noble metal by chemical plating method, bio-robot,
The fields such as biomedical engineering, microfluidic control have obtained many achievements.Traditional IP MC driver because use noble metal electrode,
Expensive, rigid metal electrode cycle uses easy to crack, the more dependence water of working environment, therefore, the nonmetallic electricity of flexibility of research and development
Stablizing the driver activated in pole material and air is the significant challenge that the field is faced.Stablize actuating in air in recent years
Electrochemical actuator start to grow up (Wu Guan, Hu Ying, Chen Wei carbon nanotube and graphene artificial-muscle Science Bulletin,
2014,59,2240-2252).Its actuating performance of this driver is mainly determined by the microstructure of electrode layer and chemical property etc.
It is fixed, so electrode material and structure are particularly critical for the performance for improving electrochemical actuator.
Summary of the invention
The technical problem to be solved in the present invention is to provide electrochemical actuators and its system that a kind of Nitrogen-rich porous carbon is electrode
Preparation Method, to overcome deficiency in the prior art, the non-metal electrode of electrochemical actuator prepared by the present invention it is not only flexible but also
Have high capacitance, drive performance is excellent, flexible drive, flexible sensing and in terms of have wide answer
Use prospect.
The present invention is implemented as follows:
A kind of Nitrogen-rich porous carbon is the electrochemical actuator of electrode, which is characterized in that the electrochemical actuator is electrode layer
And the three-decker of electrolyte layer composition, the three-decker includes first electrode layer, electrolyte layer and the second electrode lay；
The electrolyte layer upper and lower surface adhesive electrodes layer；The electrode layer includes Nitrogen-rich porous carbon and conducting polymer preparation；
The Nitrogen-rich porous carbon is prepared by the pyrolysis of zeolite imidazole ester metal organic frame；The conducting polymer is poly- (3,4- second
Alkenyl dioxy thiophene)-poly- (styrene sulfonic acid), i.e. PEDOT:PSS.The present invention provides a kind of flexible non-metallic electrodes, include
The Nitrogen-rich porous carbon material and PEDOT:PSS of the ZIF structure.
Further, the electrolyte layer includes macromolecule matrix material and ionic liquid；The basis material uses
The preparation of one or more of polyurethane, Kynoar or chitosan material；The ionic liquid uses 1- ethyl-
3- methyl imidazolium tetrafluoroborate, 1- butyl -3- methyl imidazolium tetrafluoroborate or the double trifluoro methylsulphurs of 1- ethyl-3-methylimidazole
The preparation of one or more of imide salts material.
Further, described the preparation method comprises the following steps:
Step 1: preparing zeolite imidazole ester metal organic frame, i.e. ZIF by solwution method；
Step 2: obtaining the Nitrogen-rich porous carbon material of the ZIF structure by ZIF high-temperature calcination in protective atmosphere；
Divide Step 3: dispersing the Nitrogen-rich porous carbon material for the ZIF structure that step 2 obtains in be formed in PEDOT:PSS aqueous solution
Dispersion liquid, and dispersion liquid is cast to drying in mold, electrode film is made；The solid content 1.05% of PEDOT:PSS aqueous solution, i.e. water
Contain 1.05% PEDOT:PSS inside solution.
Step 4: macromolecule matrix material and ionic liquid are mixed and added into organic solvent dissolution, it is cast in mold
Drying obtains dielectric film；
Step 5: by dielectric film be placed in step 3 preparation two electrode films, i.e., first electrode layer, the second electrode lay it
Between, the electrochemical actuator is prepared with pressure sintering assembling.
Further, the solwution method prepares the step of ZIF are as follows:
1.1, by dissolving metal salts in methanol, solution A is obtained；
1.2, glyoxaline compound is dissolved in methanol, obtains B solution；
1.3, B solution that step 2 obtains in batches or is added at one time in solution A and obtains mixed system, stand 0.5 ~ 5h,
Obtain the ZIF.
Further, the ZIF is ZIF-8, ZIF-10, ZIF-11, ZIF-12, ZIF-67 etc., but not limited to this.
Further, the metal salt includes the combination of any one in zinc salt and cobalt salt or both；The zinc salt
Including any one or the two or more combinations in zinc nitrate, zinc sulfate and zinc acetate；The cobalt salt include cobalt nitrate and
In cobalt chloride any one or both combination；The glyoxaline compound include 2-methylimidazole, 2- ethyl imidazol(e) and
Any one in 3- methylimidazole or two or more combinations.
Further, the step two specifically: in nitrogen or argon gas protective atmosphere, with the liter of 1 ~ 10 °C/min
The ZIF is heated to 600 ~ 1000 °C by warm rate, and keeps the temperature 0.5 ~ 5h, is then cooled to room temperature, is obtained the ZIF structure
Nitrogen-rich porous carbon material.
Further, the mass ratio of the Nitrogen-rich porous carbon material and PEDOT:PSS in the step three is 1:20 ~ 2:1.
Further, the mass ratio of the ionic liquid in the step four and macromolecule matrix material is 1:20 ~ 5:1；Institute
The macromolecule matrix material stated includes any one or two or more combinations in polyurethane, Kynoar and chitosan；
The ionic liquid includes 1- ethyl-3-methylimidazole tetrafluoroborate, 1- butyl -3- methyl imidazolium tetrafluoroborate and 1-
Any one or two or more combinations of ethyl-3-methylimidazole bis-trifluoromethylsulfoandimide salt；The organic solvent packet
Include any one in N,N-dimethylformamide, N-Methyl pyrrolidone and methylene chloride or two or more combinations；It is described
Solution casting method film-forming heating temperature be 50 ~ 130 °C, heating time be 2 ~ 48h.
Further, the hot pressing temperature of the pressure sintering in the step five is 50 ~ 200 °C, and hot pressing time is 10min ~ 2h,
Hot pressing form is a step hot pressing or gradually hot pressing.
The beneficial effect of the present invention and the prior art is: the Nitrogen-rich porous carbon of ZIF structure provided by the invention has height
Capacitor, the synergistic effect of Nitrogen-rich porous carbon and PEDOT:PSS assigns nonmetal flexible electrode excellent chemical property, this hair
The electrochemical actuator electromechanical based on Nitrogen-rich porous carbon nonmetal flexible electrode of bright offer is had excellent performance, electrochemistry driving
The preparation method of device is simple.Therefore, which has preferable in fields such as artificial-muscle, bionic soft robots
Application prospect.
Detailed description of the invention
Fig. 1 is the work of electrochemical actuator of an exemplary embodiment of the present invention preparation based on Nitrogen-rich porous carbon electrode
Skill flow chart；
Fig. 2 is a kind of scanning electron microscope (SEM) photograph of Nitrogen-rich porous carbon material in the embodiment of the present invention；
Fig. 3 is a kind of transmission electron microscope picture of Nitrogen-rich porous carbon material in the embodiment of the present invention；
Fig. 4 is a kind of X of Nitrogen-rich porous carbon material and parent zeolite imidazate metal-organic framework material in the embodiment of the present invention
X ray diffration pattern x；
Fig. 5 is a kind of x-ray photoelectron spectroscopy figure of Nitrogen-rich porous carbon material (C1s and N1s) in the embodiment of the present invention；
Fig. 6 is the cyclic voltammetry curves that a kind of Nitrogen-rich porous carbon/foam titanium net electrode sweeps under speed in difference in the embodiment of the present invention
Figure；
Fig. 7 is a kind of Nitrogen-rich porous carbon/PEDOT:PSS composite electrode (ZIF structure Nitrogen-rich porous carbon in the embodiment of the present invention
Mass fraction of the material in flexible electrode is the cyclic voltammetry curve figure 20%) swept in difference under speed；
Fig. 8 is a kind of electrochemical actuator of Nitrogen-rich porous carbon electrode (20%C-N/PEDOT:PSS electricity in the embodiment of the present invention
Pole) electroluminescent displacement curve (3V sine voltage) at different frequencies；
Fig. 9 is electrochemical actuator (the different x%C-N/PEDOT:PSS electricity of Nitrogen-rich porous carbon electrode in the embodiment of the present invention
Pole) the electroluminescent displacement comparison of tip peak to peak (3V sine voltage) at different frequencies.
Specific embodiment
Inventor is studied for a long period of time and is largely practiced, and is able to propose technical solution of the present invention.It as follows will be to the technical side
Case, its implementation process and principle etc. are further explained.It should be understood that specific implementation described herein is only to solve
The present invention is released, is not intended to limit the present invention.
As shown in Figure 1, the stream of the preparation method for the electrochemical actuator that a kind of Nitrogen-rich porous carbon of the invention is electrode
Journey schematic diagram, it is described the preparation method comprises the following steps:
Step 1: preparing zeolite imidazole ester metal organic frame, i.e. ZIF by solwution method；
Step 2: obtaining the Nitrogen-rich porous carbon material of the ZIF structure by ZIF high-temperature calcination in protective atmosphere；
Divide Step 3: dispersing the Nitrogen-rich porous carbon material for the ZIF structure that step 2 obtains in be formed in PEDOT:PSS aqueous solution
Dispersion liquid, solid content 1.05%, and dispersion liquid is cast to drying in mold, electrode film is made；
Step 4: macromolecule matrix material and ionic liquid are mixed and added into organic solvent dissolution, it is cast in mold and dries
Obtain dielectric film；
Step 5: by dielectric film be placed in step 3 preparation two electrode films, i.e., first electrode layer, the second electrode lay it
Between, the electrochemical actuator is prepared with pressure sintering assembling.
Utilize electrochemical actuator made from above-mentioned preparation method, including first electrode layer, electrolyte layer and second electrode
Layer, total three-decker, the electrolyte layer upper and lower surface adhesive electrodes layer.The electrolyte layer upper and lower surface adhesive electrodes
Layer；The electrode layer includes Nitrogen-rich porous carbon and conducting polymer preparation；The Nitrogen-rich porous carbon is by zeolite imidazole ester metal
Organic frame pyrolysis is prepared；The conducting polymer is poly- (3,4- ethylenedioxythiophene)-poly- (styrene sulfonic acid).Institute
The electrolyte layer stated includes macromolecule matrix material and ionic liquid；The basis material uses polyurethane, Kynoar
Or one or more of chitosan material preparation；The ionic liquid uses 1- ethyl-3-methylimidazole tetrafluoro boron
One of hydrochlorate, 1- butyl -3- methyl imidazolium tetrafluoroborate or 1- ethyl-3-methylimidazole bis-trifluoromethylsulfoandimide salt
Or two or more material preparations.
It as follows will in conjunction with specific embodiments and data are further to works such as the technical solution, its implementation process and principles
It illustrates.
Embodiment 1
It disperses 2.933 grams of zinc nitrate hexahydrates in 50mL methanol, forms solution A；6.489 grams of 2-methylimidazoles are dissolved in
50mL methanol forms solution B；Under magnetic stirring, solution A is added dropwise in solution B, then stands 6h, filtration washing obtains
Zeolite imidazole ester metal-organic framework material (i.e. carbonization precursor).The material is transferred in tube furnace, nitrogen protection is led to, with
The heating rate of 5 °C/min is heated to 800 °C and keeps the temperature 2h, is cooled to room temperature, and carbonized product taking-up is placed in dilute hydrochloric acid
It impregnates 2 hours, centrifuge separation, washes 4 times, it is ethanol washing 2 times, 12 hours dry under 50 degree, it is porous to obtain ZIF structure richness nitrogen
Carbon material.
2.1 mg ZIF structure Nitrogen-rich porous carbon materials and 1.8 g PEDOT:PSS aqueous solutions (solid content 1.05%) are super
Sound dispersion mixing uniformly (mass fraction of the ZIF structure Nitrogen-rich porous carbon material in flexible electrode is 10%), then is poured dispersion liquid
It casts onto Teflon mould, vacuum oven is dried 6 hours at a temperature of 60 DEG C, obtains flexible electrode film.By 50 mg
Polyurethane and 50 mg 1- ethyl-3-methylimidazole bis-trifluoromethylsulfoandimide ionic liquids, which are uniformly mixed, forms gelling material
Above-mentioned solution is cast in Teflon mould, later by matter after 10 mL n,N-Dimethylformamide of addition are evenly dispersed
It is 12 hours dry in 60 DEG C of vacuum ovens, until solvent all volatilizees, obtain the polymer dielectric that load has ionic liquid
Layer.Polyelectrolyte floor is placed between two panels flexible electrode film, hot pressing 5min at 95 DEG C, electrochemistry driving is prepared
Device.Electrochemical actuator based on ZIF structure Nitrogen-rich porous carbon electrode prepared by an exemplary embodiment of the present invention 1 swashs
The peak to peak displacement of driver tip is 13.1 mm under the 3V voltage 0.1Hz frequency that Optical displacement sensor measures.
In addition, Fig. 2 shows the surface sweeping Electronic Speculum of the MOF structural porous carbon material of an exemplary embodiment of the present invention
Figure;Fig. 3 shows the transmission electron microscope picture of the MOF structural porous carbon material of an exemplary embodiment of the present invention;Fig. 4 is shown
A kind of X of Nitrogen-rich porous carbon material and parent zeolite imidazate metal-organic framework material in an exemplary embodiments according to the present invention
X ray diffration pattern x;Fig. 5 shows a kind of x-ray photoelectron energy of Nitrogen-rich porous carbon material in an exemplary embodiments according to the present invention
Spectrogram (C1s and N1s);Fig. 6 shows a kind of Nitrogen-rich porous carbon/foam titanium net electrode in an exemplary embodiments according to the present invention and exists
Difference sweeps the cyclic voltammetry curve figure under speed.MOF structural porous carbon material (is also regarded as a kind of carbon as seen in Figure 2
Nitrogen faceted material) present ZIF metal organic frame shape characteristic;Transmission electron microscope photo shown in Fig. 3 demonstrates above-mentioned shape
Looks structure feature;The X-ray diffractogram of Fig. 4 further demonstrates the polyhedron of parent zeolite imidazate metal-organic framework material
Structure and the carbon material structure calcined;X-ray photoelectron spectroscopy shown in Fig. 5 demonstrates carbon and nitrogen in Nitrogen-rich porous carbon material
Presence.In addition, Nitrogen-rich porous carbon/foam titanium net electrode shown in Fig. 6 is swept the cyclic voltammetry curve under speed in difference and is provided
The capacitive property of the Nitrogen-rich porous carbon material.
Embodiment 2
The preparation process of ZIF structure Nitrogen-rich porous carbon material is same as Example 1.
4.2 mg ZIF structure Nitrogen-rich porous carbon materials are uniformly mixed with 1.6 g PEDOT:PSS aqueous solution ultrasonic disperses
(mass fraction of the ZIF structure Nitrogen-rich porous carbon material in flexible electrode is 20%), then dispersion liquid is cast to polytetrafluoroethylene (PTFE)
In mold, vacuum oven is dried 6 hours at a temperature of 60 DEG C, obtains flexible electrode film.By 50 mg polyurethane and 50 mg
1- ethyl-3-methylimidazole bis-trifluoromethylsulfoandimide ionic liquid, which is uniformly mixed, forms spawn, and 10 mL are added
After n,N-Dimethylformamide is evenly dispersed, above-mentioned solution is cast in Teflon mould, it is dry in 60 DEG C of vacuum later
Dry case is 12 hours dry, until solvent all volatilizees, obtains the polyelectrolyte floor that load has ionic liquid.By electrostrictive polymer
Solution matter is placed between two panels flexible electrode film, and hot pressing 5min, is prepared electrochemical actuator at 95 DEG C.According to the present invention
Exemplary embodiment 1 prepare the electrochemical actuator based on ZIF structure Nitrogen-rich porous carbon, what laser displacement sensor measured
The peak to peak displacement of driver tip is 17.5 mm under 3V voltage 0.1Hz frequency.
Fig. 7 is Nitrogen-rich porous carbon obtained in the embodiment of the present invention 2/PEDOT:PSS composite material film electrode (ZIF knot
Structure Nitrogen-rich porous carbon material is the cyclic voltammetry curve figure 20%) swept in difference under speed in the mass fraction in fexible film electrode,
Show the membrane electrode in 1M EMIMBF4/CH3There is good chemical property under CN test system.Fig. 8 is of the invention real
Apply the electroluminescent displacement of Nitrogen-rich porous carbon electrode electro Chemical driver (20%C-N/PEDOT:PSS electrode) at different frequencies in example 2
Curve (3V sine voltage), from the figure we can see that, driver is under the working environment of sinusoidal waveform alternating voltage, electricity
Sinusoidal waveform changing rule is presented in displacement output, and waveform is good, and output displacement is stablized.With the reduction of frequency, electric actuation displacement
Increase, this is because with the reduction of frequency, since the ionic liquid zwitterion of polymeric inner has time enough migration
And assemble to electrode, the displacement of driver gradually increases.
Embodiment 3
The preparation process of ZIF structure Nitrogen-rich porous carbon material is same as Example 1.
6.3 mg ZIF structure Nitrogen-rich porous carbon materials are uniformly mixed with 1.4 g PEDOT:PSS aqueous solution ultrasonic disperses
(mass fraction of the ZIF structure Nitrogen-rich porous carbon material in flexible electrode is 30%), then dispersion liquid is cast to polytetrafluoroethylene (PTFE)
In mold, vacuum oven is dried 6 hours at a temperature of 60 DEG C, obtains flexible electrode film.By 50 mg polyurethane and 50 mg
1- ethyl-3-methylimidazole bis-trifluoromethylsulfoandimide ionic liquid, which is uniformly mixed, forms spawn, and 10 mL are added
After n,N-Dimethylformamide is evenly dispersed, above-mentioned solution is cast in Teflon mould, it is dry in 60 DEG C of vacuum later
Dry case is 12 hours dry, until solvent all volatilizees, obtains the polyelectrolyte floor that load has ionic liquid.By electrostrictive polymer
Solution matter is placed between two panels flexible electrode film, and hot pressing 5min, is prepared electrochemical actuator at 95 DEG C.According to the present invention
Exemplary embodiment 1 prepare the electrochemical actuator based on ZIF structure Nitrogen-rich porous carbon, what laser displacement sensor measured
The peak to peak displacement of driver tip is 15.1 mm under 3V voltage 0.1Hz frequency.
Embodiment 4
The preparation process of ZIF structure Nitrogen-rich porous carbon material is same as Example 1.
8.4 mg ZIF structure Nitrogen-rich porous carbon materials are uniformly mixed with 1.2 g PEDOT:PSS aqueous solution ultrasonic disperses
(mass fraction of the ZIF structure Nitrogen-rich porous carbon material in flexible electrode is 40%), then dispersion liquid is cast to polytetrafluoroethylene (PTFE)
In mold, vacuum oven is dried 6 hours at a temperature of 60 DEG C, obtains flexible electrode film.By 50 mg polyurethane and 50 mg
1- ethyl-3-methylimidazole bis-trifluoromethylsulfoandimide ionic liquid, which is uniformly mixed, forms spawn, and 10 mL are added
After n,N-Dimethylformamide is evenly dispersed, above-mentioned solution is cast in Teflon mould, it is dry in 60 DEG C of vacuum later
Dry case is 12 hours dry, until solvent all volatilizees, obtains the polyelectrolyte floor that load has ionic liquid.By electrostrictive polymer
Solution matter is placed between two panels flexible electrode film, and hot pressing 5min, is prepared electrochemical actuator at 95 DEG C.According to the present invention
Exemplary embodiment 1 prepare the electrochemical actuator based on ZIF structure Nitrogen-rich porous carbon, what laser displacement sensor measured
The peak to peak displacement of driver tip is 12.4 mm under 3V voltage 0.1Hz frequency.
Embodiment 5
The preparation process of ZIF structure Nitrogen-rich porous carbon material is same as Example 1.
10.5mg ZIF structure Nitrogen-rich porous carbon material is uniformly mixed with 1.0 g PEDOT:PSS aqueous solution ultrasonic disperses
(mass fraction of the ZIF structure Nitrogen-rich porous carbon material in flexible electrode is 50%), then dispersion liquid is cast to polytetrafluoroethylene (PTFE)
In mold, vacuum oven is dried 6 hours at a temperature of 60 DEG C, obtains flexible electrode film.By 50 mg polyurethane and 50 mg
1- ethyl-3-methylimidazole bis-trifluoromethylsulfoandimide ionic liquid, which is uniformly mixed, forms spawn, and 10 mL are added
After n,N-Dimethylformamide is evenly dispersed, above-mentioned solution is cast in Teflon mould, it is dry in 60 DEG C of vacuum later
Dry case is 12 hours dry, until solvent all volatilizees, obtains the polyelectrolyte floor that load has ionic liquid.By electrostrictive polymer
Solution matter is placed between two panels flexible electrode film, and hot pressing 5min, is prepared electrochemical actuator at 95 DEG C.According to the present invention
Exemplary embodiment 1 prepare the electrochemical actuator based on ZIF structure Nitrogen-rich porous carbon, what laser displacement sensor measured
The peak to peak displacement of driver tip is 9.5 mm under 3V voltage 0.1Hz frequency.
In addition, Fig. 9 shows under 3V sine voltage an exemplary embodiment of the present invention 1-5 under the conditions of different frequency
Electrochemical actuator comparison of the tip peaks to peak shift value.20%C-N/PEDOT:PSS is the electrochemical actuator of electrode
It can be best.
To sum up, Nitrogen-rich porous carbon material provided by the invention has MOF structure, and has preferable chemical property.
And excellent electrochemical machinery characteristic is shown based on the Nitrogen-rich porous carbon/PEDOT:PSS electrode electrochemical actuator, because
This, has huge application prospect in terms of bionics artificial thews and intelligent wearable electronic.
Based on description of the preferred embodiment of the present invention, it should be apparent that the sheet being defined by the appended claims
Invention is not limited only to the specific detail that is illustrated in specification above, without departing from present inventive concept or range to this hair
Bright many obviously change equally possible reaches the purpose of the present invention.
Claims (10)
1. the electrochemical actuator that a kind of Nitrogen-rich porous carbon is electrode, which is characterized in that the electrochemical actuator is electrode
The three-decker of layer and electrolyte layer composition, the three-decker includes first electrode layer, electrolyte layer and second electrode
Layer；The electrolyte layer upper and lower surface adhesive electrodes layer；The electrode layer includes Nitrogen-rich porous carbon and conducting polymer system
It is standby；The Nitrogen-rich porous carbon is prepared by the pyrolysis of zeolite imidazole ester metal organic frame；The conducting polymer is poly- (3,4-
Ethylenedioxythiophene)-poly- (styrene sulfonic acid), i.e. PEDOT:PSS.
2. the electrochemical actuator that a kind of Nitrogen-rich porous carbon according to claim 1 is electrode, which is characterized in that described
Electrolyte layer includes macromolecule matrix material and ionic liquid；The basis material uses polyurethane, Kynoar or shell
The preparation of one or more of glycan material；The ionic liquid using 1- ethyl-3-methylimidazole tetrafluoroborate,
One of 1- butyl -3- methyl imidazolium tetrafluoroborate or 1- ethyl-3-methylimidazole bis-trifluoromethylsulfoandimide salt or two
Kind or more material preparation.
3. a kind of Nitrogen-rich porous carbon a kind of as described in claim 1 is the preparation method of the electrochemical actuator of electrode, special
Sign is, it is described the preparation method comprises the following steps:
Step 1: preparing zeolite imidazole ester metal organic frame, i.e. ZIF by solwution method；
Step 2: obtaining the Nitrogen-rich porous carbon material of the ZIF structure by ZIF high-temperature calcination in protective atmosphere；
Divide Step 3: dispersing the Nitrogen-rich porous carbon material for the ZIF structure that step 2 obtains in be formed in PEDOT:PSS aqueous solution
Dispersion liquid, and dispersion liquid is cast to drying in mold, electrode film is made；
Step 4: macromolecule matrix material and ionic liquid are mixed and added into organic solvent dissolution, it is cast in mold and dries
Obtain dielectric film；
Step 5: by dielectric film be placed in step 3 preparation two electrode films, i.e., first electrode layer, the second electrode lay it
Between, the electrochemical actuator is prepared with pressure sintering assembling.
4. a kind of Nitrogen-rich porous carbon according to claim 3 is the preparation method of the electrochemical actuator of electrode, feature
It is, the step of solwution method prepares ZIF are as follows:
1.1, by dissolving metal salts in methanol, solution A is obtained；
1.2, glyoxaline compound is dissolved in methanol, obtains B solution；
1.3, B solution that step 2 obtains in batches or is added at one time in solution A and obtains mixed system, stand 0.5 ~ 5h,
Obtain the ZIF.
5. a kind of Nitrogen-rich porous carbon according to claim 4 is the preparation method of the electrochemical actuator of electrode, feature
It is, the ZIF includes ZIF-8, ZIF-10, ZIF-11, ZIF-12, ZIF-67.
6. a kind of Nitrogen-rich porous carbon according to claim 4 is the preparation method of the electrochemical actuator of electrode, feature
It is, metal salt includes the combination of any one in zinc salt and cobalt salt or both in the step of solwution method prepares ZIF；
The zinc salt includes any one or two or more combinations in zinc nitrate, zinc sulfate and zinc acetate；The cobalt salt packet
Include the combination of any one in cobalt nitrate and cobalt chloride or both；The glyoxaline compound includes 2-methylimidazole, 2-
Any one in ethyl imidazol(e) and 3- methylimidazole or two or more combinations.
7. a kind of Nitrogen-rich porous carbon according to claim 3 is the preparation method of the electrochemical actuator of electrode, feature
It is, the step two specifically: in nitrogen or argon gas protective atmosphere, with the heating rate of 1 ~ 10 °C/min by institute
It states ZIF and is heated to 600 ~ 1000 °C, and keep the temperature 0.5 ~ 5h, then cool to room temperature, obtain the Nitrogen-rich porous carbon of the ZIF structure
Material.
8. a kind of Nitrogen-rich porous carbon according to claim 3 is the preparation method of the electrochemical actuator of electrode, feature
It is, the mass ratio of Nitrogen-rich porous carbon material and PEDOT:PSS in the step three is 1:20 ~ 2:1.
9. a kind of Nitrogen-rich porous carbon according to claim 3 is the preparation method of the electrochemical actuator of electrode, feature
It is, the mass ratio of ionic liquid and macromolecule matrix material in the step four is 1:20 ~ 5:1；The macromolecule
Basis material includes any one or two or more combinations in polyurethane, Kynoar and chitosan；The ion
Liquid includes 1- ethyl-3-methylimidazole tetrafluoroborate, 1- butyl -3- methyl imidazolium tetrafluoroborate and 1- ethyl -3- first
Any one or two or more combinations of base imidazoles bis-trifluoromethylsulfoandimide salt；The organic solvent includes N, N- diformazan
Any one in base formamide, N-Methyl pyrrolidone and methylene chloride or two or more combinations；The solution-cast
The heating temperature of the film-forming of method is 50 ~ 130 °C, and heating time is 2 ~ 48h.
10. a kind of Nitrogen-rich porous carbon according to claim 3 is the preparation method of the electrochemical actuator of electrode, feature
It is, the hot pressing temperature of the pressure sintering in the step five is 50 ~ 200 °C, and hot pressing time is 10min ~ 2h, and hot pressing form is
One step hot pressing or gradually hot pressing.
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