CN110415857B - Electrochemical driver with nitrogen-rich porous carbon as electrode and preparation method thereof - Google Patents
Electrochemical driver with nitrogen-rich porous carbon as electrode and preparation method thereof Download PDFInfo
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- CN110415857B CN110415857B CN201910667088.5A CN201910667088A CN110415857B CN 110415857 B CN110415857 B CN 110415857B CN 201910667088 A CN201910667088 A CN 201910667088A CN 110415857 B CN110415857 B CN 110415857B
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- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 title claims abstract description 158
- 229910052757 nitrogen Inorganic materials 0.000 title claims abstract description 79
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 41
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 38
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 239000003575 carbonaceous material Substances 0.000 claims abstract description 42
- -1 zeolite imidazole ester Chemical class 0.000 claims abstract description 39
- RAXXELZNTBOGNW-UHFFFAOYSA-N imidazole Natural products C1=CNC=N1 RAXXELZNTBOGNW-UHFFFAOYSA-N 0.000 claims abstract description 28
- 239000002608 ionic liquid Substances 0.000 claims abstract description 25
- 239000003792 electrolyte Substances 0.000 claims abstract description 21
- 239000012621 metal-organic framework Substances 0.000 claims abstract description 15
- 239000011159 matrix material Substances 0.000 claims abstract description 14
- 229920000642 polymer Polymers 0.000 claims abstract description 14
- 229910021536 Zeolite Inorganic materials 0.000 claims abstract description 11
- 239000010457 zeolite Substances 0.000 claims abstract description 11
- 229920001940 conductive polymer Polymers 0.000 claims abstract description 8
- 239000013153 zeolitic imidazolate framework Substances 0.000 claims description 40
- 239000000243 solution Substances 0.000 claims description 26
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 21
- 238000007731 hot pressing Methods 0.000 claims description 20
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 18
- 238000000034 method Methods 0.000 claims description 18
- 238000001035 drying Methods 0.000 claims description 17
- 229920000144 PEDOT:PSS Polymers 0.000 claims description 14
- 238000005266 casting Methods 0.000 claims description 13
- 238000002156 mixing Methods 0.000 claims description 13
- 239000000463 material Substances 0.000 claims description 12
- 239000006185 dispersion Substances 0.000 claims description 11
- 239000007788 liquid Substances 0.000 claims description 11
- IBZJNLWLRUHZIX-UHFFFAOYSA-N 1-ethyl-3-methyl-2h-imidazole Chemical compound CCN1CN(C)C=C1 IBZJNLWLRUHZIX-UHFFFAOYSA-N 0.000 claims description 10
- 239000007864 aqueous solution Substances 0.000 claims description 10
- 229920002635 polyurethane Polymers 0.000 claims description 10
- 239000004814 polyurethane Substances 0.000 claims description 10
- 229920001609 Poly(3,4-ethylenedioxythiophene) Polymers 0.000 claims description 9
- 238000010438 heat treatment Methods 0.000 claims description 9
- 239000012528 membrane Substances 0.000 claims description 9
- 229910052751 metal Inorganic materials 0.000 claims description 6
- 239000002184 metal Substances 0.000 claims description 6
- 229920001661 Chitosan Polymers 0.000 claims description 5
- 239000002033 PVDF binder Substances 0.000 claims description 5
- 239000003960 organic solvent Substances 0.000 claims description 5
- 229920002981 polyvinylidene fluoride Polymers 0.000 claims description 5
- 230000001681 protective effect Effects 0.000 claims description 5
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 4
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 claims description 4
- 150000001868 cobalt Chemical class 0.000 claims description 4
- 150000003839 salts Chemical class 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
- LXBGSDVWAMZHDD-UHFFFAOYSA-N 2-methyl-1h-imidazole Chemical compound CC1=NC=CN1 LXBGSDVWAMZHDD-UHFFFAOYSA-N 0.000 claims description 3
- 239000004696 Poly ether ether ketone Substances 0.000 claims description 3
- 238000001354 calcination Methods 0.000 claims description 3
- 238000001816 cooling Methods 0.000 claims description 3
- 238000004090 dissolution Methods 0.000 claims description 3
- 229920000172 poly(styrenesulfonic acid) Polymers 0.000 claims description 3
- 229920002530 polyetherether ketone 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
- PQAMFDRRWURCFQ-UHFFFAOYSA-N 2-ethyl-1h-imidazole Chemical compound CCC1=NC=CN1 PQAMFDRRWURCFQ-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
- 230000002195 synergetic effect Effects 0.000 claims description 2
- 229920002554 vinyl polymer Polymers 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
- 210000003205 muscle Anatomy 0.000 abstract description 6
- 239000011664 nicotinic acid Substances 0.000 abstract description 4
- 238000006073 displacement reaction Methods 0.000 description 17
- 239000004115 Sodium Silicate Substances 0.000 description 10
- 239000005518 polymer electrolyte Substances 0.000 description 10
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 10
- 239000004810 polytetrafluoroethylene Substances 0.000 description 10
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 description 10
- 229910052911 sodium silicate Inorganic materials 0.000 description 10
- 238000001291 vacuum drying Methods 0.000 description 10
- 229920001746 electroactive polymer Polymers 0.000 description 8
- 239000000499 gel Substances 0.000 description 6
- ZXMGHDIOOHOAAE-UHFFFAOYSA-N 1,1,1-trifluoro-n-(trifluoromethylsulfonyl)methanesulfonamide Chemical compound FC(F)(F)S(=O)(=O)NS(=O)(=O)C(F)(F)F ZXMGHDIOOHOAAE-UHFFFAOYSA-N 0.000 description 5
- 238000002484 cyclic voltammetry Methods 0.000 description 5
- 239000002904 solvent Substances 0.000 description 5
- 239000000126 substance Substances 0.000 description 5
- 238000001000 micrograph Methods 0.000 description 4
- 230000008569 process Effects 0.000 description 4
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 3
- 230000005540 biological transmission Effects 0.000 description 3
- 239000006260 foam Substances 0.000 description 3
- 239000002905 metal composite material Substances 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
- 238000005406 washing Methods 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- ISRUGXGCCGIOQO-UHFFFAOYSA-N Rhoden Chemical compound CNC(=O)OC1=CC=CC=C1OC(C)C ISRUGXGCCGIOQO-UHFFFAOYSA-N 0.000 description 2
- 238000000026 X-ray photoelectron spectrum 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
- 230000007423 decrease Effects 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 239000007772 electrode material Substances 0.000 description 2
- 229920000831 ionic polymer Polymers 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 230000000877 morphologic effect Effects 0.000 description 2
- 229910000510 noble metal Inorganic materials 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- XIOUDVJTOYVRTB-UHFFFAOYSA-N 1-(1-adamantyl)-3-aminothiourea Chemical compound C1C(C2)CC3CC2CC1(NC(=S)NN)C3 XIOUDVJTOYVRTB-UHFFFAOYSA-N 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 1
- 239000002202 Polyethylene glycol Substances 0.000 description 1
- CKUAXEQHGKSLHN-UHFFFAOYSA-N [C].[N] Chemical compound [C].[N] CKUAXEQHGKSLHN-UHFFFAOYSA-N 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 150000001450 anions Chemical class 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 150000001768 cations Chemical class 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000001419 dependent effect Effects 0.000 description 1
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 description 1
- 238000007772 electroless plating Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 229910021389 graphene Inorganic materials 0.000 description 1
- JBFYUZGYRGXSFL-UHFFFAOYSA-N imidazolide Chemical compound C1=C[N-]C=N1 JBFYUZGYRGXSFL-UHFFFAOYSA-N 0.000 description 1
- 239000003014 ion exchange membrane Substances 0.000 description 1
- 238000003760 magnetic stirring Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 230000010534 mechanism of action Effects 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 230000005012 migration Effects 0.000 description 1
- 238000013508 migration Methods 0.000 description 1
- 229910052755 nonmetal Inorganic materials 0.000 description 1
- 229920001223 polyethylene glycol Polymers 0.000 description 1
- 239000002861 polymer material Substances 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 239000002520 smart material Substances 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- KKEYFWRCBNTPAC-UHFFFAOYSA-L terephthalate(2-) Chemical compound [O-]C(=O)C1=CC=C(C([O-])=O)C=C1 KKEYFWRCBNTPAC-UHFFFAOYSA-L 0.000 description 1
- 238000012360 testing method Methods 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
-
- 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)
- Carbon And Carbon Compounds (AREA)
- Battery Electrode And Active Subsutance (AREA)
Abstract
The invention discloses an electrochemical driver taking nitrogen-rich porous carbon as an electrode, belonging to the technical field of electrochemical drivers, and comprising a first electrode layer, an electrolyte layer and a second electrode layer; electrode layers are attached to the upper and lower surfaces of the electrolyte layer; the electrode layer comprises a nitrogen-rich porous carbon material with a zeolite imidazole ester metal organic framework structure and a conductive polymer, and the electrolyte layer comprises ionic liquid and a high polymer matrix material. The invention also discloses a preparation method of the electrochemical driver, which is simple, and the prepared electrochemical driver has excellent electromechanical performance and good application prospect in the fields of artificial muscles, bionic soft robots and the like.
Description
Technical Field
The invention belongs to the technical field of electrochemical drivers, and particularly relates to an electrochemical driver taking nitrogen-rich porous carbon as an electrode and a preparation method thereof.
Background
Electroactive polymers (EAP) are smart materials with special electromechanical conversion properties. One of the most common applications of electroactive polymers is the development of artificial muscles in robotics. Thus, electroactive polymers are also commonly used as terms of artificial muscles. Electroactive polymers are largely classified into two major classes, electronic and ionic, according to the mechanism of action. Among them, ionic electroactive polymers include ionic polymer metal composites, conductive polymers, polymer gels, carbon nanotubes, and the like (Wang Lan, zhao Shujin, wang Haiyan, dang Zhimin. Research into electroactive polymers progress. Rare metal materials and engineering, 2005, 34, 728-733). Ionic electroactive polymer materials are based on electrochemical principles that induce macroscopic deformation by electrochemical mechanical action, resulting in migration of ions, also commonly referred to as electrochemical actuators.
The classical electrochemical driver of ion polymer metal composite material (Ionic polymer metal composite, IPMC) is mainly formed by compounding an ion exchange membrane and noble metal by an electroless plating method, and many achievements are achieved in the fields of bionic robots, biomedical engineering, microfluidic control and the like. Because the conventional IPMC driver uses noble metal electrodes, the price is high, the rigid metal electrodes are easy to crack when being recycled, the working environment is more dependent on water, and therefore, the development of flexible nonmetallic electrode materials and drivers for stable actuation in air is an important challenge in the field. In recent years, electrochemical drivers with stable actuation in air have begun to develop (wu, hu Ying, chen Wei. Carbon nanotubes and graphene artificial muscles. Science bulletins, 2014, 59, 2240-2252). The actuation performance of such a driver is mainly determined by the microstructure, electrochemical properties, etc. of the electrode layer, so the electrode material and structure are particularly critical for improving the performance of the electrochemical driver.
Disclosure of Invention
The invention aims to solve the technical problem of providing an electrochemical driver taking nitrogen-enriched porous carbon as an electrode and a preparation method thereof, so as to overcome the defects in the prior art.
The invention is realized in the following way:
The electrochemical driver is characterized by comprising a three-layer structure consisting of an electrode layer and an electrolyte layer, wherein the three-layer structure comprises a first electrode layer, the electrolyte layer and a second electrode layer; electrode layers are attached to the upper and lower surfaces of the electrolyte layer; the electrode layer comprises nitrogen-rich porous carbon and conductive polymer; the nitrogen-rich porous carbon is prepared by pyrolysis of a zeolite imidazole ester metal organic framework; the conductive polymer is poly (3, 4-vinyl dioxythiophene) -poly (styrenesulfonic acid), namely PEDOT: PSS. The invention provides a flexible nonmetallic electrode, which comprises a nitrogen-rich porous carbon material with a ZIF structure and PEDOT: PSS.
Further, the electrolyte layer comprises a high polymer matrix material and an ionic liquid; the matrix material is prepared from one or more than two materials selected from polyurethane, polyvinylidene fluoride or chitosan; the ionic liquid is prepared from one or more than two materials of 1-ethyl-3-methylimidazole tetrafluoroborate, 1-butyl-3-methylimidazole tetrafluoroborate or 1-ethyl-3-methylimidazole bistrifluoromethanesulfonyl imide salt.
Further, the preparation method comprises the following steps:
step one, preparing a zeolite imidazole ester metal organic framework, namely ZIF, by a solution method;
calcining the ZIF at a high temperature in a protective atmosphere to obtain the nitrogen-rich porous carbon material with the ZIF structure;
Dispersing the nitrogen-rich porous carbon material with the ZIF structure obtained in the step two in PEDOT (polyether-ether-ketone) PSS aqueous solution to form dispersion liquid, casting the dispersion liquid into a mould, and drying to prepare an electrode film; PEDOT: PSS the solid content of the aqueous solution is 1.05%, i.e. the aqueous solution contains 1.05% of PEDOT: PSS.
Step four, mixing a polymer matrix material with the ionic liquid, adding an organic solvent for dissolution, casting into a mould, and drying to obtain an electrolyte membrane;
And step five, placing the electrolyte membrane between the two electrode films prepared in the step three, namely the first electrode layer and the second electrode layer, and assembling and preparing the electrochemical driver by using a hot-pressing method.
Further, the step of preparing ZIF by the solution method comprises the following steps:
1.1, dissolving metal salt in methanol to obtain solution A;
1.2, dissolving an imidazole compound in methanol to obtain a solution B;
and 1.3, adding the solution B obtained in the step two into the solution A in batches or at one time to obtain a mixed system, and standing for 0.5-5 h to obtain the ZIF.
Further, the ZIFs are, but not limited to, ZIF-8, ZIF-10, ZIF-11, ZIF-12, ZIF-67, etc.
Further, the metal salt comprises any one or combination of zinc salt and cobalt salt; the zinc salt comprises any one or the combination of more than two of zinc nitrate, zinc sulfate and zinc acetate; the cobalt salt comprises any one or the combination of cobalt nitrate and cobalt chloride; the imidazole compound comprises any one or the combination of more than two of 2-methylimidazole, 2-ethylimidazole and 3-methylimidazole.
Further, the second step specifically comprises the following steps: and heating the ZIF to 600-1000 ℃ at a heating rate of 1-10 ℃ per minute in a nitrogen or argon protective atmosphere, preserving heat for 0.5-5 h, and cooling to room temperature to obtain the nitrogen-rich porous carbon material with the ZIF structure.
Further, the mass ratio of the nitrogen-rich porous carbon material to the PEDOT to the PSS in the third step is 1:20-2:1.
Further, the mass ratio of the ionic liquid to the polymer matrix material in the fourth step is 1:20-5:1; the polymer matrix material comprises any one or the combination of more than two of polyurethane, polyvinylidene fluoride and chitosan; the ionic liquid comprises any one or more than two of 1-ethyl-3-methylimidazole tetrafluoroborate, 1-butyl-3-methylimidazole tetrafluoroborate and 1-ethyl-3-methylimidazole bistrifluoromethanesulfonyl imide salt; the organic solvent comprises any one or more than two of N, N-dimethylformamide, N-methylpyrrolidone and methylene dichloride; the heating temperature of the solidified film formed by the solution casting method is 50-130 ℃, and the heating time is 2-48 h.
Further, the hot pressing temperature of the hot pressing method in the step five is 50-200 ℃, the hot pressing time is 10 min-2 h, and the hot pressing mode is one-step hot pressing or step-by-step hot pressing.
The beneficial effects of the invention compared with the prior art are as follows: the nitrogen-rich porous carbon with the ZIF structure provided by the invention has high capacitance, and the synergistic effect of the nitrogen-rich porous carbon and PEDOT: PSS endows the nonmetal flexible electrode with excellent electrochemical performance. Therefore, the electrochemical driver has better application prospect in the fields of artificial muscles, bionic soft robots and the like.
Drawings
FIG. 1 is a process flow diagram for preparing an electrochemical driver based on a nitrogen-enriched porous carbon electrode in accordance with an exemplary embodiment of the present invention;
FIG. 2 is a scanning electron microscope image of a nitrogen-enriched porous carbon material in an embodiment of the invention;
FIG. 3 is a transmission electron microscope image of a nitrogen-rich porous carbon material according to an embodiment of the present invention;
FIG. 4 is an X-ray diffraction pattern of a nitrogen-enriched porous carbon material and a parent zeolite imidazolate metal organic framework material in accordance with an embodiment of the invention;
FIG. 5 is an X-ray photoelectron spectrum (C1 s and N1 s) of a nitrogen-enriched porous carbon material according to an embodiment of the present invention;
FIG. 6 is a graph of cyclic voltammograms of a nitrogen-enriched porous carbon/titanium foam mesh electrode at different sweep rates in an embodiment of the present invention;
FIG. 7 is a cyclic voltammogram of a nitrogen-rich porous carbon/PEDOT: PSS composite electrode (ZIF structured nitrogen-rich porous carbon material 20% by mass in a flexible electrode) at different sweep rates in an embodiment of the present invention;
FIG. 8 is an electrodisplacive curve (3V sine wave voltage) of an electrochemical driver (20% C-N/PEDOT: PSS electrode) of a nitrogen-enriched porous carbon electrode at different frequencies according to an embodiment of the present invention;
FIG. 9 is a plot of peak-to-peak electro-displacement contrast (3V sine wave voltage) of the electrochemical drivers of the nitrogen-enriched porous carbon electrode (different x% C-N/PEDOT: PSS electrode) at different frequencies in an example of the present invention.
Detailed Description
The inventor has long studied and practiced in a large number, so as to put forward the technical scheme of the invention. The technical scheme, the implementation process, the principle and the like are further explained as follows. It should be noted that the detailed description herein is for purposes of illustration only and is not intended to limit the invention.
As shown in fig. 1, the process of the preparation method of the electrochemical driver with the nitrogen-enriched porous carbon as the electrode according to the present invention is shown in the schematic drawing, wherein the preparation method comprises:
step one, preparing a zeolite imidazole ester metal organic framework, namely ZIF, by a solution method;
calcining the ZIF at a high temperature in a protective atmosphere to obtain the nitrogen-rich porous carbon material with the ZIF structure;
Dispersing the nitrogen-rich porous carbon material with the ZIF structure obtained in the step two in PEDOT (polyether-ether-ketone) PSS (sodium silicate) aqueous solution to form dispersion liquid with the solid content of 1.05%, and casting the dispersion liquid into a mould and drying to prepare an electrode film;
step four, mixing a polymer matrix material with the ionic liquid, adding an organic solvent for dissolution, casting into a mould, and drying to obtain an electrolyte membrane;
And step five, placing the electrolyte membrane between the two electrode films prepared in the step three, namely the first electrode layer and the second electrode layer, and assembling and preparing the electrochemical driver by using a hot-pressing method.
The electrochemical driver manufactured by the manufacturing method comprises a first electrode layer, an electrolyte layer and a second electrode layer, wherein the three layers are in a three-layer structure, and the electrode layers are attached to the upper surface and the lower surface of the electrolyte layer. Electrode layers are attached to the upper and lower surfaces of the electrolyte layer; the electrode layer comprises nitrogen-rich porous carbon and conductive polymer; the nitrogen-rich porous carbon is prepared by pyrolysis of a zeolite imidazole ester metal organic framework; the conductive polymer is poly (3, 4-vinyldioxythiophene) -poly (styrenesulfonic acid). The electrolyte layer comprises a high polymer matrix material and an ionic liquid; the matrix material is prepared from one or more than two materials selected from polyurethane, polyvinylidene fluoride or chitosan; the ionic liquid is prepared from one or more than two materials of 1-ethyl-3-methylimidazole tetrafluoroborate, 1-butyl-3-methylimidazole tetrafluoroborate or 1-ethyl-3-methylimidazole bistrifluoromethanesulfonyl imide salt.
The technical scheme, implementation process and principle and the like will be further explained with reference to specific embodiments and data.
Example 1
2.933 Grams of zinc nitrate hexahydrate was dispersed in 50mL of methanol to form solution a; 6.489 g of 2-methylimidazole was dissolved in 50mL of methanol to form solution B; under the magnetic stirring, the solution B is added into the solution A dropwise, then the solution A is kept stand for 6 hours, and the zeolite imidazole ester metal organic framework material (namely carbonized precursor) is obtained through filtration and washing. Transferring the material into a tube furnace, introducing nitrogen for protection, heating to 800 ℃ at a temperature rising rate of 5 ℃ per min, preserving heat for 2 hours, cooling to room temperature, taking out a carbonized product, soaking in dilute hydrochloric acid for 2 hours, centrifugally separating, washing with water for 4 times, washing with ethanol for 2 times, and drying at 50 ℃ for 12 hours to obtain the ZIF structure nitrogen-rich porous carbon material.
Uniformly dispersing and mixing 2.1 mg ZIF-structure nitrogen-rich porous carbon material with 1.8 g PEDOT (polyethylene glycol terephthalate)/PSS (sodium silicate) aqueous solution (solid content is 1.05%) in an ultrasonic manner (the mass fraction of the ZIF-structure nitrogen-rich porous carbon material in the flexible electrode is 10%), casting the dispersion liquid into a polytetrafluoroethylene mould, and drying in a vacuum drying oven at 60 ℃ for 6 hours to obtain the flexible electrode film. Uniformly mixing 50 mg polyurethane and 50 mg 1-ethyl-3-methylimidazole bis (trifluoromethanesulfonyl) imide ionic liquid to form a gel substance, adding 10mL of N, N-dimethylformamide to uniformly disperse, pouring the solution into a polytetrafluoroethylene mould, and drying in a vacuum drying oven at 60 ℃ for 12 hours until the solvent is completely volatilized, thereby obtaining the polymer electrolyte layer loaded with the ionic liquid. And placing the polymer electrolyte layer between two flexible electrode films, and hot-pressing for 5min at 95 ℃ to prepare the electrochemical driver. An electrochemical driver based on a ZIF structured nitrogen-rich porous carbon electrode prepared according to example 1 of the present invention had a peak-to-peak displacement of the driver tip of 13.1 mm at a 3V voltage of 0.1Hz frequency, as measured by a laser displacement sensor.
In addition, fig. 2 shows a scanning electron microscope image of a porous carbon material of a MOF structure according to an exemplary embodiment of the present invention, fig. 3 shows a transmission electron microscope image of a porous carbon material of a MOF structure according to an exemplary embodiment of the present invention, fig. 4 shows an X-ray diffraction pattern of an organic frame material of a nitrogen-rich porous carbon material and a parent zeolite imidazole ester metal according to an exemplary embodiment of the present invention, fig. 5 shows X-ray photoelectron energy spectra (C1 s and N1 s) of an nitrogen-rich porous carbon material according to an exemplary embodiment of the present invention, and fig. 6 shows cyclic voltammograms of an electrode of a nitrogen-rich porous carbon/titanium foam net according to an exemplary embodiment of the present invention at different scanning speeds. The porous carbon material with MOF structure (also can be considered as a carbon nitrogen polyhedral material) can be seen from FIG. 2 to show the morphological characteristics of the ZIF metal organic framework, the transmission electron microscope photo shown in FIG. 3 shows the morphological characteristics, the X-ray diffraction diagram of FIG. 4 further shows the polyhedral structure of the parent zeolite imidazole ester metal organic framework material and the calcined carbon material structure, and the X-ray photoelectron spectrum shown in FIG. 5 shows the existence of carbon and nitrogen in the nitrogen-rich porous carbon material. In addition, the cyclic voltammogram of the nitrogen-enriched porous carbon/titanium foam mesh electrode shown in fig. 6 at different sweep rates provides the capacitive performance of the nitrogen-enriched porous carbon material.
Example 2
The preparation process of the ZIF structured nitrogen-rich porous carbon material is the same as in example 1.
Uniformly dispersing and mixing 4.2 mg ZIF-structure nitrogen-rich porous carbon material with 1.6 g PEDOT/PSS aqueous solution in an ultrasonic manner (the mass fraction of the ZIF-structure nitrogen-rich porous carbon material in the flexible electrode is 20%), casting the dispersion liquid into a polytetrafluoroethylene mould, and drying in a vacuum drying oven at the temperature of 60 ℃ for 6 hours to obtain the flexible electrode film. Uniformly mixing 50mg polyurethane and 50mg 1-ethyl-3-methylimidazole bis (trifluoromethanesulfonyl) imide ionic liquid to form a gel substance, adding 10 mL of N, N-dimethylformamide to uniformly disperse, pouring the solution into a polytetrafluoroethylene mould, and drying in a vacuum drying oven at 60 ℃ for 12 hours until the solvent is completely volatilized, thereby obtaining the polymer electrolyte layer loaded with the ionic liquid. And placing the polymer electrolyte layer between two flexible electrode films, and hot-pressing for 5min at 95 ℃ to prepare the electrochemical driver. An electrochemical driver based on a nitrogen-rich porous carbon of ZIF structure prepared according to example 1 of the present invention had a peak-to-peak displacement of the driver tip of 17.5 mm at a 3V voltage of 0.1Hz frequency, as measured by a laser displacement sensor.
FIG. 7 is a cyclic voltammogram of the nitrogen-rich porous carbon/PEDOT: PSS composite material membrane electrode (the mass fraction of the ZIF-structured nitrogen-rich porous carbon material in the flexible membrane electrode is 20%) obtained in the embodiment 2 of the invention at different sweep rates, which shows that the membrane electrode has good electrochemical performance under a 1M EMIMBF 4/CH3 CN test system. FIG. 8 shows the electro-displacement curve (3V sine wave voltage) of the electrochemical driver (20% C-N/PEDOT: PSS electrode) with nitrogen-enriched porous carbon electrode in the embodiment 2 of the invention under different frequencies, and it can be seen from the figure that the electro-displacement output shows a sine waveform change rule, a good waveform and stable output displacement under the working environment of sine waveform alternating voltage. As the frequency decreases, the electrical actuation displacement increases, since as the frequency decreases, the displacement of the driver gradually increases as the ionic liquid anions and cations within the polymer have sufficient time to migrate and accumulate toward the electrode.
Example 3
The preparation process of the ZIF structured nitrogen-rich porous carbon material is the same as in example 1.
Uniformly dispersing and mixing 6.3 mg ZIF-structure nitrogen-rich porous carbon material with 1.4 g PEDOT/PSS aqueous solution in an ultrasonic manner (the mass fraction of the ZIF-structure nitrogen-rich porous carbon material in the flexible electrode is 30%), casting the dispersion liquid into a polytetrafluoroethylene mould, and drying in a vacuum drying oven at the temperature of 60 ℃ for 6 hours to obtain the flexible electrode film. Uniformly mixing 50mg polyurethane and 50mg 1-ethyl-3-methylimidazole bis (trifluoromethanesulfonyl) imide ionic liquid to form a gel substance, adding 10 mL of N, N-dimethylformamide to uniformly disperse, pouring the solution into a polytetrafluoroethylene mould, and drying in a vacuum drying oven at 60 ℃ for 12 hours until the solvent is completely volatilized, thereby obtaining the polymer electrolyte layer loaded with the ionic liquid. And placing the polymer electrolyte layer between two flexible electrode films, and hot-pressing for 5min at 95 ℃ to prepare the electrochemical driver. An electrochemical driver based on a nitrogen-rich porous carbon of ZIF structure prepared according to example 1 of the present invention had a peak-to-peak displacement of the driver tip of 15.1 mm at a 3V voltage of 0.1Hz frequency, as measured by a laser displacement sensor.
Example 4
The preparation process of the ZIF structured nitrogen-rich porous carbon material is the same as in example 1.
Uniformly dispersing and mixing 8.4 mg ZIF-structure nitrogen-rich porous carbon material with 1.2 g PEDOT/PSS aqueous solution in an ultrasonic manner (the mass fraction of the ZIF-structure nitrogen-rich porous carbon material in the flexible electrode is 40%), casting the dispersion liquid into a polytetrafluoroethylene mould, and drying in a vacuum drying oven at the temperature of 60 ℃ for 6 hours to obtain the flexible electrode film. Uniformly mixing 50mg polyurethane and 50mg 1-ethyl-3-methylimidazole bis (trifluoromethanesulfonyl) imide ionic liquid to form a gel substance, adding 10 mL of N, N-dimethylformamide to uniformly disperse, pouring the solution into a polytetrafluoroethylene mould, and drying in a vacuum drying oven at 60 ℃ for 12 hours until the solvent is completely volatilized, thereby obtaining the polymer electrolyte layer loaded with the ionic liquid. And placing the polymer electrolyte layer between two flexible electrode films, and hot-pressing for 5min at 95 ℃ to prepare the electrochemical driver. An electrochemical driver based on a nitrogen-rich porous carbon of ZIF structure prepared according to example 1 of the present invention had a peak-to-peak displacement of the driver tip of 12.4 mm at a 3V voltage of 0.1Hz frequency, as measured by a laser displacement sensor.
Example 5
The preparation process of the ZIF structured nitrogen-rich porous carbon material is the same as in example 1.
Uniformly dispersing and mixing 10.5mg of the ZIF structure nitrogen-rich porous carbon material with 1.0 g of PEDOT/PSS aqueous solution in an ultrasonic manner (the mass fraction of the ZIF structure nitrogen-rich porous carbon material in the flexible electrode is 50%), casting the dispersion liquid into a polytetrafluoroethylene mould, and drying in a vacuum drying oven at the temperature of 60 ℃ for 6 hours to obtain the flexible electrode film. Uniformly mixing 50mg polyurethane and 50mg 1-ethyl-3-methylimidazole bis (trifluoromethanesulfonyl) imide ionic liquid to form a gel substance, adding 10 mL of N, N-dimethylformamide to uniformly disperse, pouring the solution into a polytetrafluoroethylene mould, and drying in a vacuum drying oven at 60 ℃ for 12 hours until the solvent is completely volatilized, thereby obtaining the polymer electrolyte layer loaded with the ionic liquid. And placing the polymer electrolyte layer between two flexible electrode films, and hot-pressing for 5min at 95 ℃ to prepare the electrochemical driver. An electrochemical driver based on a nitrogen-rich porous carbon of ZIF structure prepared according to example 1 of the present invention had a peak-to-peak displacement of the driver tip of 9.5 mm at a 3V voltage of 0.1Hz frequency, as measured by a laser displacement sensor.
In addition, fig. 9 shows a comparison of peak-to-peak displacement values for the electrochemical drivers according to exemplary embodiments 1-5 of the present invention at different frequencies for a 3V sine wave voltage. 20% C-N/PEDOT PSS is the best electrochemical driver for the electrode.
In conclusion, the nitrogen-rich porous carbon material provided by the invention has a MOF structure and has better electrochemical performance. The electrochemical driver based on the nitrogen-rich porous carbon/PEDOT: PSS electrode shows excellent electrochemical mechanical characteristics, so that the electrochemical driver has a huge application prospect in the aspects of bionic artificial muscles and intelligent wearable electronic equipment.
Based on the description of the preferred embodiments of the present invention, it should be clear that the invention defined by the appended claims is not limited to the specific details set forth in the above description, but that many apparent variations of the invention are possible without departing from the spirit or scope thereof.
Claims (7)
1. The electrochemical driver is characterized by comprising a three-layer structure consisting of an electrode layer and an electrolyte layer, wherein the three-layer structure comprises a first electrode layer, the electrolyte layer and a second electrode layer; electrode layers are attached to the upper and lower surfaces of the electrolyte layer; the electrode layer comprises nitrogen-rich porous carbon and conductive polymer; the nitrogen-rich porous carbon is prepared by pyrolysis of a zeolite imidazole ester metal organic framework; the conductive polymer is poly (3, 4-vinyl dioxythiophene) -poly (styrenesulfonic acid), namely PEDOT: PSS;
the preparation method of the electrochemical driver taking the nitrogen-rich porous carbon as the electrode comprises the following steps:
step one, preparing a zeolite imidazole ester metal organic framework, namely ZIF, by a solution method;
Calcining the ZIF at a high temperature in a protective atmosphere to obtain the nitrogen-rich porous carbon material with the ZIF structure; the second step is specifically as follows: heating the ZIF to 600-1000 ℃ at a heating rate of 1-10 ℃ per minute in a nitrogen or argon protective atmosphere, preserving heat for 0.5-5 h, and then cooling to room temperature to obtain the nitrogen-rich porous carbon material with the ZIF structure;
dispersing the nitrogen-rich porous carbon material with the ZIF structure obtained in the step two in PEDOT (polyether-ether-ketone) PSS aqueous solution to form dispersion liquid, casting the dispersion liquid into a mould, and drying to prepare an electrode film;
step four, mixing a polymer matrix material with the ionic liquid, adding an organic solvent for dissolution, casting into a mould, and drying to obtain an electrolyte membrane;
step five, placing the electrolyte membrane between the two electrode films prepared in the step three, namely a first electrode layer and a second electrode layer, and assembling and preparing the electrochemical driver by a hot-pressing method;
The ZIF preparation method by the solution method comprises the following steps:
1.1, dissolving metal salt in methanol to obtain solution A;
1.2, dissolving an imidazole compound in methanol to obtain a solution B;
1.3, adding the solution B obtained in the step two into the solution A in batches or at one time to obtain a mixed system, and standing for 0.5-5 h to obtain the ZIF;
the nitrogen-rich porous carbon with the ZIF structure has high capacitance, and the synergistic effect of the nitrogen-rich porous carbon and PEDOT: PSS endows the nonmetallic flexible electrode with excellent electrochemical performance.
2. The electrochemical actuator using nitrogen-enriched porous carbon as an electrode according to claim 1, wherein the electrolyte layer comprises a polymer matrix material and an ionic liquid; the matrix material is prepared from one or more than two materials selected from polyurethane, polyvinylidene fluoride or chitosan; the ionic liquid is prepared from one or more than two materials of 1-ethyl-3-methylimidazole tetrafluoroborate, 1-butyl-3-methylimidazole tetrafluoroborate or 1-ethyl-3-methylimidazole bistrifluoromethanesulfonyl imide salt.
3. The electrochemical driver of claim 1, wherein the ZIF comprises ZIF-8, ZIF-10, ZIF-11, ZIF-12, ZIF-67.
4. The electrochemical driver with the nitrogen-enriched porous carbon as an electrode according to claim 1, wherein the metal salt in the step of preparing the ZIF by the solution method comprises any one or a combination of zinc salt and cobalt salt; the zinc salt comprises any one or the combination of more than two of zinc nitrate, zinc sulfate and zinc acetate; the cobalt salt comprises any one or the combination of cobalt nitrate and cobalt chloride; the imidazole compound comprises any one or the combination of more than two of 2-methylimidazole, 2-ethylimidazole and 3-methylimidazole.
5. The electrochemical driver with the nitrogen-rich porous carbon as an electrode according to claim 1, wherein the mass ratio of the nitrogen-rich porous carbon material to PEDOT: PSS in the third step is 1:20-2:1.
6. The electrochemical driver with the nitrogen-enriched porous carbon as an electrode according to claim 1, wherein the mass ratio of the ionic liquid to the polymer matrix material in the fourth step is 1:20-5:1; the polymer matrix material comprises any one or the combination of more than two of polyurethane, polyvinylidene fluoride and chitosan; the ionic liquid comprises any one or more than two of 1-ethyl-3-methylimidazole tetrafluoroborate, 1-butyl-3-methylimidazole tetrafluoroborate and 1-ethyl-3-methylimidazole bistrifluoromethanesulfonyl imide salt; the organic solvent comprises any one or more than two of N, N-dimethylformamide, N-methylpyrrolidone and methylene dichloride; the heating temperature of the solidified film formed by the solution casting method is 50-130 ℃, and the heating time is 2-48 h.
7. The electrochemical driver with the nitrogen-rich porous carbon as an electrode according to claim 1, wherein the hot pressing temperature of the hot pressing method in the fifth step is 50-200 ℃, the hot pressing time is 10 min-2 h, and the hot pressing mode is one-step hot pressing or step-by-step hot pressing.
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