CN110648853A - Self-supporting electrode material with sandwich structure and preparation method thereof - Google Patents
Self-supporting electrode material with sandwich structure and preparation method thereof Download PDFInfo
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- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
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- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
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- H—ELECTRICITY
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- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
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- H—ELECTRICITY
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- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
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- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
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Abstract
The invention relates to a sandwich structure self-supporting electrode material and a preparation method thereof. The electrode material is a porous graphene polymer carbon nanomaterial/heteroatom-doped polymer carbon nanomaterial/porous graphene polymer carbon nanomaterial with a sandwich structure. The method comprises the following steps: preparing graphene/polymer fibers, preparing heteroatom/polymer fibers, preparing sandwich self-supporting nano fibers and preparing a sandwich structure self-supporting electrode material. The electrode material has better electrochemical performance. The method has simple process, can be used for mass production, can be used as a power source of a wearable electronic device, and has great application potential.
Description
Technical Field
The invention belongs to the field of electrode materials of supercapacitors and preparation thereof, and particularly relates to a self-supporting electrode material with a sandwich structure and a preparation method thereof.
Background
A supercapacitor is an energy storage element that can provide a higher power density than a battery. At present, the electrode material of the super capacitor is mainly a carbon-based material with a large specific surface area, and comprises activated carbon, activated carbon fibers, carbon nanotubes and the like. In recent years, heteroatom-doped carbon materials have shown excellent electrochemical properties. Wherein heteroatom doping such as phosphorus, nitrogen, boron and the like shows very excellent electrochemical performance, Yang et al researches the capacitance characteristic of boron-doped acrylonitrile-based carbon nanofibers and finds that boron doping can improve the specific capacitance of the polyacrylonitrile-based carbon fibers by 2 times and increase the specific capacitance from 60F/g to 180F/g, which is attributed to the synergistic effect of element doping (enhanced electrical capacitance of pore carbon fibers derived from polyacrylonitrile and boron trioxide [ J ]. Electrochim. acta,2013,88: 597-; yandao et al studied a phosphorus-doped polyacrylonitrile carbon nanofiber electrode material, with a mass specific capacitance of 224F/g at a current density of 0.5A/g when a nitrogen-phosphorus-doped carbon nanofiber with a phosphorus content of 9 wt% exhibited the best capacitance characteristics (Yandao. phosphorus-doped polyacrylonitrile carbon material preparation and its use in supercapacitors [ D ]. Beijing university of chemical industry, 2014). Besides, heteroatom doping has other advantages, and dawneastern et al research on phosphorus doped polyacrylonitrile carbon nanofiber electrode materials, such as high specific capacity, excellent cycling stability, wide electrochemical window and the like, and can improve the energy density of a capacitor.
Polyacrylonitrile is an excellent electrostatic spinning raw material, the polyacrylonitrile process is simple, the obtained nano-fibers have uniform diameters, and the fibers can still maintain fiber shapes after being pre-oxidized and carbonized at high temperature, so that the polyacrylonitrile has wide attention in the field of super capacitors. In 2011, Yang et al prepared porous polyacrylonitrile carbon fibers using tetraethyl orthosilicate as a pore forming agent, and the specific capacitance of which reached 160F/g (Thin, bound electrolytes regulating of porous carbon fiber a. the specific capacitance for porous cellulose acetate copolymer [ J ]. Electrochem. Commun,2011,13:1042 1046). In 2013, Kalra and the like adopt defluorinated sulfonic acid as a pore-making agent and polyacrylonitrile as a carbon source to prepare the porous carbon nanofiber. When the mass ratio of the perfluorosulfonic acid to the polyacrylonitrile is 60: at 40, the specific capacitance is up to 270F/g at a charge/discharge current density of 1A/g (noise of carbon nanoparticles with adjustable pores as electrodes for supercapacitors [ J ]. J.Power Sources,2013,235: 289). Graphene has the characteristics of large specific surface area, high tensile strength, excellent electric and heat conducting properties and the like, and in 2013, the specific capacitance of the carbon nanofiber modified by Graphene prepared by using a mixed solution of polyacrylonitrile and Graphene by Zhou and the like is up to 264F/g and is higher than that of a pure carbon nanofiber (150F/g) under the charge-discharge current density of 0.1A/g, which is attributed to the high specific surface area and high conductivity of Graphene (Graphene-reinforced carbon nanofibers for use in surfactant fibers: synthetic and chemical [ J ]. J.Power Sources,2013,222: 410-. The method has great potential in the fields of electronic elements, nano composite materials, sensors, super capacitors and the like. And (3) blending polyacrylonitrile and polyvinylidene fluoride, and carbonizing at high temperature to obtain the carbon nanofiber with a porous structure, so that the performance of the capacitor is improved. The graphene is added into the polyacrylonitrile and polyvinylidene fluoride spinning solution, and the strength, softness and conductivity of the carbon nanofiber can be improved after high-temperature carbonization, so that the electrode material of the supercapacitor can be prepared by adding a conductive polymer and an adhesive without grinding.
Disclosure of Invention
The invention aims to solve the technical problem of providing a sandwich-structure self-supporting electrode material and a preparation method thereof so as to fill the blank in the prior art.
The invention provides a self-supporting electrode material with a sandwich structure, which is a porous graphene polymer carbon nano material/heteroatom-doped polymer carbon nano material/porous graphene polymer carbon nano material with a sandwich structure.
The polymer comprises one or more of Polyacrylonitrile (PAN), polyvinylidene fluoride (PVDF), polyvinylpyrrolidone (PVP) and polyvinyl alcohol (PVA).
The heteroatom comprises one or more of nitrogen, phosphorus, sulfur and silicon.
The invention also provides a preparation method of the sandwich structure self-supporting electrode material, which comprises the following steps:
(1) dissolving a polymer and graphene in a solvent at a mass ratio of 90: 10-99: 1 to obtain a graphene/polymer spinning solution, then performing electrostatic spinning to obtain graphene/polymer fibers,
(2) dissolving a polymer and a substance containing a heteroatom into a solvent according to a mass ratio of 100-70:0-30 to obtain a heteroatom/polymer spinning solution, and then carrying out electrostatic spinning to obtain a heteroatom/polymer fiber, wherein the mass of the substance containing the heteroatom is not 0;
(3) respectively attaching the upper surface and the lower surface of the heteroatom/polymer fiber in the step (2) to the graphene/polymer fiber in the step (1) to obtain the sandwich self-supporting nanofiber;
(4) and (4) pre-oxidizing and crosslinking the sandwich self-supporting nanofiber obtained in the step (3), and then carbonizing the sandwich self-supporting nanofiber in an inert atmosphere to obtain a porous graphene polymer carbon nanomaterial/heteroatom-doped polymer carbon nanomaterial/porous graphene polymer carbon nanomaterial, namely the sandwich structure self-supporting electrode material.
The total mass concentration of the polymer and the graphene in the solvent in the step (1) is 5-15% wt.
The polymer in the steps (1) and (2) comprises one or more of Polyacrylonitrile (PAN), polyvinylidene fluoride (PVDF), polyvinylpyrrolidone (PVP) and polyvinyl alcohol (PVA).
The polymer comprises one or two of Polyacrylonitrile (PAN), polyvinylidene fluoride (PVDF), polyvinylpyrrolidone (PVP) and polyvinyl alcohol (PVA), and the mixture ratio is (100-50): (0-50).
The solvent in the steps (1) and (2) comprises one or more of dimethylformamide, DMAc and acetone.
The electrostatic spinning process parameters in the steps (1) and (2) are as follows: the positive pressure is 15-20kV, the negative pressure is-2 kV, the receiving distance is 10-25cm, the flow rate of the spinning solution is 0.5-1.0ml/h, the humidity is 40-80%, and the spinning time is 1-20 hours.
The total mass concentration of the polymer and the substance containing the heteroatom in the solvent in the step (2) is 10-15 wt%.
The heteroatom-containing substance in the step (2) comprises phosphoric acid.
The technological parameters of the pre-oxidation crosslinking in the step (4) are as follows: heating to 200-300 deg.C at a rate of 2-5 deg.C/min, maintaining for 60-150min, and cooling to room temperature at a rate of 4-10 deg.C/min.
The carbonization process parameters in the step (4) are as follows: heating to 600-1000 ℃ at a heating rate of 2-8 ℃/min under an inert atmosphere, preserving heat for 60-240min, and then cooling to room temperature at a cooling rate of 4-10 ℃/min, wherein the inert atmosphere is high-purity nitrogen with the purity of more than or equal to 99.999%.
The invention also provides an application of the self-supporting electrode material with the sandwich structure in the super capacitor.
According to the invention, the heteroatom doping is realized by inserting the heteroatom polymer carbon nanofiber into the porous polymer carbon nanofiber, so that the electrochemical performance of the supercapacitor is improved, and meanwhile, the graphene is added to increase the conductivity and strength of the electrode material, so that the method is simple to operate, the used medicines and equipment are low in cost, and the industrial production is easy to realize; the electrode material of the supercapacitor does not need to be prepared by grinding or adding a binder.
Advantageous effects
(1) The medicine and equipment used in the invention have low cost, simple operation and easy realization of industrial production;
(2) according to the invention, the nanofiber precursor polymer with good spinnability is selected as a raw material, and heteroatom doping is realized by utilizing a sandwich structure, so that the electrochemical performance of the supercapacitor is improved.
(3) The electrode material prepared by the invention does not need to be ground and added with a conductive polymer to prepare the electrode material.
(4) The invention has short production period, and the appearance, the diameter, the quality of heteroatoms and the orderliness of fibers of the electrode material can be regulated and controlled by effective means; can be used as a power source of wearable electronic devices and has huge application potential.
Detailed Description
The invention will be further illustrated with reference to the following specific examples. It should be understood that these examples are for illustrative purposes only and are not intended to limit the scope of the present invention. Further, it should be understood that various changes or modifications of the present invention may be made by those skilled in the art after reading the teaching of the present invention, and such equivalents may fall within the scope of the present invention as defined in the appended claims.
The invention uses various chemicals which are commercially available and have no special purity requirement.
Example 1
(1) Adding PAN and PVDF into DMF (the mass ratio of the total mass of PAN and PVDF to DMF is 1: 9) according to the mass ratio of 80:20, adding 2 wt% (based on the total mass of PAN and PVDF) of graphene, placing the mixture on an ultrasonic oscillator to vibrate for 60 minutes, and finally placing the mixture on a magnetic stirrer to stir for 10 hours to prepare the PAN/PVDF graphene electrostatic spinning precursor solution.
(2) PAN and phosphoric acid were mixed as 80: dissolving 20 mass percent of the mixture in DMF (the mass ratio of the total mass of the PAN and the PVDF to the DMF is 1: 9), and placing the mixture on an ultrasonic oscillator to oscillate for 60 minutes to prepare PAN and phosphoric acid electrostatic spinning precursor solution.
(3) Putting the PAN/PVDF graphene electrostatic spinning precursor solution obtained in the step (1) into a 20ml injector, spinning for 10 hours, wherein the spinning parameters are as follows: positive pressure is 20kV, and negative pressure is-2 kV; the spinning receiving distance is 18 cm; the flow rate of the spinning solution is 0.5 ml/h; spinning humidity is 40%, and PAN/PVDF/graphene fibers are obtained.
(4) And (3) putting the PAN and phosphoric acid electrostatic spinning precursor solution obtained in the step (2) into a 20ml injector, and spinning for 3 hours to obtain the phosphorus/PAN fiber, wherein the spinning parameters are the same as those in the step (3).
(5) And (3) respectively attaching the upper surface and the lower surface of the phosphorus/PAN fiber in the step (4) to the PAN/PVDF/graphene fiber in the step (3) to obtain the sandwich self-supporting nanofiber.
(6) Placing the sandwich self-supporting nano-fiber in the step (5) into a tubular furnace for pre-oxidation under the pre-oxidation conditionComprises the following steps: heating to 280 ℃ at the heating rate of 3 ℃/min, preserving the heat for 120min, and then cooling to room temperature at the speed of 5 ℃/min. The preoxidized sandwich-type nano-fiber is calcined at high temperature under the protection of inert (high-purity nitrogen with the purity of more than or equal to 99.999%) atmosphere, and the calcining conditions are as follows: heating to 800 ℃ at the heating rate of 3 ℃/min, preserving the heat for 120min, and then cooling to room temperature at the cooling rate of 5 ℃/min to obtain the carbon nanofiber, thereby obtaining the electrode material of the super capacitor. In this example, the prepared supercapacitor electrode material was used as a working electrode, a platinum electrode was used as a counter electrode, and a saturated silver/AgCl electrode was used as a reference electrode in a three-electrode test system (shanghai chenhua instruments co., ltd CHI 660E). The electrolytic liquid system is 1M H2SO4When the current density was 1A/g, the specific capacitance was measured to be 139F/g.
Example 2
(1) PAN and PVDF are added into acetone according to the mass ratio of 80:20 (the mass ratio of the total mass of PAN and PVDF to the mass of acetone is 1: 9), 5 wt% (based on the total mass of PAN and PVDF) of graphene is added, and the rest is the same as that of example 1, so that PAN/PVDF graphene electrostatic spinning precursor solution is prepared.
(2) PAN and phosphoric acid were mixed as 70: dissolving 30 mass percent of the mixture in DMF (the mass ratio of the total mass of the PAN and the PVDF to the mass of the DMF is 1: 9), and placing the mixture on an ultrasonic oscillator to oscillate for 60 minutes to prepare PAN and phosphoric acid electrostatic spinning precursor solution.
(3) Putting the PAN/PVDF graphene electrostatic spinning precursor solution obtained in the step (1) into a 20ml injector, spinning for 9 hours, wherein the spinning parameters are as follows: positive pressure is 20kV, and negative pressure is-2 kV; the spinning receiving distance is 25 cm; the flow rate of the spinning solution is 1.0 ml/h; spinning humidity is 40%, and PAN/PVDF/graphene fibers are obtained.
(4) And (3) putting the PAN and phosphoric acid electrostatic spinning precursor solution obtained in the step (2) into a 10ml injector, and spinning for 1 hour, wherein the spinning parameters are the same as those in the step (3), so as to obtain the phosphorus/PAN fiber.
(5) And (3) respectively attaching the upper surface and the lower surface of the phosphorus/PAN fiber in the step (4) to the PAN/PVDF/graphene fiber in the step (3) to obtain the sandwich self-supporting nanofiber.
(6) Placing the sandwich self-supporting nano-fiber in the step (5) into a tube furnace for pre-oxidation, and pre-oxidizingThe conditions were the same as in example 1. The preoxidized sandwich-type nano-fiber is calcined at high temperature under the protection of inert (high-purity nitrogen with the purity of more than or equal to 99.999%) atmosphere, and the calcining conditions are as follows: heating to 700 ℃ at the heating rate of 3 ℃/min, preserving the heat for 120min, and then cooling to room temperature at the cooling rate of 5 ℃/min to obtain the carbon nanofiber, thereby obtaining the electrode material of the super capacitor. In this example, the prepared supercapacitor electrode material was used as a working electrode, a platinum electrode was used as a counter electrode, and a saturated silver/AgCl electrode was used as a reference electrode in a three-electrode test system (shanghai chenhua instruments co., ltd CHI 660E). The electrolytic liquid system is 1M H2SO4When the current density was 1A/g, the specific capacitance was measured to be 150F/g.
Example 3
(1) PAN and PVDF are added into DMF (the mass ratio of the total mass of PAN and PVDF to DMF is 1: 9) according to the mass ratio of 70:30, 5 wt% (based on the total mass of PAN and PVDF) of graphene is added, and the rest is the same as that of the example 1, so that PAN/PVDF graphene electrostatic spinning precursor solution is prepared.
(2) PAN and phosphoric acid were mixed as 80: dissolving 20 mass percent of the mixture in acetone (the mass ratio of the total mass of the PAN and the PVDF to the mass of the acetone is 1: 9), and placing the mixture on an ultrasonic oscillator to oscillate for 60 minutes to prepare PAN and phosphoric acid electrostatic spinning precursor solution.
(3) Putting the PAN/PVDF graphene electrostatic spinning precursor solution obtained in the step (1) into a 20ml injector, spinning for 8 hours, wherein the spinning parameters are as follows: positive pressure of 17kV and negative pressure of-2 kV; the spinning receiving distance is 20 cm; the flow rate of the spinning solution is 0.8 ml/h; spinning humidity is 45%, and PAN/PVDF/graphene fibers are obtained.
(4) And (3) putting the PAN and phosphoric acid electrostatic spinning precursor solution in the step (2) into a 10ml injector, and spinning for 2 hours to obtain the phosphorus/PAN fiber, wherein the spinning parameters are the same as those in the step (3).
(5) And (3) respectively attaching the upper surface and the lower surface of the phosphorus/PAN fiber in the step (4) to the PAN/PVDF/graphene fiber in the step (3) to obtain the sandwich self-supporting nanofiber.
(6) And (3) placing the sandwich self-supporting nano-fiber in the step (5) into a tube furnace for pre-oxidation, wherein the pre-oxidation conditions are the same as those of the example 1. Pre-oxidized sandwich type nano fiberCalcining the carbon nano fiber under the protection of inert (high-purity nitrogen with the purity of more than or equal to 99.999%) atmosphere at high temperature under the same calcining condition as the embodiment 1 to obtain the carbon nano fiber, thereby obtaining the electrode material of the super capacitor. In this example, the prepared supercapacitor electrode material was used as a working electrode, a platinum electrode was used as a counter electrode, and a saturated silver/AgCl electrode was used as a reference electrode in a three-electrode test system (shanghai chenhua instruments co., ltd CHI 660E). The electrolytic liquid system is 1M H2SO4When the current density was 1A/g, the specific capacitance was measured to be 226F/g.
Example 4
(1) PAN and PVDF were added to DMAc (the mass ratio of the total mass of PAN and PVDF to DMAc was 1: 9) at a mass ratio of 70:30, 5 wt% (based on the total mass of PAN and PVDF) of graphene was added, and the remainder was the same as in example 1, to prepare a PAN/PVDF graphene electrospinning precursor solution.
(2) PAN and phosphoric acid were mixed as 70: dissolving 30 mass percent of the precursor solution in acetone (the mass ratio of the total mass of the PAN and the PVDF to the mass of the acetone is 1: 9), and placing the mixture on an ultrasonic oscillator to oscillate for 60 minutes to prepare the PAN and phosphoric acid electrostatic spinning precursor solution.
(3) Putting the PAN/PVDF graphene electrostatic spinning precursor solution obtained in the step (1) into a 20ml injector, spinning for 7 hours, wherein the spinning parameters are as follows: positive pressure 15kV and negative pressure-2 kV; the spinning receiving distance is 15 cm; the flow rate of the spinning solution is 0.5 ml/h; and spinning humidity is 50%, and PAN/PVDF/graphene fiber is obtained.
(4) And (3) putting the PAN and phosphoric acid electrostatic spinning precursor solution obtained in the step (2) into a 10ml injector, and spinning for 3 hours to obtain the phosphorus/PAN fiber, wherein the spinning parameters are the same as those in the step (3).
(5) And (3) respectively attaching the upper surface and the lower surface of the phosphorus/PAN fiber in the step (4) to the PAN/PVDF/graphene fiber in the step (3) to obtain the sandwich self-supporting nanofiber.
(6) And (3) placing the sandwich self-supporting nano-fiber in the step (5) into a tube furnace for pre-oxidation, wherein the pre-oxidation conditions are the same as those of the example 1. The preoxidized sandwich-type nanofibers are calcined at high temperature under the protection of inert (high-purity nitrogen with purity of more than or equal to 99.999%) atmosphere, the calcining conditions are the same as those in example 1, carbon nanofibers are obtained, and therefore the carbon nanofibers of the supercapacitor are obtainedAn electrode material. In this example, the prepared supercapacitor electrode material was used as a working electrode, a platinum electrode was used as a counter electrode, and a saturated silver/AgCl electrode was used as a reference electrode in a three-electrode test system (shanghai chenhua instruments co., ltd CHI 660E). The electrolytic liquid system is 1M H2SO4When the current density of the electrode material of the super capacitor prepared in the embodiment is 1A/g, the specific capacitance measured is 184F/g.
Comparative example 1
(1) 2g of PAN and 0.1g of phosphoric acid are respectively dissolved in 16mL of DMF, and the mixture is heated at 60 ℃ and subjected to ultrasonic treatment for 3 hours to prepare PAN and phosphoric acid electrostatic spinning precursor solution.
(2) And (2) putting the PAN/phosphoric acid electrostatic spinning precursor solution obtained in the step (1) into a 20ml injector, spinning for 10 hours, wherein the spinning parameters are as follows: positive pressure 16kV and negative pressure-2 kV; the spinning receiving distance is 18 cm; the flow rate of the spinning solution is 0.4 ml/h; spinning humidity is 50%, and PAN/phosphoric acid nano-fiber is obtained.
(3) And (3) placing the electrospun nanofiber membrane obtained in the step (2) in a tubular furnace, heating to 800 ℃ at the heating rate of 5 ℃/min, and preserving the heat in nitrogen for two hours to obtain the nitrogen-phosphorus doped electrode material. The comparative example was conducted in a three-electrode test system using the prepared supercapacitor electrode material as the working electrode, a platinum electrode as the counter electrode, and a saturated silver/AgCl electrode as the reference electrode. The electrolytic liquid system is 1M H2SO4At a current density of 0.5A/g, the specific capacitance was measured to be 224F/g.
Claims (9)
1. The self-supporting electrode material with the sandwich structure is characterized in that the electrode material is a porous graphene polymer carbon nanomaterial/heteroatom-doped polymer carbon nanomaterial/porous graphene polymer carbon nanomaterial with the sandwich structure.
2. The electrode material as claimed in claim 1, wherein the polymer comprises one or more of polyacrylonitrile, polyvinylidene fluoride, polyvinylpyrrolidone and polyvinyl alcohol; the heteroatom comprises one or more of nitrogen, phosphorus, sulfur and silicon.
3. A preparation method of a sandwich structure self-supporting electrode material comprises the following steps:
(1) dissolving a polymer and graphene in a solvent according to a mass ratio of 90: 10-99: 1 to obtain a graphene/polymer spinning solution, and then performing electrostatic spinning to obtain graphene/polymer fibers;
(2) dissolving a polymer and a substance containing a heteroatom into a solvent according to a mass ratio of 100-70:0-30 to obtain a heteroatom/polymer spinning solution, and then carrying out electrostatic spinning to obtain a heteroatom/polymer fiber, wherein the mass of the substance containing the heteroatom is not 0;
(3) respectively attaching the upper surface and the lower surface of the heteroatom/polymer fiber in the step (2) to the graphene/polymer fiber in the step (1) to obtain the sandwich self-supporting nanofiber;
(4) and (4) pre-oxidizing and crosslinking the sandwich self-supporting nanofiber obtained in the step (3), and then carbonizing the sandwich self-supporting nanofiber in an inert atmosphere to obtain a porous graphene polymer carbon nanomaterial/heteroatom-doped polymer carbon nanomaterial/porous graphene polymer carbon nanomaterial, namely the sandwich structure self-supporting electrode material.
4. The method according to claim 3, wherein the polymer in the steps (1) and (2) comprises one or more of polyacrylonitrile, polyvinylidene fluoride, polyvinylpyrrolidone and polyvinyl alcohol; the solvent comprises one or more of dimethylformamide, DMAc and acetone.
5. The method according to claim 3, wherein the electrostatic spinning in the steps (1) and (2) has the following technological parameters: the positive pressure is 15-20kV, the negative pressure is-2 kV, the receiving distance is 10-25cm, the flow rate of the spinning solution is 0.5-1.0ml/h, the humidity is 40-80%, and the spinning time is 1-20 hours.
6. The method according to claim 3, wherein the heteroatom-containing substance in step (2) comprises phosphoric acid.
7. The method as claimed in claim 3, wherein the pre-oxidation crosslinking in the step (4) has the following process parameters: heating to 200-300 deg.C at a rate of 2-5 deg.C/min, maintaining for 60-150min, and cooling to room temperature at a rate of 4-10 deg.C/min.
8. The method according to claim 3, wherein the carbonization in step (4) has the following process parameters: heating to 600-1000 ℃ at a heating rate of 2-8 ℃/min under an inert atmosphere, preserving heat for 60-240min, and then cooling to room temperature at a cooling rate of 4-10 ℃/min, wherein the inert atmosphere is high-purity nitrogen with the purity of more than or equal to 99.999%.
9. Use of the electrode material according to claim 1 in a supercapacitor.
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| CN110253984A (en) * | 2019-06-19 | 2019-09-20 | 大连工业大学 | A kind of electrostatic spinning nano fiber film-fabric composite coating material and preparation method |
| CN115036151A (en) * | 2022-07-08 | 2022-09-09 | 嘉兴学院 | Preparation method of conductive high polymer-based composite electrode material |
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| CN115036151A (en) * | 2022-07-08 | 2022-09-09 | 嘉兴学院 | Preparation method of conductive high polymer-based composite electrode material |
| CN115036151B (en) * | 2022-07-08 | 2023-11-24 | 嘉兴学院 | Preparation method of conductive polymer-based composite electrode material |
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