CN113451052A - Conductive polymer-based supercapacitor electrode and preparation method thereof - Google Patents
Conductive polymer-based supercapacitor electrode and preparation method thereof Download PDFInfo
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- CN113451052A CN113451052A CN202110765162.4A CN202110765162A CN113451052A CN 113451052 A CN113451052 A CN 113451052A CN 202110765162 A CN202110765162 A CN 202110765162A CN 113451052 A CN113451052 A CN 113451052A
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- 229920001940 conductive polymer Polymers 0.000 title claims abstract description 39
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- 230000001590 oxidative effect Effects 0.000 claims abstract description 24
- 239000007772 electrode material Substances 0.000 claims abstract description 22
- 239000000758 substrate Substances 0.000 claims abstract description 19
- 238000005229 chemical vapour deposition Methods 0.000 claims abstract description 18
- 239000007800 oxidant agent Substances 0.000 claims abstract description 18
- 239000000178 monomer Substances 0.000 claims abstract description 17
- 239000000463 material Substances 0.000 claims abstract description 16
- 239000002086 nanomaterial Substances 0.000 claims abstract description 15
- 238000000034 method Methods 0.000 claims abstract description 13
- 239000003990 capacitor Substances 0.000 claims abstract description 12
- QENGPZGAWFQWCZ-UHFFFAOYSA-N 3-Methylthiophene Chemical compound CC=1C=CSC=1 QENGPZGAWFQWCZ-UHFFFAOYSA-N 0.000 claims description 12
- 229920001609 Poly(3,4-ethylenedioxythiophene) Polymers 0.000 claims description 10
- 239000002073 nanorod Substances 0.000 claims description 9
- 230000003647 oxidation Effects 0.000 claims description 9
- 238000007254 oxidation reaction Methods 0.000 claims description 9
- 238000000151 deposition Methods 0.000 claims description 8
- GKWLILHTTGWKLQ-UHFFFAOYSA-N 2,3-dihydrothieno[3,4-b][1,4]dioxine Chemical compound O1CCOC2=CSC=C21 GKWLILHTTGWKLQ-UHFFFAOYSA-N 0.000 claims description 7
- 229920000049 Carbon (fiber) Polymers 0.000 claims description 7
- 239000004917 carbon fiber Substances 0.000 claims description 7
- 239000004744 fabric Substances 0.000 claims description 7
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims description 7
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 7
- PAYRUJLWNCNPSJ-UHFFFAOYSA-N Aniline Chemical compound NC1=CC=CC=C1 PAYRUJLWNCNPSJ-UHFFFAOYSA-N 0.000 claims description 6
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 6
- YTPLMLYBLZKORZ-UHFFFAOYSA-N Thiophene Chemical compound C=1C=CSC=1 YTPLMLYBLZKORZ-UHFFFAOYSA-N 0.000 claims description 6
- 238000006243 chemical reaction Methods 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 6
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 4
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 4
- SICLLPHPVFCNTJ-UHFFFAOYSA-N 1,1,1',1'-tetramethyl-3,3'-spirobi[2h-indene]-5,5'-diol Chemical compound C12=CC(O)=CC=C2C(C)(C)CC11C2=CC(O)=CC=C2C(C)(C)C1 SICLLPHPVFCNTJ-UHFFFAOYSA-N 0.000 claims description 3
- VMPVEPPRYRXYNP-UHFFFAOYSA-I antimony(5+);pentachloride Chemical compound Cl[Sb](Cl)(Cl)(Cl)Cl VMPVEPPRYRXYNP-UHFFFAOYSA-I 0.000 claims description 3
- ZHXZNKNQUHUIGN-UHFFFAOYSA-N chloro hypochlorite;vanadium Chemical compound [V].ClOCl ZHXZNKNQUHUIGN-UHFFFAOYSA-N 0.000 claims description 3
- 239000002127 nanobelt Substances 0.000 claims description 3
- 229920000767 polyaniline Polymers 0.000 claims description 3
- 238000006116 polymerization reaction Methods 0.000 claims description 3
- 229930192474 thiophene Natural products 0.000 claims description 3
- BMYNFMYTOJXKLE-UHFFFAOYSA-N 3-azaniumyl-2-hydroxypropanoate Chemical compound NCC(O)C(O)=O BMYNFMYTOJXKLE-UHFFFAOYSA-N 0.000 claims description 2
- 238000002791 soaking Methods 0.000 claims description 2
- 238000001291 vacuum drying Methods 0.000 claims description 2
- 239000000843 powder Substances 0.000 claims 1
- 230000014759 maintenance of location Effects 0.000 abstract description 3
- 229920000642 polymer Polymers 0.000 abstract description 2
- 238000004146 energy storage Methods 0.000 description 8
- 239000002322 conducting polymer Substances 0.000 description 7
- 230000001276 controlling effect Effects 0.000 description 7
- 239000002131 composite material Substances 0.000 description 5
- 239000010408 film Substances 0.000 description 5
- 238000005086 pumping Methods 0.000 description 5
- 238000000576 coating method Methods 0.000 description 4
- 238000001816 cooling Methods 0.000 description 4
- 239000002070 nanowire Substances 0.000 description 4
- 229910021578 Iron(III) chloride Inorganic materials 0.000 description 3
- 239000011248 coating agent Substances 0.000 description 3
- 238000002484 cyclic voltammetry Methods 0.000 description 3
- 239000000835 fiber Substances 0.000 description 2
- 238000001000 micrograph Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 230000001351 cycling effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000003618 dip coating Methods 0.000 description 1
- 238000012983 electrochemical energy storage Methods 0.000 description 1
- 238000004070 electrodeposition Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000001747 exhibiting effect Effects 0.000 description 1
- 238000006479 redox reaction Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000004528 spin coating Methods 0.000 description 1
- 238000010408 sweeping Methods 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
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Classifications
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G9/00—Electrolytic capacitors, rectifiers, detectors, switching devices, light-sensitive or temperature-sensitive devices; Processes of their manufacture
- H01G9/004—Details
- H01G9/04—Electrodes or formation of dielectric layers thereon
- H01G9/042—Electrodes or formation of dielectric layers thereon characterised by the material
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
- D06M15/37—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/40—Fibres of carbon
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/13—Energy storage using capacitors
Abstract
The invention discloses a super capacitor electrode material and a preparation method thereof. The material of the invention is obtained by oxidizing a chemical vapor deposition conductive polymer on a substrate with a nano structure; the oxidative chemical vapor deposition is to introduce gasified monomers and oxidant into a reactor to react on a substrate with controllable temperature to generate a conductive polymer film layer with controllable thickness and good shape retention. The supercapacitor electrode material prepared by the method not only improves the specific capacitance of the polymer-based supercapacitor, but also keeps the good cycle life of the electrode material.
Description
Technical Field
The invention relates to the field of super capacitors, in particular to a conducting polymer-based super capacitor electrode and a preparation method thereof.
Background
The increasing development of intelligent electronic products has stimulated a great demand for safe and reliable energy storage devices. Among the many energy storage devices, supercapacitors have been extensively studied for their higher power and energy density. Conductive polymers have attracted considerable attention in energy storage applications due to their advantages of good conductivity, flexibility, processability, and low cost. However, redox reactions in electrochemical energy storage processes can cause volume changes of conductive polymers, thereby causing poor cycle stability, which is an important factor limiting practical applications. The conductive polymer is coated on other stable substrate materials with nano structures to construct the composite electrode, so that the stability of the composite electrode can be improved, the specific surface area of the composite electrode can be enlarged, the active sites can be increased, and the charge transfer distance can be shortened. However, conventional solution coating methods, such as spin coating, dip coating, or electrochemical deposition, are selective for the substrate material, the resulting thin film is poorly conductive, and it is difficult to retain the nanostructure of the substrate, which may block the nanocavities inside the substrate material, thereby reducing the number of active sites. Therefore, the search for a gas phase process to prepare highly conductive, highly conformal conductive polymers is critical to facilitate their use in energy storage.
Disclosure of Invention
The invention aims to provide a conducting polymer-based supercapacitor electrode; the invention also aims to provide a preparation method of the conducting polymer-based supercapacitor electrode; the method provides a method for conformally depositing a high-conductivity polymer on the surface of a substrate with a nano structure by utilizing a chemical vapor deposition technology, and simultaneously provides a stable and efficient electrode material of a super capacitor.
In order to achieve the above object, the present invention provides a supercapacitor electrode material comprising a conductive polymer and a substrate material having a nanostructure;
the conductive polymer is one or more of poly (3, 4-ethylenedioxythiophene), polyaniline and poly (3-methylthiophene);
the substrate material with the nano structure is any one of SiC nanowires, nanobelts, nanorods and carbon fiber cloth with the SiC material.
The preparation method of the supercapacitor electrode material adopts a chemical vapor deposition method to deposit a layer of conductive polymer on the surface of a substrate with a nano structure, and the reaction is completed in a reactor for oxidizing chemical vapor deposition, and comprises the following steps:
fixing a base material to be deposited on a sample table above a reactor, and controlling the base material at 25-200 ℃;
placing an oxidant into a crucible below the reactor, covering a baffle plate in a screwing manner, and controlling the temperature of the crucible to be 150-250 ℃;
pumping a preset vacuum degree in the reactor, wherein the vacuum degree is 200-900 mTorr, and unscrewing a baffle above the crucible;
and step four, introducing the gasified conductive polymer monomer into a reactor, reacting under the action of oxidant gas, and covering the surface of the substrate with a conductive polymer film layer to obtain the electrode material of the supercapacitor.
The rotation frequency of a sample stage in the oxidation chemical vapor deposition reactor is 0-100 rad/min; the temperature of the sample stage is 25-200 ℃.
The conductive polymer is prepared by the polymerization reaction of the following monomers; the monomer is one or the combination of more than two of 3, 4-ethylenedioxythiophene, thiophene, aniline and 3-methylthiophene.
And finally obtaining the conductive polymer film layer with the composition gradient through monomer flow control.
The oxidant is one or the combination of more than two of ferric trichloride, vanadium oxychloride and antimony pentachloride.
The ratio of the monomer to the oxidant is 1: 10-1: 30.
The sample obtained after the oxidation chemical vapor deposition can be subjected to one or more of hydrobromic acid, sulfuric acid, hydrochloric acid and methanol soaking treatment in sequence according to needs, and then vacuum drying is carried out.
The conductive polymer is Cl-Doping the conductive polymer.
The conductive polymer-based supercapacitor electrode and the preparation method thereof have the beneficial effects that: the method has no special requirements on the substrate, no solvent residue, uniform film, good shape retention and high conductivity; aiming at the defect that the specific capacitance of the conventional conductive polymer used for the electrode material of the super capacitor is lower, the conductive polymer is deposited on the substrate material with the nano structure and used as the self-supporting electrode material of the super capacitor, so that the specific capacitance of the super capacitor is improved, and the cycling stability of the electrode material is kept.
Drawings
FIG. 1 is a schematic view of an oxidative chemical vapor deposition coating apparatus according to the present invention;
FIG. 2 is a scanning electron microscope image of PEDOT-coated SiC nanorods prepared in examples 1-4, respectively;
FIG. 3 is a transmission electron microscope image of PEDOT-coated SiC nanorods prepared in example 3;
fig. 4(a) is a cyclic voltammogram of the PEDOT-coated SiC nanowire composite electrode and the pure SiC nanowire electrode prepared in examples 1 to 4;
FIG. 4(b) is a graph showing the change of specific capacitance with sweeping speed of the PEDOT-coated SiC nanowire composite electrode and the pure SiC nanowire electrode prepared in examples 1 to 4;
FIG. 5 shows the construction of an electrode in example 3 with a sweep rate of 10 to 200mV s under a two-electrode system-1Cyclic voltammetry of (a);
fig. 6 is a graph showing the cycle stability of the electrode constructed in example 3 measured by a constant current charge and discharge method under a two-electrode system.
Detailed Description
Example 1
The invention relates to a preparation method of a conducting polymer-based supercapacitor electrode, which is prepared by the following steps:
fixing the carbon fiber cloth with the SiC nano-rods on a sample table above an oxidation chemical vapor deposition reactor, and controlling the temperature of the sample table at 100 ℃; ferric trichloride is taken as an oxidant, and the temperature of the oxidant is controlled at 230 ℃; pumping the mixture to 300mTorr, introducing 3, 4-ethylene dioxythiophene monomer with the flow of 3sccm, depositing for 5min, stopping the reaction, and naturally cooling.
Example 2
The invention relates to a preparation method of a conducting polymer-based supercapacitor electrode, which is prepared by the following steps:
fixing the carbon fiber cloth with the SiC nano-rods on a sample table above an oxidation chemical vapor deposition reactor, and controlling the temperature of the sample table at 100 ℃; ferric chloride is used as an oxidant, and the temperature of the oxidant is controlled at 230 ℃; pumping the mixture to 300mTorr in vacuum, introducing 3, 4-ethylene dioxythiophene monomer with the flow rate of 3sccm, depositing for 10min, stopping the reaction, and naturally cooling.
Example 3
The invention relates to a preparation method of a conducting polymer-based supercapacitor electrode, which is prepared by the following steps:
fixing the carbon fiber cloth with the SiC nano-rods on a sample table above an oxidation chemical vapor deposition reactor, and controlling the temperature of the sample table at 100 ℃; ferric chloride is used as an oxidant, and the temperature of the oxidant is controlled at 230 ℃; pumping the mixture to 300mTorr in vacuum, introducing 3, 4-ethylene dioxythiophene monomer with the flow rate of 3sccm, depositing for 15min, stopping the reaction, and naturally cooling.
Example 4
The invention relates to a preparation method of a conducting polymer-based supercapacitor electrode, which is prepared by the following steps:
fixing the carbon fiber cloth with the SiC nano-rods on a sample table above an oxidation chemical vapor deposition reactor, and controlling the temperature of the sample table at 100 ℃; ferric chloride is used as an oxidant, and the temperature of the oxidant is controlled at 230 ℃; pumping the mixture to 300mTorr in vacuum, introducing 3, 4-ethylene dioxythiophene monomer with the flow rate of 3sccm, depositing for 20min, stopping the reaction, and naturally cooling.
In summary, examples 1-4 show that:
depositing a PEDOT film on the surface of the SiC fiber by using an oxidation chemical vapor deposition method, wherein the obtained film layer is uniform and has good shape retention (figures 2 and 3);
the approximate rectangular cyclic voltammetry curve proves that the electrode material has good conductivity and small internal resistance (figure 4 a);
the energy storage characteristics of the SiC fibers can be obviously improved by depositing the PEDOT coating through comparing the specific capacitance, and the optimal specific capacitance is obtained by regulating and controlling the morphology of the coating (figure 4 b);
an optimized SiC @ PEDOT-15 electrode is selected for constructing the super capacitor, and a two-electrode system is adopted for representing the energy storage characteristic of the super capacitor, so that the result shows that the super capacitor has great potential in the aspect of energy storage of the super capacitor (figure 5);
the cycle stability of the obtained device was measured, and it was found that the energy storage characteristics thereof remained 104% of the initial value after 10000 cycles, exhibiting excellent cycle stability (fig. 6).
The conductive polymer can be one or more of poly (3, 4-ethylenedioxythiophene), polyaniline and poly (3-methylthiophene), but is not limited to the poly (3, 4-ethylenedioxythiophene);
the substrate material having the nanostructure may be, but is not limited to, any one of SiC nanowires, nanobelts, nanorods, and carbon fiber cloth on which SiC nanomaterial is grown.
The conductive polymer is prepared by the polymerization reaction of the following monomers; the monomer can be one or the combination of more than two of 3, 4-ethylene dioxythiophene, thiophene, aniline and 3-methyl thiophene.
The oxidant can be one or the combination of any two or more of ferric trichloride, vanadium oxychloride and antimony pentachloride.
Claims (9)
1. A supercapacitor electrode material, characterized in that: the supercapacitor electrode material comprises a conductive polymer and a substrate material with a nano structure, and is obtained by oxidizing a chemical vapor deposition conductive polymer on a substrate with the nano structure;
the conductive polymer is one or more of poly (3, 4-ethylenedioxythiophene), polyaniline and poly (3-methylthiophene);
the substrate material with the nano structure is any one of SiC nanowires, nanobelts, nanorods and carbon fiber cloth on which SiC nanomaterials grow.
2. A preparation method of a super capacitor electrode material is characterized by comprising the following steps: depositing a layer of conductive polymer on the surface of a substrate material with a nano structure by using a chemical vapor deposition method, wherein the reaction is completed in a reactor for oxidizing chemical vapor deposition, and the method comprises the following steps:
fixing a base material to be deposited on a reactor sample table, and controlling the base material to be deposited at 25-200 ℃;
placing oxidant powder into a crucible below the reactor, covering a baffle plate in a screwing manner, and controlling the temperature of the crucible to be 150-250 ℃;
vacuumizing the reactor, wherein the vacuum degree is 200-900 mTorr, and unscrewing a baffle above the crucible after the set vacuum degree is reached;
and step four, introducing the gasified conductive polymer monomer into a reactor, reacting under the action of a gaseous oxidant, and covering a conductive polymer film layer on the surface of the substrate to prepare the electrode material of the supercapacitor.
3. The preparation method of the electrode material of the supercapacitor as claimed in claim 2, wherein: the rotation frequency of a sample stage in the oxidation chemical vapor deposition reactor is 0-100 rad/min; the temperature of the sample stage is 25-200 ℃.
4. The preparation method of the electrode material of the supercapacitor as claimed in claim 2, wherein: the conductive polymer is prepared by the polymerization reaction of the following monomers; the monomer is one or the combination of more than two of 3, 4-ethylenedioxythiophene, thiophene, aniline and 3-methylthiophene.
5. The method for preparing the electrode material of the supercapacitor as claimed in claim 2 or 4, wherein: and finally obtaining the conductive polymer film layer with the composition gradient through monomer flow control.
6. The preparation method of the electrode material of the supercapacitor as claimed in claim 2, wherein: the oxidant is one or the combination of more than two of ferric trichloride, vanadium oxychloride and antimony pentachloride.
7. The preparation method of the electrode material of the supercapacitor as claimed in claim 6, wherein: the ratio of the monomer to the oxidant is 1: 10-1: 30.
8. The preparation method of the electrode material of the supercapacitor as claimed in claim 7, wherein: the sample obtained after the oxidation chemical vapor deposition method can be subjected to one or more of hydrobromic acid, sulfuric acid, hydrochloric acid and methanol soaking treatment in sequence according to needs, and then is subjected to vacuum drying.
9. The preparation method of the electrode material of the supercapacitor as claimed in claim 8, wherein: the conductive polymer is Cl-Doping the conductive polymer.
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| CN202110765162.4A CN113451052A (en) | 2021-07-06 | 2021-07-06 | Conductive polymer-based supercapacitor electrode and preparation method thereof |
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| CN202110765162.4A CN113451052A (en) | 2021-07-06 | 2021-07-06 | Conductive polymer-based supercapacitor electrode and preparation method thereof |
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|---|---|---|---|---|
| US20100255303A1 (en) * | 2008-12-03 | 2010-10-07 | Massachusetts Institute Of Technology | Multifunctional composites based on coated nanostructures |
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-
2021
- 2021-07-06 CN CN202110765162.4A patent/CN113451052A/en active Pending
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| US20100255303A1 (en) * | 2008-12-03 | 2010-10-07 | Massachusetts Institute Of Technology | Multifunctional composites based on coated nanostructures |
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