CN109216663A - A kind of nano particle/carbon cloth combination electrode material and preparation method thereof - Google Patents
A kind of nano particle/carbon cloth combination electrode material and preparation method thereof Download PDFInfo
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- CN109216663A CN109216663A CN201710531488.4A CN201710531488A CN109216663A CN 109216663 A CN109216663 A CN 109216663A CN 201710531488 A CN201710531488 A CN 201710531488A CN 109216663 A CN109216663 A CN 109216663A
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- Prior art keywords
- electrode material
- nano particle
- combination electrode
- carbon cloth
- transition metal
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- 239000004744 fabric Substances 0.000 title claims abstract description 54
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 45
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 45
- 239000007772 electrode material Substances 0.000 title claims abstract description 42
- 239000002105 nanoparticle Substances 0.000 title claims abstract description 42
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical class C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims abstract description 44
- 238000000034 method Methods 0.000 claims abstract description 24
- 229920000049 Carbon (fiber) Polymers 0.000 claims abstract description 22
- 239000004917 carbon fiber Substances 0.000 claims abstract description 22
- 229910052723 transition metal Inorganic materials 0.000 claims abstract description 20
- -1 transition metal salt Chemical class 0.000 claims abstract description 13
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000005011 phenolic resin Substances 0.000 claims abstract description 11
- 229920001568 phenolic resin Polymers 0.000 claims abstract description 11
- 239000000126 substance Substances 0.000 claims abstract description 11
- 150000003624 transition metals Chemical class 0.000 claims abstract description 11
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims abstract description 10
- 229910017604 nitric acid Inorganic materials 0.000 claims abstract description 10
- 238000007254 oxidation reaction Methods 0.000 claims abstract description 7
- 238000004073 vulcanization Methods 0.000 claims abstract description 7
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 claims abstract description 5
- 238000001802 infusion Methods 0.000 claims abstract description 5
- 150000004767 nitrides Chemical class 0.000 claims abstract description 5
- 238000010306 acid treatment Methods 0.000 claims abstract description 4
- 229910052976 metal sulfide Inorganic materials 0.000 claims abstract description 3
- 229910000314 transition metal oxide Inorganic materials 0.000 claims abstract description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 32
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 16
- 229910052786 argon Inorganic materials 0.000 claims description 16
- 239000007789 gas Substances 0.000 claims description 13
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 12
- 238000002791 soaking Methods 0.000 claims description 12
- 229910052757 nitrogen Inorganic materials 0.000 claims description 10
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 claims description 8
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims description 7
- 239000005864 Sulphur Substances 0.000 claims description 7
- KWSLGOVYXMQPPX-UHFFFAOYSA-N 5-[3-(trifluoromethyl)phenyl]-2h-tetrazole Chemical compound FC(F)(F)C1=CC=CC(C2=NNN=N2)=C1 KWSLGOVYXMQPPX-UHFFFAOYSA-N 0.000 claims description 6
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 6
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 6
- 235000019441 ethanol Nutrition 0.000 claims description 6
- 239000000835 fiber Substances 0.000 claims description 6
- 239000000463 material Substances 0.000 claims description 6
- 239000000843 powder Substances 0.000 claims description 6
- 229910001379 sodium hypophosphite Inorganic materials 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 5
- 239000002131 composite material Substances 0.000 claims description 5
- 239000001257 hydrogen Substances 0.000 claims description 5
- 229910052739 hydrogen Inorganic materials 0.000 claims description 5
- 229910052759 nickel Inorganic materials 0.000 claims description 5
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 4
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 4
- 239000004202 carbamide Substances 0.000 claims description 4
- 229910052802 copper Inorganic materials 0.000 claims description 4
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 claims description 4
- 229910001380 potassium hypophosphite Inorganic materials 0.000 claims description 4
- CRGPNLUFHHUKCM-UHFFFAOYSA-M potassium phosphinate Chemical compound [K+].[O-]P=O CRGPNLUFHHUKCM-UHFFFAOYSA-M 0.000 claims description 4
- 229910021529 ammonia Inorganic materials 0.000 claims description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 3
- 239000008246 gaseous mixture Substances 0.000 claims description 3
- 229910052742 iron Inorganic materials 0.000 claims description 3
- 230000003647 oxidation Effects 0.000 claims description 3
- 239000001301 oxygen Substances 0.000 claims description 3
- 229910052760 oxygen Inorganic materials 0.000 claims description 3
- 239000011148 porous material Substances 0.000 claims description 3
- 229910052718 tin Inorganic materials 0.000 claims description 3
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 claims description 2
- 229910002651 NO3 Inorganic materials 0.000 claims description 2
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 claims description 2
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 claims description 2
- 229910052782 aluminium Inorganic materials 0.000 claims description 2
- 229910052797 bismuth Inorganic materials 0.000 claims description 2
- 229910052793 cadmium Inorganic materials 0.000 claims description 2
- 229910052804 chromium Inorganic materials 0.000 claims description 2
- 238000007598 dipping method Methods 0.000 claims description 2
- 229910052733 gallium Inorganic materials 0.000 claims description 2
- 229910052738 indium Inorganic materials 0.000 claims description 2
- 229910052745 lead Inorganic materials 0.000 claims description 2
- 229910052748 manganese Inorganic materials 0.000 claims description 2
- 229910052750 molybdenum Inorganic materials 0.000 claims description 2
- 229910052758 niobium Inorganic materials 0.000 claims description 2
- 229910052763 palladium Inorganic materials 0.000 claims description 2
- 229910052707 ruthenium Inorganic materials 0.000 claims description 2
- 229910052709 silver Inorganic materials 0.000 claims description 2
- PUZPDOWCWNUUKD-UHFFFAOYSA-M sodium fluoride Chemical compound [F-].[Na+] PUZPDOWCWNUUKD-UHFFFAOYSA-M 0.000 claims description 2
- 239000002904 solvent Substances 0.000 claims description 2
- LSNNMFCWUKXFEE-UHFFFAOYSA-L sulfite Chemical compound [O-]S([O-])=O LSNNMFCWUKXFEE-UHFFFAOYSA-L 0.000 claims description 2
- 229910052719 titanium Inorganic materials 0.000 claims description 2
- 229910052721 tungsten Inorganic materials 0.000 claims description 2
- 229910052720 vanadium Inorganic materials 0.000 claims description 2
- 229910052725 zinc Inorganic materials 0.000 claims description 2
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims 2
- 229910052698 phosphorus Inorganic materials 0.000 claims 2
- 239000011574 phosphorus Substances 0.000 claims 2
- IOVCWXUNBOPUCH-UHFFFAOYSA-M Nitrite anion Chemical compound [O-]N=O IOVCWXUNBOPUCH-UHFFFAOYSA-M 0.000 claims 1
- 239000002253 acid Substances 0.000 claims 1
- 150000002576 ketones Chemical class 0.000 claims 1
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 claims 1
- FKNQFGJONOIPTF-UHFFFAOYSA-N Sodium cation Chemical compound [Na+] FKNQFGJONOIPTF-UHFFFAOYSA-N 0.000 abstract description 8
- 229910001415 sodium ion Inorganic materials 0.000 abstract description 8
- 229910001416 lithium ion Inorganic materials 0.000 abstract description 6
- 238000006555 catalytic reaction Methods 0.000 abstract description 4
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 abstract description 3
- 238000004146 energy storage Methods 0.000 abstract description 3
- 238000006243 chemical reaction Methods 0.000 abstract description 2
- 150000001875 compounds Chemical class 0.000 description 13
- 239000011149 active material Substances 0.000 description 11
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 8
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 5
- 239000002245 particle Substances 0.000 description 5
- 239000003990 capacitor Substances 0.000 description 4
- 239000010949 copper Substances 0.000 description 4
- 239000003792 electrolyte Substances 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- 238000001000 micrograph Methods 0.000 description 4
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 3
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 3
- 239000007864 aqueous solution Substances 0.000 description 3
- 239000008187 granular material Substances 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- 239000011230 binding agent Substances 0.000 description 2
- 235000013339 cereals Nutrition 0.000 description 2
- 229910017052 cobalt Inorganic materials 0.000 description 2
- 239000010941 cobalt Substances 0.000 description 2
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 2
- KTVIXTQDYHMGHF-UHFFFAOYSA-L cobalt(2+) sulfate Chemical compound [Co+2].[O-]S([O-])(=O)=O KTVIXTQDYHMGHF-UHFFFAOYSA-L 0.000 description 2
- 239000006258 conductive agent Substances 0.000 description 2
- ARUVKPQLZAKDPS-UHFFFAOYSA-L copper(II) sulfate Chemical compound [Cu+2].[O-][S+2]([O-])([O-])[O-] ARUVKPQLZAKDPS-UHFFFAOYSA-L 0.000 description 2
- 125000004122 cyclic group Chemical group 0.000 description 2
- 230000005611 electricity Effects 0.000 description 2
- 238000007654 immersion Methods 0.000 description 2
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 2
- KBJMLQFLOWQJNF-UHFFFAOYSA-N nickel(ii) nitrate Chemical compound [Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O KBJMLQFLOWQJNF-UHFFFAOYSA-N 0.000 description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 2
- 238000002336 sorption--desorption measurement Methods 0.000 description 2
- XJDNKRIXUMDJCW-UHFFFAOYSA-J titanium tetrachloride Chemical compound Cl[Ti](Cl)(Cl)Cl XJDNKRIXUMDJCW-UHFFFAOYSA-J 0.000 description 2
- 230000007704 transition Effects 0.000 description 2
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- 229910001290 LiPF6 Inorganic materials 0.000 description 1
- 239000007832 Na2SO4 Substances 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- 239000004743 Polypropylene Substances 0.000 description 1
- 229910021607 Silver chloride Inorganic materials 0.000 description 1
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 1
- 238000005452 bending Methods 0.000 description 1
- 239000004918 carbon fiber reinforced polymer Substances 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 239000011530 conductive current collector Substances 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 239000008358 core component Substances 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000004070 electrodeposition Methods 0.000 description 1
- 238000010041 electrostatic spinning Methods 0.000 description 1
- AQRRVVAHUPXEMW-UHFFFAOYSA-L ethanol;iron(2+);dichloride Chemical compound [Cl-].[Cl-].[Fe+2].CCO AQRRVVAHUPXEMW-UHFFFAOYSA-L 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 239000003365 glass fiber Substances 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- FBAFATDZDUQKNH-UHFFFAOYSA-M iron chloride Chemical compound [Cl-].[Fe] FBAFATDZDUQKNH-UHFFFAOYSA-M 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 238000001755 magnetron sputter deposition Methods 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 239000010955 niobium Substances 0.000 description 1
- GQPLMRYTRLFLPF-UHFFFAOYSA-N nitrous oxide Inorganic materials [O-][N+]#N GQPLMRYTRLFLPF-UHFFFAOYSA-N 0.000 description 1
- 238000007747 plating Methods 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 229920001155 polypropylene Polymers 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- HKZLPVFGJNLROG-UHFFFAOYSA-M silver monochloride Chemical compound [Cl-].[Ag+] HKZLPVFGJNLROG-UHFFFAOYSA-M 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- BAZAXWOYCMUHIX-UHFFFAOYSA-M sodium perchlorate Chemical compound [Na+].[O-]Cl(=O)(=O)=O BAZAXWOYCMUHIX-UHFFFAOYSA-M 0.000 description 1
- 229910001488 sodium perchlorate Inorganic materials 0.000 description 1
- 229910052938 sodium sulfate Inorganic materials 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/362—Composites
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/24—Electrodes characterised by structural features of the materials making up or comprised in the electrodes, e.g. form, surface area or porosity; characterised by the structural features of powders or particles used therefor
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
- H01G11/46—Metal oxides
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
- H01M4/581—Chalcogenides or intercalation compounds thereof
- H01M4/5815—Sulfides
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M2004/021—Physical characteristics, e.g. porosity, surface area
-
- 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
- Y02E60/10—Energy storage using batteries
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/13—Energy storage using capacitors
Landscapes
- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Power Engineering (AREA)
- Materials Engineering (AREA)
- Microelectronics & Electronic Packaging (AREA)
- General Chemical & Material Sciences (AREA)
- Electrochemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Composite Materials (AREA)
- Nanotechnology (AREA)
- Physics & Mathematics (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- General Physics & Mathematics (AREA)
- Crystallography & Structural Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Electric Double-Layer Capacitors Or The Like (AREA)
- Battery Electrode And Active Subsutance (AREA)
Abstract
The invention discloses a kind of nano particle/carbon cloth combination electrode materials and preparation method thereof, include: by infusion process in the micron order phenolic resin based activated carbon fiber of pre- nitric acid treatment carrying transition metal salt, mesoporous carbon fiber is obtained by high-temperature process again and embeds transition metal simple substance or the combination electrode material of its oxide nano particles, the embedded transition metal oxide/sulfide/nitride/phosphide nano particle combination electrode material of mesoporous carbon fiber can also be obtained by continuing high-temperature oxydation/vulcanization/nitridation/phosphatization.Nano particle prepared by the present invention/carbon cloth combination electrode material has excellent chemical property, can apply in the energy storages such as supercapacitor, lithium/sodium-ion battery and electro-catalysis and conversion field.
Description
Technical field
The present invention relates to a kind of for energy storage and converts the nano particle/carbon cloth combination electrode material in field,
Belong to technical field of material.
Background technique
In recent years, the demand of wearable flexible electronic device increasingly increases, and the flexible battery of flexible folding, super
Capacitor is the core component of flexible electronic device, and wherein flexible electrode is prepared into indispensable one of key.Currently,
It is received significant attention by the carbon-based collector of flexibility of representative of carbon cloth, with excellent foldable bending property, excellent
Electric conductivity, higher the advantages that loading specific surface area and light weight, electrode prepared therefrom is relative to conventional metals collection
The electrode of fluid preparation energy density with higher is without the use of conductive agent and binder, and has stronger foldable curved
Qu Xingneng.Meanwhile the electrode material based on carbon cloth also starts to be applied to other energy storages such as electro-catalysis and conversion field,
And it makes some progress.
However, existing carbon cloth based combined electrode is made in a manner of carbon fiber surface composite active material
It is standby, the side such as growth in situ and magnetron sputtering plating of the methods of direct coating, hydro-thermal method or electro-deposition including active material
Method.Electrode prepared by this kind of mode continuous active material configuration in surface during folded bent is easy to damage, and active material
It is directly exposed in electrolyte, active material apparent for bulk effect is easy to fall off in the circulating cycle to lead to reduced performance.This
Outside, the polyacrylonitrile-radical Carbon fiber nanoelectrode material of method of electrostatic spinning preparation, has higher cost, production efficiency low, uncomfortable
Close large area preparation and not environmentally the disadvantages of.
Transition-metals and their oxides, sulfide, nitride, phosphide are in supercapacitor, lithium/sodium-ion battery, electricity
The fields such as catalysis using long-standing, they generally have preferable electric conductivity, higher energy density and preferable circulation
Service life and chemical property stabilization, safety non-pollution, it is cheap and easy to get the features such as, thus be concerned, before wide application
Scape.It is it is compound with carbon material, reduce the designs such as its particle size and think currently, in order to improve the chemical property of this kind of material
Road, which has been obtained, generally to use
Summary of the invention
The purpose of the present invention is to provide a kind of nano particle/carbon cloth combination electrode material and preparation method thereof, gram
Take that the continuous active material configuration in surface during folded bent is easy to damage, active material is easy to fall off etc. in cyclic process lacks
Point.
To achieve the goals above, technical scheme is as follows:
A kind of nano particle/carbon cloth combination electrode material and preparation method thereof, by infusion process in pre- nitric acid treatment
Micron order phenolic resin based activated carbon fiber in carrying transition metal salt, then by high-temperature process obtain mesoporous carbon fiber embed transition
The combination electrode material of metal simple-substance or its oxide nano particles continues high-temperature oxydation/vulcanization/nitridation/phosphatization and may be used also
Transition metal oxide/sulfide/nitride/phosphide nano particle combination electrode material is embedded to obtain mesoporous carbon fiber
Material.
Further, the diameter dimension of micron order phenolic resin based activated carbon fiber is 2-20 μm.
Further, the pre- nitric acid treatment method of phenolic resin based activated carbon fiber are as follows: carbon cloth is immersed in concentrated nitric acid,
Soaking temperature is 40-120 DEG C, soaking time 4-24h.
Further, the dip time of infusion process is 6-48h, and dipping temperature is 10-60 DEG C, and the solvent for impregnating selection is
One or both of water, methanol, ethyl alcohol, acetone, ether.
Further, transition metal refer specifically to Ti, V, Cr, Mn, Fe, Co, Ni, Cu, Zn, Nb, Mo, Ru, Pd, Ag, Cd, W,
Any one or more in Al, Ga, In, Sn, Pb, Bi；The transition metal salt is nitrate, the nitrous of above-mentioned transition metal
Hydrochlorate, sulfate, sulphite, villaumite, villiaumite, any one or more in acetate, the concentration of transition metal salt is
0.05-2mol/L。
Further, the carbon cloth of carrying transition metal salt is placed in tube furnace and carries out high-temperature process, handle institute
Atmosphere is nitrogen, argon gas, hydrogen or argon hydrogen gaseous mixture, and treatment temperature is 600-1500 DEG C, soaking time 0.5-5h.
Further, the carbon cloth of embedded transition metal simple substance or its oxide is placed in tube furnace and carries out high temperature
Oxidation/vulcanization/nitridation/phosphatization；Wherein atmosphere used in oxidation processes is oxygen or air, and treatment temperature is 250-550 DEG C, is protected
The warm time is 5-20h；Atmosphere used in vulcanizing treatment is nitrogen or argon gas, and sulphur powder or thiocarbamide are placed on tube furnace by air inlet
One end, treatment temperature be 150-450 DEG C, soaking time 5-15h；Atmosphere used in nitrogen treatment is nitrogen or argon gas, is incited somebody to action
Urea is placed on one end that tube furnace leans on air inlet, or directly uses ammonia atmosphere, and treatment temperature is 150-800 DEG C, when heat preservation
Between be 3-10h；Atmosphere used in phosphorating treatment be nitrogen or argon gas, by sodium hypophosphite/potassium hypophosphite be placed on tube furnace lean on into
One end of port, treatment temperature are 200-450 DEG C, soaking time 1-5h；Wherein in vulcanization/nitridation/parkerizing process, transition gold
Belong to simple substance or its oxide and sulphur powder/thiocarbamide/urea/sodium hypophosphite/potassium hypophosphite molar ratio is 1:0.2-1:10.
Combination electrode material made from the above method, for Jie for generating 2-50nm inside micron order phenolic aldehyde base carbon fibre
Hole, nano particle are uniformly filled in mesoporous inside the carbon fiber, are formed nano particle and are embedded in mesoporous carbon fibrous inside
Composite construction.
Further, the BET specific surface area of mesoporous carbon fiber is 700-1500m2/ g, specific pore volume product are 0.1-0.8cm3/g。
Further, the diameter of nano particle is 10-500nm, and nano particle compares carrying capacity relative to the quality of entire electrode
For 10-70%, area ratio carrying capacity is 1-12mg/cm2。
The present invention compares compared with the prior art:
1, the flexible electrode material prepared does not need metal collector, binder and conductive agent, and active material is embedded in
Carbon fiber (conductive current collector) is internal, effectively reduces electrode volume, is conducive to the energy density and power density that improve electrode.
2, the mesoporous carbon cloth prepared embeds composite transition metal and its oxide, sulfide, nitride, phosphide
Flexible electrode is compared to the conventional electrode that active material is compounded in carbon fiber surface and is prepared, not only increase ion,
The transport capability of electronics, while effectively reducing mass loss of the active material in cyclic process, apply supercapacitor,
Lithium/sodium-ion battery and electro-catalysis etc. embody superior chemical property in fields.
3, the flexible electrode material prepared is not easily to fall off in folded bent process active material, and has preferable mechanics soft
Tough performance can be efficiently applied to the preparation of flexible electronic device.
Detailed description of the invention
Fig. 1 is NiS in embodiment 12Nano particle/carbon cloth combination electrode material photo in kind；
Fig. 2 is the BET adsorption desorption curve of the mesoporous carbon cloth of gained in embodiment 1；
Fig. 3 is Ni nano particle/carbon fiber reinforced polymers scanning electron microscope image in embodiment 1；
Fig. 4 is NiS in embodiment 12Nano particle/carbon cloth combination electrode material scanning electron microscope image；
Fig. 5 is NiS in embodiment 12Nano particle/carbon cloth combination electrode material exists as negative electrode of lithium ion battery
Cycle performance figure under 0.1A/g；
Fig. 6 is NiS in embodiment 12Nano particle/carbon cloth combination electrode material exists as sodium-ion battery cathode
Cycle performance figure under 0.1A/g；
Fig. 7 is NiS in embodiment 12Nano particle/carbon cloth combination electrode material as sodium-ion battery cathode
High rate performance figure；
Fig. 8 is Fe in embodiment 22O3Nano particle/carbon cloth combination electrode material exists as electrode of super capacitor
Cycle performance figure under 10A/g.
Specific embodiment
Embodiment 1
One piece of phenolic resin based activated carbon fiber cloth is immersed in 100 DEG C of pretreatment 12h in concentrated nitric acid, it is clear with water and ethyl alcohol later
Wash clean is spare.Pretreated carbon cloth is placed on 20 DEG C of immersion 6h in the nickel nitrate aqueous solution of 0.5M.Load is had
The carbon cloth of nickel nitrate is placed in tube furnace, leads to argon hydrogen gaseous mixture, is heated to 800 DEG C, is kept the temperature 0.5h, is obtained mesoporous carbon fiber
Tie up the compound of embedded nano nickle granules.Wherein the BET specific surface area of mesoporous carbon cloth is about 1100m2/ g, specific pore volume product is about
For 0.5cm3/ g, nickel particle is having a size of 20-60nm.Obtained compound is placed in tube furnace, sulphur powder is placed on pipe
Formula furnace leans on one end of air inlet, and the molar ratio of nickel and sulphur powder is 1:2 in compound, leads to argon gas, is heated to 200 DEG C, keeps the temperature 10h,
It finally obtains mesoporous carbon cloth and embeds NiS2The combination electrode material of nano particle.NiS2Particle diameter is 50-120nm, quality
It is about 30% than carrying capacity, area ratio carrying capacity is about 5mg/cm2.Fig. 1 is that mesoporous carbon fiber embeds NiS2The electrode material of nano particle
Photo in kind, as can be seen from the figure the electrode material has preferable flexible；Fig. 2 is the BET of the mesoporous carbon cloth of gained
Adsorption desorption curve；Fig. 3 is the scanning electron microscope image that mesoporous carbon fiber embeds nano nickle granules compound, from section, nickel
Grain is evenly distributed in inside carbon fiber；Fig. 4 is that carbon fiber embeds NiS2The scanning electron microscope image of nano particle, NiS2Nanometer
Grain is uniformly embedded in mesoporous carbon fibrous inside.
It will obtain NiS2Carbon fibre cloth is used as directly as test electrode, lithium metal to electrode, polypropylene screen conduct
Diaphragm is assembled into lithium ion half-cell, electrolyte are as follows: 1M LiPF6/ DMC:EC=1:1, test charging/discharging voltage section are
0.01-3V.Fig. 5 is cycle performance figure of the lithium ion half-cell of production under 0.1A/g current density, is still protected after 500 circles
1000mAh/g is held, conservation rate about 95% is recycled.
It will obtain NiS2Carbon fibre cloth is directly as test electrode, and metallic sodium is used as to electrode, and glass fibre membrane is made
Sodium ion half-cell, electrolyte are assembled into for diaphragm are as follows: 1M NaClO4/ EC:DEC (1:1)+2wt%FEC, test charge and discharge electricity
It is 0.01-3V between pressure area.Cycle performance figure of the sodium ion half-cell of Fig. 6 production under 0.1A/g current density, after 200 circles
600mAh/g is still kept, conservation rate about 91% is recycled；Fig. 7 is the high rate performance figure of the sodium ion half-cell of production, in 5A/g
Current density under capacity still keep 360mAh/g, embody preferable high rate performance.
Embodiment 2
One piece of phenolic resin based activated carbon fiber cloth is immersed in 90 DEG C of pretreatment 4h in concentrated nitric acid, is cleaned later with water and ethyl alcohol
It is clean spare.Pretreated carbon cloth is placed in the iron chloride ethanol solution of 0.1M and is impregnated for 24 hours for 40 DEG C.Load is had
The carbon cloth of iron chloride is placed in tube furnace, is led to argon gas, is heated to 900 DEG C, and 2h is kept the temperature, and obtains that mesoporous carbon fiber is embedded to be received
The compound of rice iron particle.Obtained compound is placed in tube furnace, oxygen is led to, is heated to 350 DEG C, keeps the temperature 10h, most
After obtain mesoporous carbon cloth embed Fe2O3The combination electrode material of nano particle.
The Fe that will be obtained2O3Carbon fibre cloth carries out three-electrode system test, platinized platinum as electrode material for super capacitor
As to electrode, Ag/AgCl is as reference electrode, 1M Na2SO4As electrolyte, constant current charge-discharge survey is carried out at room temperature
Examination, voltage range are -0.9-0V.Fig. 8 is Fe2O3Cycle performance figure of the carbon fibre cloth as electrode material for super capacitor,
Specific capacity at 2A/g is 180F/g (being based on entire electrode), and the circulation conservation rate of 5000 circles is about 88% at 10A/g.
Embodiment 3
One piece of phenolic resin based activated carbon fiber cloth is immersed in 120 DEG C of pretreatment 4h in concentrated nitric acid, it is clear with water and ethyl alcohol later
Wash clean is spare.Pretreated carbon cloth is placed on 20 DEG C of immersion 48h in the titanium tetrachloride aqueous solution of 0.05M.It will bear
The carbon cloth for being loaded with titanium tetrachloride is placed in tube furnace, leads to argon gas, is heated to 1200 DEG C, is kept the temperature 1h, is obtained mesoporous carbon fiber
Tie up the compound of embedded nano titania particle.Obtained compound is placed in tube furnace, leads to ammonia, is heated to 650
DEG C, 10h is kept the temperature, the combination electrode material that mesoporous carbon cloth embeds TiN nano particle is finally obtained.
Embodiment 4
One piece of phenolic resin based activated carbon fiber cloth is immersed in 100 DEG C of pretreatment 6h in concentrated nitric acid, it is clear with water and ethyl alcohol later
Wash clean is spare.Pretreated carbon cloth is placed on 30 in the copper sulphate of 0.1M and the mixed aqueous solution of 0.1M cobaltous sulfate
DEG C impregnate for 24 hours.There is the carbon cloth of copper sulphate and cobaltous sulfate to be placed in tube furnace load, lead to argon gas, be heated to 1000 DEG C,
2h is kept the temperature, the compound that mesoporous carbon fiber embeds Nanometer Copper and cobalt granule is obtained.Obtained compound is placed on tube furnace
In, sodium hypophosphite is placed on one end that tube furnace leans on air inlet, the molar ratio of copper and cobalt and sodium hypophosphite is 1 in compound:
5, lead to argon gas, be heated to 400 DEG C, keep the temperature 2h, finally obtains mesoporous carbon cloth and embed Cu3P and Co2The compound electric of P nano particle
Pole material.
Claims (10)
1. a kind of nano particle/carbon cloth combination electrode material preparation method, which is characterized in that by infusion process in pre- nitre
Carrying transition metal salt in the micron order phenolic resin based activated carbon fiber of acid processing, then obtained in mesoporous carbon fiber by high-temperature process
The combination electrode material of embedding transition metal simple substance or its oxide nano particles continues high-temperature oxydation/vulcanization/nitridation/phosphorus
Change obtains mesoporous carbon fiber and embeds transition metal oxide/sulfide/nitride/phosphide nano particle combination electrode material
Material.
2. nano particle according to claim 1/carbon cloth combination electrode material preparation method, which is characterized in that
The diameter dimension of the micron order phenolic resin based activated carbon fiber is 2-20 μm.
3. nano particle according to claim 1/carbon cloth combination electrode material preparation method, which is characterized in that
The pre- nitric acid treatment method of the phenolic resin based activated carbon fiber are as follows: carbon cloth is immersed in concentrated nitric acid, soaking temperature 40-
120 DEG C, soaking time 4-24h.
4. nano particle according to claim 1/carbon cloth combination electrode material preparation method, which is characterized in that
The dip time of the infusion process is 6-48h, and dipping temperature is 10-60 DEG C, and the solvent for impregnating selection is water, methanol, ethyl alcohol, third
One or both of ketone, ether.
5. nano particle according to claim 1/carbon cloth combination electrode material preparation method, which is characterized in that
The transition metal refer specifically to Ti, V, Cr, Mn, Fe, Co, Ni, Cu, Zn, Nb, Mo, Ru, Pd, Ag, Cd, W, Al, Ga, In, Sn,
Any one or more in Pb, Bi；The transition metal salt be the nitrate of above-mentioned transition metal, nitrite, sulfate,
Sulphite, villaumite, villiaumite, any one or more in acetate, the concentration of transition metal salt is 0.05-2mol/L.
6. nano particle according to claim 1/carbon cloth combination electrode material preparation method, which is characterized in that
The carbon cloth of carrying transition metal salt is placed in tube furnace and carries out high-temperature process, handling atmosphere used is nitrogen, argon
Gas, hydrogen or argon hydrogen gaseous mixture, treatment temperature are 600-1500 DEG C, soaking time 0.5-5h.
7. nano particle according to claim 1/carbon cloth combination electrode material preparation method, which is characterized in that
The carbon cloth of embedded transition metal simple substance or its oxide is placed on progress high-temperature oxydation/vulcanization/nitridation/phosphorus in tube furnace
Change；Wherein atmosphere used in oxidation processes is oxygen or air, and treatment temperature is 250-550 DEG C, soaking time 5-20h；Sulphur
Changing processing atmosphere used is nitrogen or argon gas, and sulphur powder or thiocarbamide are placed on one end that tube furnace leans on air inlet, treatment temperature
It is 150-450 DEG C, soaking time 5-15h；Atmosphere used in nitrogen treatment is nitrogen or argon gas, and urea is placed on tube furnace
By one end of air inlet, or ammonia atmosphere is directly used, treatment temperature is 150-800 DEG C, soaking time 3-10h；At phosphatization
Reason atmosphere used is nitrogen or argon gas, and sodium hypophosphite/potassium hypophosphite is placed on one end that tube furnace leans on air inlet, processing temperature
Degree is 200-450 DEG C, soaking time 1-5h；Wherein, in vulcanization/nitridation/parkerizing process, transition metal simple substance or its oxide
It is 1:0.2-1:10 with sulphur powder/thiocarbamide/urea/sodium hypophosphite/potassium hypophosphite molar ratio.
8. a kind of based on multiple made from nano particle described in claim 1-7/carbon cloth combination electrode material preparation method
Composite electrode material, which is characterized in that the combination electrode material is that the mesoporous of 2-50nm is generated inside micron order phenolic aldehyde base carbon fibre,
Nano particle is uniformly filled in mesoporous inside the carbon fiber, is formed nano particle and is embedded in the composite junction inside carbon fiber
Structure.
9. combination electrode material according to claim 8, which is characterized in that the BET specific surface of the mesoporous carbon fiber
Product is 700-1500m2/ g, specific pore volume product are 0.1-0.8cm3/g。
10. combination electrode material according to claim 8, which is characterized in that the diameter of the nano particle is 10-
500nm, nano particle relative to entire electrode quality than carrying capacity be 10-70%, area ratio carrying capacity be 1-12mg/cm2。
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