CN109216044A - Graphene/metal oxide combination electrode material is prepared in situ in mechanochemical reaction - Google Patents
Graphene/metal oxide combination electrode material is prepared in situ in mechanochemical reaction Download PDFInfo
- Publication number
- CN109216044A CN109216044A CN201811063495.7A CN201811063495A CN109216044A CN 109216044 A CN109216044 A CN 109216044A CN 201811063495 A CN201811063495 A CN 201811063495A CN 109216044 A CN109216044 A CN 109216044A
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- Prior art keywords
- metal oxide
- graphene
- electrode material
- combination electrode
- situ
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 98
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 73
- 239000007772 electrode material Substances 0.000 title claims abstract description 52
- 229910044991 metal oxide Inorganic materials 0.000 title claims abstract description 48
- 150000004706 metal oxides Chemical class 0.000 title claims abstract description 48
- 238000011065 in-situ storage Methods 0.000 title claims abstract description 30
- 238000010303 mechanochemical reaction Methods 0.000 title claims description 24
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- 239000010439 graphite Substances 0.000 claims abstract description 25
- 238000006243 chemical reaction Methods 0.000 claims abstract description 19
- 239000012702 metal oxide precursor Substances 0.000 claims abstract description 10
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- 239000004094 surface-active agent Substances 0.000 claims description 4
- HVCOBJNICQPDBP-UHFFFAOYSA-N 3-[3-[3,5-dihydroxy-6-methyl-4-(3,4,5-trihydroxy-6-methyloxan-2-yl)oxyoxan-2-yl]oxydecanoyloxy]decanoic acid;hydrate Chemical compound O.OC1C(OC(CC(=O)OC(CCCCCCC)CC(O)=O)CCCCCCC)OC(C)C(O)C1OC1C(O)C(O)C(O)C(C)O1 HVCOBJNICQPDBP-UHFFFAOYSA-N 0.000 claims description 3
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- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 2
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 claims description 2
- 229920000084 Gum arabic Polymers 0.000 claims description 2
- 229910002567 K2S2O8 Inorganic materials 0.000 claims description 2
- WAEMQWOKJMHJLA-UHFFFAOYSA-N Manganese(2+) Chemical compound [Mn+2] WAEMQWOKJMHJLA-UHFFFAOYSA-N 0.000 claims description 2
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 2
- 239000004698 Polyethylene Substances 0.000 claims description 2
- 239000002202 Polyethylene glycol Substances 0.000 claims description 2
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- KJTLSVCANCCWHF-UHFFFAOYSA-N Ruthenium Chemical compound [Ru] KJTLSVCANCCWHF-UHFFFAOYSA-N 0.000 claims description 2
- 241000978776 Senegalia senegal Species 0.000 claims description 2
- PRXRUNOAOLTIEF-ADSICKODSA-N Sorbitan trioleate Chemical compound CCCCCCCC\C=C/CCCCCCCC(=O)OC[C@@H](OC(=O)CCCCCCC\C=C/CCCCCCCC)[C@H]1OC[C@H](O)[C@H]1OC(=O)CCCCCCC\C=C/CCCCCCCC PRXRUNOAOLTIEF-ADSICKODSA-N 0.000 claims description 2
- 235000021355 Stearic acid Nutrition 0.000 claims description 2
- LWZFANDGMFTDAV-BURFUSLBSA-N [(2r)-2-[(2r,3r,4s)-3,4-dihydroxyoxolan-2-yl]-2-hydroxyethyl] dodecanoate Chemical compound CCCCCCCCCCCC(=O)OC[C@@H](O)[C@H]1OC[C@H](O)[C@H]1O LWZFANDGMFTDAV-BURFUSLBSA-N 0.000 claims description 2
- 235000010489 acacia gum Nutrition 0.000 claims description 2
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- 229910001870 ammonium persulfate Inorganic materials 0.000 claims description 2
- 238000000498 ball milling Methods 0.000 claims description 2
- WOWHHFRSBJGXCM-UHFFFAOYSA-M cetyltrimethylammonium chloride Chemical compound [Cl-].CCCCCCCCCCCCCCCC[N+](C)(C)C WOWHHFRSBJGXCM-UHFFFAOYSA-M 0.000 claims description 2
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical group [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims description 2
- YDEXUEFDPVHGHE-GGMCWBHBSA-L disodium;(2r)-3-(2-hydroxy-3-methoxyphenyl)-2-[2-methoxy-4-(3-sulfonatopropyl)phenoxy]propane-1-sulfonate Chemical group [Na+].[Na+].COC1=CC=CC(C[C@H](CS([O-])(=O)=O)OC=2C(=CC(CCCS([O-])(=O)=O)=CC=2)OC)=C1O YDEXUEFDPVHGHE-GGMCWBHBSA-L 0.000 claims description 2
- 238000001125 extrusion Methods 0.000 claims description 2
- 229910052736 halogen Inorganic materials 0.000 claims description 2
- 150000002367 halogens Chemical class 0.000 claims description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 2
- 229910052742 iron Inorganic materials 0.000 claims description 2
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims description 2
- 229940059939 kayexalate Drugs 0.000 claims description 2
- 150000002696 manganese Chemical class 0.000 claims description 2
- 229910001437 manganese ion Inorganic materials 0.000 claims description 2
- 238000003801 milling Methods 0.000 claims description 2
- 150000002815 nickel Chemical class 0.000 claims description 2
- 229910001453 nickel ion Inorganic materials 0.000 claims description 2
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 claims description 2
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 claims description 2
- 229920001467 poly(styrenesulfonates) Polymers 0.000 claims description 2
- 229920000570 polyether Polymers 0.000 claims description 2
- 229920000573 polyethylene Polymers 0.000 claims description 2
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- 150000003077 polyols Chemical class 0.000 claims description 2
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- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 2
- 235000019422 polyvinyl alcohol Nutrition 0.000 claims description 2
- KMUONIBRACKNSN-UHFFFAOYSA-N potassium dichromate Chemical compound [K+].[K+].[O-][Cr](=O)(=O)O[Cr]([O-])(=O)=O KMUONIBRACKNSN-UHFFFAOYSA-N 0.000 claims description 2
- 229910001487 potassium perchlorate Inorganic materials 0.000 claims description 2
- 238000010008 shearing Methods 0.000 claims description 2
- 239000007790 solid phase Substances 0.000 claims description 2
- 235000011067 sorbitan monolaureate Nutrition 0.000 claims description 2
- 239000008117 stearic acid Substances 0.000 claims description 2
- 229920000428 triblock copolymer Polymers 0.000 claims description 2
- 150000003751 zinc Chemical class 0.000 claims description 2
- HVUMOYIDDBPOLL-UHFFFAOYSA-N 2-(3,4-Dihydroxyoxolan-2-yl)-2-hydroxyethyl octadecanoate Chemical compound CCCCCCCCCCCCCCCCCC(=O)OCC(O)C1OCC(O)C1O HVUMOYIDDBPOLL-UHFFFAOYSA-N 0.000 claims 1
- 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 claims 1
- 229920003171 Poly (ethylene oxide) Polymers 0.000 claims 1
- 150000001408 amides Chemical class 0.000 claims 1
- 239000003599 detergent Substances 0.000 claims 1
- NBVXSUQYWXRMNV-UHFFFAOYSA-N fluoromethane Chemical compound FC NBVXSUQYWXRMNV-UHFFFAOYSA-N 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
- 229910052708 sodium Inorganic materials 0.000 claims 1
- 239000011734 sodium Substances 0.000 claims 1
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 claims 1
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- NUJOXMJBOLGQSY-UHFFFAOYSA-N manganese dioxide Chemical compound O=[Mn]=O NUJOXMJBOLGQSY-UHFFFAOYSA-N 0.000 description 18
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- 235000007079 manganese sulphate Nutrition 0.000 description 4
- 239000011702 manganese sulphate Substances 0.000 description 4
- SQQMAOCOWKFBNP-UHFFFAOYSA-L manganese(II) sulfate Chemical compound [Mn+2].[O-]S([O-])(=O)=O SQQMAOCOWKFBNP-UHFFFAOYSA-L 0.000 description 4
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 description 4
- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 description 3
- 239000007864 aqueous solution Substances 0.000 description 3
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- ZHNUHDYFZUAESO-UHFFFAOYSA-N Formamide Chemical compound NC=O ZHNUHDYFZUAESO-UHFFFAOYSA-N 0.000 description 2
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 2
- MQRWBMAEBQOWAF-UHFFFAOYSA-N acetic acid;nickel Chemical compound [Ni].CC(O)=O.CC(O)=O MQRWBMAEBQOWAF-UHFFFAOYSA-N 0.000 description 2
- 229940011182 cobalt acetate Drugs 0.000 description 2
- QGUAJWGNOXCYJF-UHFFFAOYSA-N cobalt dinitrate hexahydrate Chemical compound O.O.O.O.O.O.[Co+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O QGUAJWGNOXCYJF-UHFFFAOYSA-N 0.000 description 2
- QAHREYKOYSIQPH-UHFFFAOYSA-L cobalt(II) acetate Chemical compound [Co+2].CC([O-])=O.CC([O-])=O QAHREYKOYSIQPH-UHFFFAOYSA-L 0.000 description 2
- SNRUBQQJIBEYMU-UHFFFAOYSA-N dodecane Chemical compound CCCCCCCCCCCC SNRUBQQJIBEYMU-UHFFFAOYSA-N 0.000 description 2
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 description 2
- 238000001027 hydrothermal synthesis Methods 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- VCJMYUPGQJHHFU-UHFFFAOYSA-N iron(3+);trinitrate Chemical compound [Fe+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O VCJMYUPGQJHHFU-UHFFFAOYSA-N 0.000 description 2
- 229910001416 lithium ion Inorganic materials 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 229940078494 nickel acetate Drugs 0.000 description 2
- 229920000128 polypyrrole Polymers 0.000 description 2
- 239000012266 salt solution Substances 0.000 description 2
- 238000003746 solid phase reaction Methods 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- TXUICONDJPYNPY-UHFFFAOYSA-N (1,10,13-trimethyl-3-oxo-4,5,6,7,8,9,11,12,14,15,16,17-dodecahydrocyclopenta[a]phenanthren-17-yl) heptanoate Chemical compound C1CC2CC(=O)C=C(C)C2(C)C2C1C1CCC(OC(=O)CCCCCC)C1(C)CC2 TXUICONDJPYNPY-UHFFFAOYSA-N 0.000 description 1
- ATRRKUHOCOJYRX-UHFFFAOYSA-N Ammonium bicarbonate Chemical compound [NH4+].OC([O-])=O ATRRKUHOCOJYRX-UHFFFAOYSA-N 0.000 description 1
- 229910000013 Ammonium bicarbonate Inorganic materials 0.000 description 1
- 241000790917 Dioxys <bee> Species 0.000 description 1
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 description 1
- 229910002651 NO3 Inorganic materials 0.000 description 1
- 229910003266 NiCo Inorganic materials 0.000 description 1
- 229910005949 NiCo2O4 Inorganic materials 0.000 description 1
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 1
- HVUMOYIDDBPOLL-XWVZOOPGSA-N Sorbitan monostearate Chemical compound CCCCCCCCCCCCCCCCCC(=O)OC[C@@H](O)[C@H]1OC[C@H](O)[C@H]1O HVUMOYIDDBPOLL-XWVZOOPGSA-N 0.000 description 1
- 229910021626 Tin(II) chloride Inorganic materials 0.000 description 1
- 229910021627 Tin(IV) chloride Inorganic materials 0.000 description 1
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 1
- DFGMFVYRMVYRRA-UHFFFAOYSA-N [O].CC Chemical compound [O].CC DFGMFVYRMVYRRA-UHFFFAOYSA-N 0.000 description 1
- 235000012538 ammonium bicarbonate Nutrition 0.000 description 1
- 239000001099 ammonium carbonate Substances 0.000 description 1
- YHWCPXVTRSHPNY-UHFFFAOYSA-N butan-1-olate;titanium(4+) Chemical compound [Ti+4].CCCC[O-].CCCC[O-].CCCC[O-].CCCC[O-] YHWCPXVTRSHPNY-UHFFFAOYSA-N 0.000 description 1
- 239000004202 carbamide Substances 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 229910000428 cobalt oxide Inorganic materials 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
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- 238000001035 drying Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005518 electrochemistry Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 238000003682 fluorination reaction Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- FBAFATDZDUQKNH-UHFFFAOYSA-M iron chloride Chemical compound [Cl-].[Fe] FBAFATDZDUQKNH-UHFFFAOYSA-M 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000003701 mechanical milling Methods 0.000 description 1
- 229910000000 metal hydroxide Inorganic materials 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- KBJMLQFLOWQJNF-UHFFFAOYSA-N nickel(ii) nitrate Chemical compound [Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O KBJMLQFLOWQJNF-UHFFFAOYSA-N 0.000 description 1
- IJRVLVIFMRWJRQ-UHFFFAOYSA-N nitric acid zinc Chemical compound [Zn].O[N+]([O-])=O IJRVLVIFMRWJRQ-UHFFFAOYSA-N 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 229910052755 nonmetal Inorganic materials 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000033116 oxidation-reduction process Effects 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 229920000056 polyoxyethylene ether Polymers 0.000 description 1
- 229940051841 polyoxyethylene ether Drugs 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 230000006798 recombination Effects 0.000 description 1
- 238000005215 recombination Methods 0.000 description 1
- 238000006479 redox reaction Methods 0.000 description 1
- 229910052703 rhodium Inorganic materials 0.000 description 1
- 239000010948 rhodium Substances 0.000 description 1
- MZSDGDXXBZSFTG-UHFFFAOYSA-M sodium;benzenesulfonate Chemical compound [Na+].[O-]S(=O)(=O)C1=CC=CC=C1 MZSDGDXXBZSFTG-UHFFFAOYSA-M 0.000 description 1
- 239000001119 stannous chloride Substances 0.000 description 1
- 235000011150 stannous chloride Nutrition 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
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- HPGGPRDJHPYFRM-UHFFFAOYSA-J tin(iv) chloride Chemical compound Cl[Sn](Cl)(Cl)Cl HPGGPRDJHPYFRM-UHFFFAOYSA-J 0.000 description 1
- 229910000349 titanium oxysulfate Inorganic materials 0.000 description 1
- 238000001132 ultrasonic dispersion Methods 0.000 description 1
- 238000002604 ultrasonography Methods 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
Classifications
-
- 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
-
- 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
- H01G11/32—Carbon-based
- H01G11/36—Nanostructures, e.g. nanofibres, nanotubes or fullerenes
-
- 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
-
- 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
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Abstract
The present invention provides a kind of mechanochemistry polymerizations to prepare graphene/metal oxide combination electrode material, it is characterized in that, the following steps are included: being added in mechanico-chemical reaction device using graphite and metal oxide precursor as raw material, graphene/metal oxide combination electrode material is obtained by a step mechanico-chemical reaction.Metal oxide precursor is poly functional reagent in the present invention, on the one hand it is as ion insertion agent, graphite removing is promoted to prepare graphene under mechanical force, on the other hand, metal salt is synchronous to occur mechanico-chemical reaction, in-situ preparation metal oxide on the surface of graphene, obtain graphene/metal oxide combination electrode material, to will prepare, graphene, multiple one steps of process such as metal oxide-loaded will be completed in situ, be simplified preparation flow and be improved graphene/metal oxide composite material preparation efficiency.
Description
Technical field
The invention belongs to field of composite material preparation, and in particular to graphene/metal oxidation is prepared in situ in mechanochemical reaction
Object combination electrode material.
Technical background
Along with the demands rapid growth such as electronic equipment such as mobile phone, electric tool, electric bus, electric car, make
With side to the energy storage device demand of high-energy density, high power density also rapid growth.Supercapacitor and traditional capacitor phase
Than there is relatively high energy density, having higher power density compared with battery is one of energy storage device of superior performance.It is super
Capacitor is divided into electric double layer energy-storage capacitor and two kinds of fake capacitance energy-storage capacitor, and wherein fake capacitance storage capacitor utilizes electrode material
Material surface oxidation reduction reaction can provide higher energy density by industry extensive concern.Lithium ion battery is also
A kind of energy storage device haveing excellent performance, because the characteristic with high-energy density has been favored by people.
Metal oxide has its excellent performance as energy storage material, such as redox reaction can occur and improve ratio
The ability etc. of reservoir lithium ion can be improved in capacitor, but they all have conductivity not high defect, and which prevent metal oxygens
The raising of compound energy-storage property.Since graphene has excellent electric conductivity and high-specific surface area, it is aoxidized with metal and is tied
Closing preparation graphene/metal oxide composite material is to obtain the feasible method of high-performance energy storage electrode material.Chinese patent [CN
102185139 A] graphene oxide is dispersed into nanoscale twins using ultrasonic dispersion and is sufficiently mixed with metal salt solution, it passes through
Nanometer metal oxide/graphene composite material is made after reduction, dry, calcining.This method wants previously prepared graphene oxide,
Then graphene oxide/metal oxide composite is mixed with metal salt then also needs by calcining reduction, entire mistake
When journey energy charge and not environmentally.Chinese invention patent [108022760 A of CN] first passes through electrolytic method and graphite is prepared
Then alkene mixes graphene with the mixing salt solution of rhodium ion, tin ion and cobalt ions, 220 DEG C~300 DEG C conditions after drying
Lower calcining, obtains graphene/metal oxide combination electrode material.This method needs to prepare graphene, and electrochemistry in advance
Preparing graphene has the disadvantages of process is complicated, and yield is small.Chinese invention patent [104701035 A of CN] first prepares graphite oxide
Alkene suspension stirs two kinds of substances respectively using nonmetal oxide, metal oxide and/or poly-metal deoxide as precursor
It mixes and moves into hydrothermal reaction kettle after mixing, kept for certain temperature a few hours obtain graphene/metal oxide combination electrode
Material.This method uses more expensive graphene oxide to be also unfavorable for large-scale production as raw material colleague's hydrothermal synthesis small scale.
Chinese invention patent [105719850 A of CN] first prepares graphene oxide and polypyrrole compound, then and before bimetal salt
It drives bluk recombination and graphene/polypyrrole/double-metal hydroxide combination electrode material is obtained by hydro-thermal.The above patented method all needs
Graphene is prepared separately, it is then compound with metal oxide precursor, the complex processes such as graphene are restored, graphite is unfavorable for
Alkene/metal oxide composite energy storage electrode material efficiently with the requirement of prepare with scale.
Summary of the invention
The present invention is to carry out to solve the above-mentioned problems, and it is an object of the present invention to provide stone is prepared in situ in a kind of mechanochemical reaction
It is more will to prepare graphene, dispersed graphite alkene and graphene-supported metal oxide etc. for black alkene/metal oxide composite electrode material
A one step of process is completed, and the preparation efficiency that preparation flow improves graphene/metal oxide composite material is simplified.
The present invention to achieve the goals above, uses following scheme:
The present invention provides a kind of mechanochemical reaction and graphene/metal oxide combination electrode material, feature is prepared in situ
It is, comprising the following steps: be added in mechanico-chemical reaction device, pass through using graphite and metal oxide precursor as raw material
One step mechanico-chemical reaction obtains graphene/metal oxide combination electrode material.
Preferably, graphene/metal oxide combination electrode material is prepared in situ in mechanochemical reaction provided by the invention, also
It can have following characteristics: in mechanico-chemical reaction, the applying mode of mechanical energy are as follows: ball milling, sand milling, grinding, extrusion, shearing
One or more of combination.Ball mill, double screw extruder, three rod grinders etc. can be used in mechanico-chemical reaction device.
Preferably, graphene/metal oxide combination electrode material is prepared in situ in mechanochemical reaction provided by the invention, also
Can have following characteristics: in mechanico-chemical reaction, the action time of mechanical energy is 0.5~12h.
Preferably, graphene/metal oxide combination electrode material is prepared in situ in mechanochemical reaction provided by the invention, also
Can have following characteristics: graphite is graphite oxide, artificial graphite, natural flake graphite, expanded graphite, amorphous graphite, fluorination
Any one in graphite, size is in 10~12000 mesh.
Preferably, graphene/metal oxide combination electrode material is prepared in situ in mechanochemical reaction provided by the invention, also
Can have following characteristics: metal oxide precursor is cobalt salt, manganese salt, nickel salt, molysite, zinc salt, any one in pink salt.
Preferably, graphene/metal oxide combination electrode material is prepared in situ in mechanochemical reaction provided by the invention, also
Can have following characteristics: metal oxide precursor is iron ion, manganese ion, nickel ion, cobalt ions, ruthenium ion, tin ion
Nitrate, acetate, any one in halogen.Such as metal oxide precursor may is that potassium permanganate, manganese sulfate,
Ferric nitrate, iron chloride, stannic chloride, titanyl sulfate, tetrabutyl titanate, cobalt nitrate hexahydrate, nickel nitrate, nickel acetate, cobalt acetate, nitric acid
Zinc etc..
Preferably, graphene/metal oxide combination electrode material is prepared in situ in mechanochemical reaction provided by the invention, also
Can have following characteristics: also comprising surfactant in raw material, and the surfactant is sodium lignin sulfonate, dodecane
Base benzene sulfonic acid sodium salt, kayexalate, stearic acid, gum arabic, polyvinyl alcohol, gathers at cetyltrimethylammonium bromide
Acrylamide, polyethylene glycol, seaweed glycolipid, hexadecyltrimethylammonium chloride, polyethylene oxide-polypropylene oxide-polycyclic oxygen
Ethane triblock copolymer (P123), Tween 80, polysorbate60, polysorbas20, span60, span85, span20, in polyether polyol
Any one.
Preferably, graphene/metal oxide combination electrode material is prepared in situ in mechanochemical reaction provided by the invention, also
Can have following characteristics: also comprising auxiliary agent in raw material, and the auxiliary agent is KOH, NaOH, NH4OH、NH4HCO3、NaCO3、
KClO4、KMnO4、K2Cr2O7、(NH4)2S2O8、K2S2O8At least one of.
It, can be in addition, graphene/metal oxide combination electrode material is prepared in situ in mechanochemical reaction provided by the invention
Using solid phase reaction, liquid phase reactor can also be used;When using solid phase reaction, do not need using solvent;When anti-using liquid phase
At once, solvent is preferably isopropanol, ethyl alcohol, methanol, acetone, methyl ethyl ketone, N-Methyl pyrrolidone, N, N- dimethyl in mixed liquor
At least one of formamide.
In addition, by graphene/metal oxide combination electrode material obtained by the above method, the quality hundred of graphene
Divide than being 5~40%.
The action and effect of invention
Graphene and metal oxide composite is prepared in situ in mechanochemical reaction proposed by the present invention, with metal oxide
Presoma is poly functional reagent, is on the one hand used as ion insertion agent, promotes graphite removing to prepare graphene under mechanical force,
On the other hand, metal salt is synchronous occurs mechanico-chemical reaction, and in-situ preparation metal oxide, obtains graphite on the surface of graphene
Alkene/metal oxide composite electrode material, to will prepare, graphene, multiple one steps of process such as metal oxide-loaded will be complete in situ
At simplifying preparation flow and improve graphene/metal oxide composite material preparation efficiency.This method process is simple, and
Combined coefficient height, stable product quality, safety and environmental protection, yield are high, are suitble to scale of mass production.
Detailed description of the invention
Fig. 1 is the graphene/manganese dioxide composite electrode material scanning electron microscope (SEM) prepared in the embodiment of the present invention one
Figure;
Fig. 2 is the graphene/manganese dioxide composite electrode material constant current charge-discharge song prepared in the embodiment of the present invention one
Line chart.
Specific embodiment
Graphene/metal oxide combination electrode is prepared in situ to mechanochemical reaction of the present invention below in conjunction with attached drawing
The specific embodiment of material is described in detail.
<embodiment one>
It is that graphene/manganese dioxide composite electrode material is prepared by mechanochemistry polymerization in the present embodiment one.
Preparation method:
(1) 100 mesh crystalline flake graphite 0.2g, 1.58g potassium permanganate are taken, 50mL deionized water is added to and is uniformly mixed, ultrasound
10min, as A liquid.
(2) it by 2.27g manganese sulfate, 0.5g Tween 80, is added in 50mL aqueous solution, 30min is stirred, as B liquid.
(3) A liquid is uniformly mixed with B liquid, 6h is handled using sand mill, revolving speed 2000rpm obtains mixture C.
(4) mixture C is washed repeatedly with deionized water, is filtered, then with ethanol washing, filtering, then dry in 80 DEG C of vacuum
It is dry for 24 hours, obtain graphene/manganese dioxide composite electrode material.
In the present embodiment one, using potassium permanganate and manganese sulfate as ion insertion agent, promote graphite in Mechanical Milling Process
Removing obtains graphene, meanwhile, mechanico-chemical reaction occurs for potassium permanganate and manganese sulfate, on the surface of graphene in-situ preparation dioxy
Change manganese, so that a step obtains graphene/manganese dioxide composite electrode material, then passes through heat treatment process, regulate and control manganese dioxide
Crystalline structure, improve chemical property.
Performance characterization:
By resulting graphene/manganese dioxide composite electrode material using scanning electron microscope shoot, pattern as shown in Figure 1,
It can be seen that graphene sheet layer is dispersed in manganese dioxide nano particle, conductive path can be formed inside electrode material, is mentioned
Rise the high rate performance of supercapacitor.
As shown in Fig. 2, graphene/manganese dioxide composite electrode material constant current charge-discharge curve shows ideal capacitor
Characteristic, the specific capacitance in 1A/g reach 315F/g, and when current density is increased to 10A/g, specific capacitance still retains 159F/
G, capacity retention 50.5%, embody superelevation specific capacitance and excellent high rate performance.
<embodiment two>
In the present embodiment two, graphene/tetra- cobalt oxide combination electrode materials are prepared by mechanochemistry polymerization, it is specific to wrap
Include following steps:
(1) 80 mesh artificial graphite 0.25g, cobalt nitrate hexahydrate 2.91g are taken, be added to 50mL ethanol water (volume ratio 1:
1) it is uniformly mixed in, ultrasonic 10min, as A liquid.
(2) 8g ammonium hydrogen carbonate, 2.5g polyoxyethylene ether are taken, is added in 50mL ethanol water (volume ratio 1:1), is stirred
30min, as B liquid.
(3) A liquid is uniformly mixed with B liquid, 2h, revolving speed 20000rpm, control reaction is handled using high speed shear dispersion machine
Temperature < 50 DEG C obtain mixture C.
(4) mixture C ionized water and ethyl alcohol washed repeatedly, filtered, then in 60 DEG C of vacuum drying 12h, answered
Close object D.
(5) compound D is transferred in tube furnace, handles 4h in 300 DEG C of air atmospheres, obtain graphene/tetra- cobalt oxides
Combination electrode material combination electrode material.
<embodiment three>
In the present embodiment three, graphene/NiCo is prepared by mechanochemistry polymerization2O4Combination electrode material combination electrode
Material specifically comprises the following steps:
(1) 325 mesh expanded graphite 0.5g, nickel acetate 1.77g, cobalt acetate 3.54g is taken to be uniformly mixed, as solid mixture
A。
(2) 1.2g sodium hydroxide is added into solid mixture A, is uniformly mixed, as solid mixture B.
(3) solid mixture B is transferred to closed in ball-grinding machine, solid phase mechanical ball mill reacts 6h, and revolving speed 300rpm obtains
To solid mixture C.
(4) solid mixture C deionized water and ethyl alcohol washed repeatedly, filtered, then in 60 DEG C of vacuum drying 12h,
Compound D is obtained,
(5) compound D is transferred in tube furnace, handles 4h in 350 DEG C of air atmospheres, obtains graphene/NiCo2O4It is multiple
Composite electrode material.
<example IV>
In the present embodiment four, graphene/stannic oxide combination electrode material is prepared by mechanochemistry polymerization, it is specific to wrap
Include following steps:
(1) 100 mesh graphite oxide 0.5g, stannous chloride 2.6g are taken, the n,N-Dimethylformamide solution of 50mL is added to
In aqueous solution (volume ratio 2:1), it is uniformly mixed, as A liquid,
(2) 10g urea, 0.5g seaweed glycolipid are taken, the n,N-Dimethylformamide solution aqueous solution (volume of 20mL is added to
Than 2:1) in, stirring 20min is uniformly mixed, as B liquid.
(3) A liquid is uniformly mixed with B liquid, handles 8h in three-roll grinder, revolving speed 50rpm obtains mixture C.
(4) mixture C deionized water, ethyl alcohol washed repeatedly, filtered, then answered in 80 DEG C of vacuum drying 10h
Close object D.
(5) compound D is transferred in tube furnace, is heat-treated 3h in 400 DEG C of inert gas atmospheres, obtain graphene/
Stannic oxide combination electrode material.
Above embodiments are only the illustration done to technical solution of the present invention.Mechanochemistry according to the present invention
Method is prepared in situ graphene/metal oxide combination electrode material and is not merely defined in described in the embodiment above
Hold, but is defined by the scope defined by the claims..Those skilled in the art of the invention are in the embodiment on the basis of institute
Any modify or supplement or equivalence replacement done, all in claim range claimed of the invention.
Claims (9)
1. graphene/metal oxide combination electrode material is prepared in situ in mechanochemical reaction, which is characterized in that including following step
It is rapid:
It is added in mechanico-chemical reaction device using graphite and metal oxide precursor as raw material, it is anti-by a step mechanochemistry
It should obtain graphene/metal oxide combination electrode material.
2. graphene/metal oxide combination electrode material is prepared in situ in mechanochemical reaction according to claim 1, special
Sign is:
Wherein, in the mechanico-chemical reaction, the applying mode of mechanical energy are as follows: ball milling, sand milling, grinding, extrusion, in shearing
One or more combination.
3. graphene/metal oxide combination electrode material is prepared in situ in mechanochemical reaction according to claim 1, special
Sign is:
Wherein, in the mechanico-chemical reaction, the action time of mechanical energy is 0.5~12h.
4. graphene/metal oxide combination electrode material is prepared in situ in mechanochemical reaction according to claim 1, special
Sign is:
Wherein, the mechanico-chemical reaction includes solid phase mechanico-chemical reaction and liquid phase mechanico-chemical reaction,
When using liquid phase mechanico-chemical reaction, reaction dissolvent is water, ethyl alcohol, methanol, acetone, isopropanol, N- crassitude
At least one of ketone, N,N-dimethylformamide.
5. graphene/metal oxide combination electrode material is prepared in situ in mechanochemical reaction according to claim 1, special
Sign is:
Wherein, the graphite is graphite oxide, artificial graphite, natural flake graphite, expanded graphite, amorphous graphite, fluorographite
In any one.
6. graphene/metal oxide combination electrode material is prepared in situ in mechanochemical reaction according to claim 1, special
Sign is:
Wherein, the metal oxide precursor is cobalt salt, manganese salt, nickel salt, molysite, zinc salt, any one in pink salt.
7. graphene/metal oxide combination electrode material is prepared in situ in mechanochemical reaction according to claim 1, special
Sign is:
Wherein, the metal oxide precursor is the nitre of iron ion, manganese ion, nickel ion, cobalt ions, ruthenium ion, tin ion
Hydrochlorate, acetate, any one in halogen.
8. graphene/metal oxide combination electrode material is prepared in situ in mechanochemical reaction according to claim 1, special
Sign is:
It wherein, also include surfactant in the raw material, and the surfactant is sodium lignin sulfonate, detergent alkylate
Sodium sulfonate, cetyltrimethylammonium bromide, kayexalate, stearic acid, gum arabic, polyvinyl alcohol, polypropylene
Amide, polyethylene glycol, seaweed glycolipid, hexadecyltrimethylammonium chloride, polyethylene oxide-polypropylene oxide-polyethylene oxide
It is triblock copolymer, Tween 80, polysorbate60, polysorbas20, sorbester p18, span 85, span 20, any one in polyether polyol
Kind.
9. graphene/metal oxide combination electrode material is prepared in situ in mechanochemical reaction according to claim 1, special
Sign is:
It wherein, also include auxiliary agent in the raw material, and the auxiliary agent is KOH, NaOH, NH4OH、NH4HCO3、NaCO3、KClO4、
KMnO4、K2Cr2O7、(NH4)2S2O8、K2S2O8At least one of.
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Application publication date: 20190115 |
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