CN116453877A - Super capacitor electrode material and preparation method thereof - Google Patents
Super capacitor electrode material and preparation method thereof Download PDFInfo
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- CN116453877A CN116453877A CN202310658796.9A CN202310658796A CN116453877A CN 116453877 A CN116453877 A CN 116453877A CN 202310658796 A CN202310658796 A CN 202310658796A CN 116453877 A CN116453877 A CN 116453877A
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- 238000002360 preparation method Methods 0.000 title claims abstract description 83
- 239000007772 electrode material Substances 0.000 title claims abstract description 60
- 239000003990 capacitor Substances 0.000 title abstract description 31
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical class [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 182
- 239000011259 mixed solution Substances 0.000 claims abstract description 99
- 239000000243 solution Substances 0.000 claims abstract description 82
- 238000002156 mixing Methods 0.000 claims abstract description 69
- 239000002244 precipitate Substances 0.000 claims abstract description 63
- 239000002114 nanocomposite Substances 0.000 claims abstract description 45
- 239000004020 conductor Substances 0.000 claims abstract description 38
- 239000002270 dispersing agent Substances 0.000 claims abstract description 38
- 229910052723 transition metal Inorganic materials 0.000 claims abstract description 34
- 238000000034 method Methods 0.000 claims abstract description 32
- 238000005406 washing Methods 0.000 claims abstract description 32
- 150000003624 transition metals Chemical class 0.000 claims abstract description 31
- 239000000853 adhesive Substances 0.000 claims abstract description 25
- 230000001070 adhesive effect Effects 0.000 claims abstract description 25
- 238000001035 drying Methods 0.000 claims abstract description 24
- 238000001914 filtration Methods 0.000 claims abstract description 23
- 239000007864 aqueous solution Substances 0.000 claims abstract description 20
- 239000012670 alkaline solution Substances 0.000 claims abstract description 11
- 239000003929 acidic solution Substances 0.000 claims abstract description 8
- 230000001590 oxidative effect Effects 0.000 claims abstract description 4
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 93
- 239000003575 carbonaceous material Substances 0.000 claims description 42
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 42
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 26
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 24
- 239000008367 deionised water Substances 0.000 claims description 18
- 229910021641 deionized water Inorganic materials 0.000 claims description 18
- WMFOQBRAJBCJND-UHFFFAOYSA-M Lithium hydroxide Chemical compound [Li+].[OH-] WMFOQBRAJBCJND-UHFFFAOYSA-M 0.000 claims description 15
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 12
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 11
- 230000003213 activating effect Effects 0.000 claims description 11
- 239000011229 interlayer Substances 0.000 claims description 11
- 229910017604 nitric acid Inorganic materials 0.000 claims description 11
- 238000010000 carbonizing Methods 0.000 claims description 10
- 230000004913 activation Effects 0.000 claims description 9
- 239000002006 petroleum coke Substances 0.000 claims description 7
- 239000012298 atmosphere Substances 0.000 claims description 6
- 239000000463 material Substances 0.000 claims description 6
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 5
- 239000002253 acid Substances 0.000 claims description 5
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 4
- 230000001681 protective effect Effects 0.000 claims description 4
- 238000004519 manufacturing process Methods 0.000 claims description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N ammonia Natural products N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 2
- 229910052786 argon Inorganic materials 0.000 claims description 2
- 238000003763 carbonization Methods 0.000 claims description 2
- 239000011335 coal coke Substances 0.000 claims description 2
- 229910052737 gold Inorganic materials 0.000 claims description 2
- 238000000227 grinding Methods 0.000 claims description 2
- 238000010438 heat treatment Methods 0.000 claims description 2
- 229910052751 metal Inorganic materials 0.000 claims description 2
- 239000002184 metal Substances 0.000 claims description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N nitrogen Substances N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 2
- 229910052757 nitrogen Inorganic materials 0.000 claims description 2
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 claims description 2
- 239000000126 substance Substances 0.000 claims description 2
- 229910052719 titanium Inorganic materials 0.000 claims description 2
- 229910052720 vanadium Inorganic materials 0.000 claims description 2
- 239000011300 coal pitch Substances 0.000 claims 1
- 239000011301 petroleum pitch Substances 0.000 claims 1
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 32
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical group CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 28
- 238000000498 ball milling Methods 0.000 description 25
- DNIAPMSPPWPWGF-UHFFFAOYSA-N Propylene glycol Chemical group CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 description 24
- 239000012153 distilled water Substances 0.000 description 24
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 17
- 239000010426 asphalt Substances 0.000 description 16
- 230000008569 process Effects 0.000 description 16
- 239000003208 petroleum Substances 0.000 description 15
- 239000011230 binding agent Substances 0.000 description 13
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical group CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 12
- -1 activated carbon-copper hydroxide Chemical class 0.000 description 10
- 239000012300 argon atmosphere Substances 0.000 description 9
- 239000003513 alkali Substances 0.000 description 8
- 238000011068 loading method Methods 0.000 description 8
- 229910052759 nickel Inorganic materials 0.000 description 8
- 230000005540 biological transmission Effects 0.000 description 7
- 230000000536 complexating effect Effects 0.000 description 7
- 239000012299 nitrogen atmosphere Substances 0.000 description 7
- PHFQLYPOURZARY-UHFFFAOYSA-N chromium trinitrate Chemical compound [Cr+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O PHFQLYPOURZARY-UHFFFAOYSA-N 0.000 description 6
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 description 6
- ONDPHDOFVYQSGI-UHFFFAOYSA-N zinc nitrate Chemical compound [Zn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O ONDPHDOFVYQSGI-UHFFFAOYSA-N 0.000 description 6
- 239000004372 Polyvinyl alcohol Substances 0.000 description 5
- 239000006230 acetylene black Substances 0.000 description 5
- 239000000203 mixture Substances 0.000 description 5
- 229920002451 polyvinyl alcohol Polymers 0.000 description 5
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical group CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 4
- 235000011114 ammonium hydroxide Nutrition 0.000 description 4
- 239000002131 composite material Substances 0.000 description 4
- YBCAZPLXEGKKFM-UHFFFAOYSA-K ruthenium(iii) chloride Chemical compound [Cl-].[Cl-].[Cl-].[Ru+3] YBCAZPLXEGKKFM-UHFFFAOYSA-K 0.000 description 4
- 229910003771 Gold(I) chloride Inorganic materials 0.000 description 3
- AZFUOHYXCLYSQJ-UHFFFAOYSA-N [V+5].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O Chemical compound [V+5].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O AZFUOHYXCLYSQJ-UHFFFAOYSA-N 0.000 description 3
- 229910052799 carbon Inorganic materials 0.000 description 3
- 229940116318 copper carbonate Drugs 0.000 description 3
- 229910000365 copper sulfate Inorganic materials 0.000 description 3
- ARUVKPQLZAKDPS-UHFFFAOYSA-L copper(II) sulfate Chemical compound [Cu+2].[O-][S+2]([O-])([O-])[O-] ARUVKPQLZAKDPS-UHFFFAOYSA-L 0.000 description 3
- GEZOTWYUIKXWOA-UHFFFAOYSA-L copper;carbonate Chemical compound [Cu+2].[O-]C([O-])=O GEZOTWYUIKXWOA-UHFFFAOYSA-L 0.000 description 3
- FDWREHZXQUYJFJ-UHFFFAOYSA-M gold monochloride Chemical compound [Cl-].[Au+] FDWREHZXQUYJFJ-UHFFFAOYSA-M 0.000 description 3
- YPJCVYYCWSFGRM-UHFFFAOYSA-H iron(3+);tricarbonate Chemical compound [Fe+3].[Fe+3].[O-]C([O-])=O.[O-]C([O-])=O.[O-]C([O-])=O YPJCVYYCWSFGRM-UHFFFAOYSA-H 0.000 description 3
- 230000003647 oxidation Effects 0.000 description 3
- 238000007254 oxidation reaction Methods 0.000 description 3
- GPNDARIEYHPYAY-UHFFFAOYSA-N palladium(ii) nitrate Chemical compound [Pd+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O GPNDARIEYHPYAY-UHFFFAOYSA-N 0.000 description 3
- NWAHZABTSDUXMJ-UHFFFAOYSA-N platinum(2+);dinitrate Chemical compound [Pt+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O NWAHZABTSDUXMJ-UHFFFAOYSA-N 0.000 description 3
- 229920002037 poly(vinyl butyral) polymer Polymers 0.000 description 3
- 239000002243 precursor Substances 0.000 description 3
- 229910001961 silver nitrate Inorganic materials 0.000 description 3
- 229920002134 Carboxymethyl cellulose Polymers 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 2
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical group CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 description 2
- 239000004962 Polyamide-imide Substances 0.000 description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 2
- 239000006229 carbon black Substances 0.000 description 2
- 239000001768 carboxy methyl cellulose Substances 0.000 description 2
- 235000010948 carboxy methyl cellulose Nutrition 0.000 description 2
- 239000008112 carboxymethyl-cellulose Substances 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 239000011294 coal tar pitch Substances 0.000 description 2
- 229940044175 cobalt sulfate Drugs 0.000 description 2
- 229910000361 cobalt sulfate Inorganic materials 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
- 238000010668 complexation reaction Methods 0.000 description 2
- 238000002484 cyclic voltammetry Methods 0.000 description 2
- 239000003792 electrolyte Substances 0.000 description 2
- 239000010410 layer Substances 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-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
- 229920002312 polyamide-imide Polymers 0.000 description 2
- 229920000049 Carbon (fiber) Polymers 0.000 description 1
- 239000006245 Carbon black Super-P Substances 0.000 description 1
- 239000002033 PVDF binder Substances 0.000 description 1
- 239000004642 Polyimide Substances 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- DAAILNBDLGFGKZ-UHFFFAOYSA-H [C+4].[Mn+2].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-] Chemical compound [C+4].[Mn+2].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-] DAAILNBDLGFGKZ-UHFFFAOYSA-H 0.000 description 1
- QGDZMJQHTGPRTF-UHFFFAOYSA-G [C+4].[OH-].[Cr+3].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-] Chemical compound [C+4].[OH-].[Cr+3].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-] QGDZMJQHTGPRTF-UHFFFAOYSA-G 0.000 description 1
- OPOUVFMXMOZJMT-UHFFFAOYSA-H [C+4].[OH-].[Zn+2].[OH-].[OH-].[OH-].[OH-].[OH-] Chemical compound [C+4].[OH-].[Zn+2].[OH-].[OH-].[OH-].[OH-].[OH-] OPOUVFMXMOZJMT-UHFFFAOYSA-H 0.000 description 1
- UMAHOFNLHNWTDQ-UHFFFAOYSA-L [C].[Co](O)O Chemical compound [C].[Co](O)O UMAHOFNLHNWTDQ-UHFFFAOYSA-L 0.000 description 1
- SAJUROZXXGFMST-UHFFFAOYSA-L [C].[Pt](O)O Chemical compound [C].[Pt](O)O SAJUROZXXGFMST-UHFFFAOYSA-L 0.000 description 1
- NOBRBSQQPRMXME-UHFFFAOYSA-L [Ni](O)O.[C] Chemical class [Ni](O)O.[C] NOBRBSQQPRMXME-UHFFFAOYSA-L 0.000 description 1
- OFWZYGUVWGHBMB-UHFFFAOYSA-F [OH-].[Ti+4].[C+4].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-] Chemical compound [OH-].[Ti+4].[C+4].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-] OFWZYGUVWGHBMB-UHFFFAOYSA-F 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- 229910021383 artificial graphite Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000004917 carbon fiber Substances 0.000 description 1
- 239000003245 coal Substances 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- ZOMNIUBKTOKEHS-UHFFFAOYSA-L dimercury dichloride Chemical class Cl[Hg][Hg]Cl ZOMNIUBKTOKEHS-UHFFFAOYSA-L 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 229960004887 ferric hydroxide Drugs 0.000 description 1
- 239000011888 foil Substances 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 239000003273 ketjen black Substances 0.000 description 1
- UKVIEHSSVKSQBA-UHFFFAOYSA-N methane;palladium Chemical class C.[Pd] UKVIEHSSVKSQBA-UHFFFAOYSA-N 0.000 description 1
- 229910021382 natural graphite Inorganic materials 0.000 description 1
- 239000011295 pitch Substances 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 229920000191 poly(N-vinyl pyrrolidone) Polymers 0.000 description 1
- 229920001721 polyimide Polymers 0.000 description 1
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 1
- 239000004810 polytetrafluoroethylene Substances 0.000 description 1
- 229920002981 polyvinylidene fluoride Polymers 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- RUOJZAUFBMNUDX-UHFFFAOYSA-N propylene carbonate Chemical compound CC1COC(=O)O1 RUOJZAUFBMNUDX-UHFFFAOYSA-N 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 230000002441 reversible effect Effects 0.000 description 1
- 229920003048 styrene butadiene rubber Polymers 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/84—Processes for the manufacture of hybrid or EDL capacitors, or components thereof
- H01G11/86—Processes for the manufacture of hybrid or EDL capacitors, or components thereof specially adapted for electrodes
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- 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 OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
- H01G11/32—Carbon-based
- H01G11/34—Carbon-based characterised by carbonisation or activation 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 application discloses a supercapacitor electrode material and a preparation method thereof, wherein the preparation method of the supercapacitor electrode material comprises the following steps: s1, preparing porous activated carbon powder; s2, oxidizing the porous activated carbon powder in an acidic solution; s3, adding the transition metal aqueous solution into the oxidized porous activated carbon solution to prepare a mixed solution; s4, alkaline solution is dripped into the mixed solution; s5, filtering the mixed solution to obtain a precipitate, and washing and drying the precipitate to obtain the nanocomposite; and S6, mixing the nanocomposite, the conductive material, the adhesive and the dispersing agent to prepare the supercapacitor electrode material. The electrode material prepared by the method is applied to the super capacitor, and the volume specific capacitance of the super capacitor is higher than 21F/cc.
Description
Technical Field
The application relates to the technical field of supercapacitors, in particular to a supercapacitor electrode material and a preparation method thereof.
Background
Supercapacitors are extremely large capacity capacitors with capacitances up to thousands of farads. Taking the super capacitor of Cooper company in us as an example, the capacitance depends on the inter-electrode distance and the electrode surface area according to the principle of the capacitor, in order to obtain such a large capacitance, the inter-electrode distance of the super capacitor is reduced as much as possible, and the electrode surface area is increased, so that the super capacitor comprises two electrodes, an anode and a cathode, and a porous separator interposed between the two electrodes using the principle of electric double layer and the active carbon porous electrode.
The electrode active material is a key factor influencing the performance of the super capacitor, and the specific surface area of the currently marketed active carbon electrode material is not more than 200m 2 However, with expansion of the application field of the supercapacitor, the electrode active material currently on the market is difficult to better meet the use requirement, so that development of an electrode material with larger specific surface area and larger volume specific capacitance is needed.
Disclosure of Invention
In order to solve at least one technical problem, a preparation process of an electrode material with larger specific surface area and larger volume specific capacitance is developed.
In one aspect, the preparation method of the supercapacitor electrode material provided by the application comprises the following steps:
s1, preparing porous activated carbon powder, wherein the specific surface area of the porous activated carbon powder is 300-1300 m 2 And/g, wherein the average interlayer spacing of the porous activated carbon powder is 3.385-4.445 nm;
s2, oxidizing the porous activated carbon powder in an acid solution to obtain an oxidized porous activated carbon solution;
s3, adding the transition metal aqueous solution into the oxidized porous activated carbon solution to prepare a mixed solution;
s4, dripping the alkaline solution into the mixed solution, and adjusting the pH value of the mixed solution to 8-12 to separate out a precipitate in the mixed solution;
s5, filtering the mixed solution to obtain a precipitate, and washing and drying the precipitate to obtain the nanocomposite;
s6, mixing the nanocomposite, the conductive material, the adhesive and the dispersing agent according to the weight ratio of 10: (0.2-2): (0.2-2): (0.1-30) and mixing to obtain the supercapacitor electrode material.
By adopting the technical scheme, the specific surface area of the porous activated carbon powder prepared by the method is 300-1300 m 2 The specific surface is larger, the average interlayer spacing of the prepared porous activated carbon powder is 3.385-4.445 nm, and the average interlayer spacing is smaller and reaches the nanometer level; the porous activated carbon powder with larger specific surface and smaller average interlayer spacing is subjected to oxidation treatment in an acid solution, so that the complexing of the porous activated carbon powder and transition metal hydroxide can be promoted; adding a transition metal aqueous solution into an oxidized porous activated carbon solution, taking transition metal as a transition metal hydroxide precursor, along with dripping of an alkaline solution, complexing porous activated carbon powder with the transition metal hydroxide to form a precipitate, filtering, washing and drying to obtain a nanocomposite composited by complexing porous activated carbon-transition metal hydroxide, mixing the nanocomposite with a conductive material, an adhesive and a dispersing agent according to a specific proportion to prepare a super capacitor electrode material, and adopting the super capacitor electrode material to prepare an anode and a cathode, wherein the volume specific capacitance of the formed super capacitor is higher than 21F/cc.
Optionally, in the step S1, the preparation method of the porous activated carbon powder includes the following steps:
step one, carbonizing a carbon material under the condition of atmosphere protection;
step two, activating the carbonized carbon material;
and thirdly, washing and drying the activated carbon material to obtain the porous activated carbon powder.
By adopting the technical scheme, the porous activated carbon powder prepared by the methodHas a specific surface area of 300 to 1300m 2 And/g, the average interlayer spacing is 3.385-4.445 nm.
Optionally, in the first step, the protective atmosphere is nitrogen or argon, and the carbonization treatment temperature is 550-900 ℃.
By adopting the technical scheme, the carbon material can be carbonized better.
Optionally, in the first step, the carbon material is selected from one of petroleum asphalt, coal asphalt, petroleum coke and coal coke.
Optionally, in the second step, the activating treatment is performed in the following manner: the carbonized carbon material and potassium hydroxide or sodium hydroxide are mixed according to the weight ratio of 1: (1-5) mixing, grinding, and heating for 0.16-12 hours in a protective atmosphere at 600-900 ℃ to obtain the activated carbon material.
By adopting the technical scheme, the carbon material has more holes and a corresponding specific surface area.
Optionally, in the step S2, the weight of the porous activated carbon powder is 0.1-0.3 g, the volume of the acidic solution is 20-40 ml, the molar concentration of the acidic solution is 0.1-5 mol/L, and the acidic solution is one selected from nitric acid, hydrochloric acid and sulfuric acid.
By adopting the technical scheme, the complexation of the porous activated carbon powder and the transition metal hydroxide can be effectively improved.
Optionally, in the step S3, the addition amount of the transition metal aqueous solution is 1-5 ml, and the volume molar concentration of the transition metal aqueous solution is 0.1-5 mol/L.
Optionally, in the step S3, the preparation method of the transition metal aqueous solution includes: dissolving a transition metal source in deionized water, wherein the transition metal source has a chemical formula of M (NO 3 ) n ，M(CO 3 ) n/2 ，M(SO 4 ) n/2 Or MCl n Wherein M is selected from one of Ti, V, cr, mn, fe, co, ni, cu, cd, zn, ru, pd, ag, pt and Au, and the value of n is matched with the valence of the metal M.
Optionally, in the step S4, the alkaline solution is selected from one of an aqueous lithium hydroxide solution, an aqueous sodium hydroxide solution, an aqueous potassium hydroxide solution or aqueous ammonia, and the volume molar concentration of the alkaline solution is 0.1-10 mol/L.
By adopting the technical scheme, the porous activated carbon powder can be fully complexed with the transition metal hydroxide to form a precipitate.
In a second aspect, the present application provides an electrode material prepared by the method for preparing an electrode material of a supercapacitor.
By adopting the technical scheme, the anode and the cathode are manufactured by adopting the super capacitor electrode material, and the volume specific capacitance of the formed super capacitor is higher than 21F/cc.
In summary, the present invention includes at least one of the following beneficial technical effects:
1. the super capacitor electrode material is used for manufacturing an anode and a cathode, and is applied to a super capacitor, and the volume specific capacitance of the super capacitor is higher than 21F/cc.
2. The specific surface area of the porous activated carbon powder prepared by the method is 300-1300 m 2 And/g, the average interlayer spacing is 3.385-4.445 nm.
3. The porous activated carbon powder is subjected to oxidation treatment in an acidic solution, so that complexation of the porous activated carbon powder and transition metal hydroxide can be promoted.
4. The application adds the transition metal aqueous solution into the oxidized porous activated carbon solution, takes the transition metal source as a precursor of the transition metal hydroxide, and along with the dropping of the alkaline solution, the porous activated carbon powder can be more fully complexed with the transition metal hydroxide to form a precipitate, and then the nano composite material synthesized by complexing the porous activated carbon-transition metal hydroxide can be obtained after filtration, washing and drying treatment.
Drawings
FIG. 1 is a high resolution transmission electron microscope (HR-TEM) image of the carbonized carbon material produced in preparation example 1;
FIG. 2 is a high resolution transmission electron microscope (HR-TEM) image of the porous activated carbon powder prepared in preparation example 1;
FIG. 3 is a high resolution transmission electron microscope (HR-TEM) image of the nanocomposite obtained in preparation example 9;
FIG. 4 is a high resolution transmission electron microscope (HR-TEM) image of the nanocomposite obtained in preparation example 9;
fig. 5 is a cyclic voltammogram of the electrode current values for a three-electrode cell made from the electrode material of example 1 while maintaining a constant potential scan rate change over a constant potential window.
Detailed Description
The present application is described in further detail below with reference to the drawings and examples.
The application designs a supercapacitor electrode material and a preparation method thereof.
The supercapacitor electrode material is prepared by the following method, and comprises the following steps:
s1, preparing porous activated carbon powder, wherein the specific surface area of the porous activated carbon powder is 300-1300 m 2 And/g, wherein the average interlayer spacing of the porous activated carbon powder is 3.385-4.445 nm;
s2, oxidizing the porous activated carbon powder in an acid solution to obtain an oxidized porous activated carbon solution;
s3, adding the transition metal aqueous solution into the porous activated carbon solution to prepare a mixed solution;
s4, dripping the alkaline solution into the mixed solution, and adjusting the pH value of the mixed solution to 8-12 to separate out a precipitate in the mixed solution;
s5, filtering the mixed solution to obtain a precipitate, and washing and drying the precipitate to obtain the nanocomposite;
s6, mixing the nanocomposite, the conductive material, the adhesive and the dispersing agent according to the weight ratio of 10: (0.2-2): (0.2-2): (0.1-30) and mixing to obtain the supercapacitor electrode material.
The supercapacitor electrode material can be applied to the field of supercapacitors.
The specific surface area of the porous activated carbon powder prepared by the method is 300-1300 m 2 The specific surface is larger, the average interlayer spacing of the prepared porous activated carbon powder is 3.385-4.445 nm, and the average interlayer spacing is smaller and reaches the nanometer level; the porous activated carbon powder with larger specific surface and smaller average interlayer spacing is subjected to oxidation treatment in an acid solution, so that the complexing of the porous activated carbon powder and transition metal hydroxide can be promoted; adding a transition metal aqueous solution into an oxidized porous activated carbon solution, taking transition metal as a transition metal hydroxide precursor, along with dripping of an alkaline solution, complexing porous activated carbon powder with the transition metal hydroxide to form a precipitate, filtering, washing and drying to obtain a nanocomposite composited by complexing porous activated carbon-transition metal hydroxide, mixing the nanocomposite with a conductive material, an adhesive and a dispersing agent according to a specific proportion, and preparing the super capacitor electrode material, wherein the volume specific capacitance of the formed super capacitor is higher than 21F/cc by adopting the super capacitor electrode material for electrode preparation.
Examples
Preparation examples 1 to 8 are preparation of porous activated carbon powder
Preparation example 1
Carbonizing 2kg of petroleum asphalt in a nitrogen atmosphere at 600 ℃ for 2 hours to obtain carbonized carbon material, wherein the petroleum asphalt has 18% of asphaltene content and 46% of oil content; high resolution transmission electron microscope (HR-TEM) pictures of carbonized carbon materials are shown in FIG. 1;
the carbonized carbon material and potassium hydroxide are mixed according to the weight ratio of 1:4, mixing, crushing by using a dry ball milling process, wherein zirconia balls are used in the ball milling process, the average diameter of the zirconia balls is 5mm, the rotating speed of the ball mill is 100rpm, and the ball milling time is 2 hours;
loading the ball-milled carbon material and potassium hydroxide into a nickel reactor, and activating the carbon material and potassium hydroxide for 2 hours in an argon atmosphere at 900 ℃;
after the activation treatment, the alkali component was neutralized with hydrochloric acid having a volume molar concentration of 0.1mol/L, and washed 5 times with distilled water, and after washing, dried at 150℃for 24 hours, a porous activated carbon powder was obtained for use, and a high resolution transmission electron microscope (HR-TEM) photograph of the porous activated carbon powder was shown in FIG. 2.
Preparation example 2
Carbonizing 2kg of petroleum asphalt in an argon atmosphere at 550 ℃ for 2 hours to obtain carbonized carbon material, wherein the petroleum asphalt is the same as the petroleum asphalt in preparation example 1;
the carbonized carbon material and potassium hydroxide are mixed according to the weight ratio of 1:5, mixing, crushing by using a dry ball milling process, wherein zirconia balls are used in the ball milling process, the average diameter of the zirconia balls is 5mm, the rotating speed of the ball mill is 110rpm, and the ball milling time is 10 hours;
loading the ball-milled carbon material and potassium hydroxide into a nickel reactor, and activating for 5 hours in an argon atmosphere at 800 ℃;
after the activation treatment, the alkali component was neutralized with hydrochloric acid having a volume molar concentration of 0.1mol/L, and washed with distilled water 4 times, and after washing, dried at 160℃for 20 hours, to obtain a porous activated carbon powder for use.
Preparation example 3
Carbonizing 2kg of petroleum asphalt in a nitrogen atmosphere at 650 ℃ for 2 hours to obtain carbonized carbon material, wherein the petroleum asphalt is the same as the petroleum asphalt in preparation example 1;
the carbonized carbon material and potassium hydroxide are mixed according to the weight ratio of 1:3, mixing, crushing by using a dry ball milling process, wherein zirconia balls are used in the ball milling process, the average diameter of the zirconia balls is 5mm, the rotating speed of the ball mill is 120rpm, and the ball milling time is 17 hours;
loading the ball-milled carbon material and potassium hydroxide into a nickel reactor, and activating the carbon material and potassium hydroxide for 4 hours in an argon atmosphere at 600 ℃;
after the activation treatment, the alkali component was neutralized with nitric acid having a volume molar concentration of 0.1mol/L, and washed 5 times with distilled water, and after washing, dried at 120℃for 24 hours, to obtain a porous activated carbon powder for use.
Preparation example 4
Carbonizing 2kg of petroleum asphalt in a nitrogen atmosphere at 700 ℃ for 2 hours to obtain carbonized carbon material, wherein the petroleum asphalt is the same as the petroleum asphalt in preparation example 1;
the carbonized carbon material and potassium hydroxide are mixed according to the weight ratio of 1:4, mixing, crushing by using a dry ball milling process, wherein zirconia balls are used in the ball milling process, the average diameter of the zirconia balls is 4.8mm, the rotating speed of the ball mill is 130rpm, and the ball milling time is 25 hours;
loading the ball-milled carbon material and potassium hydroxide into a nickel reactor, and activating the carbon material and potassium hydroxide for 8 hours in an argon atmosphere at the temperature of 850 ℃;
after the activation treatment, the alkali component was neutralized with nitric acid having a volume molar concentration of 0.1mol/L, and washed 5 times with distilled water, and after washing, dried at 150℃for 20 hours, to obtain a porous activated carbon powder for use.
Preparation example 5
Carbonizing 2kg of petroleum asphalt in a nitrogen atmosphere at 750 ℃ for 2 hours to obtain carbonized carbon material, wherein the petroleum asphalt is the same as the petroleum asphalt in preparation example 1;
the carbonized carbon material and potassium hydroxide are mixed according to the weight ratio of 1:1, mixing, crushing by using a dry ball milling process, wherein zirconia balls are used in the ball milling process, the average diameter of the zirconia balls is 4.5mm, the rotating speed of the ball mill is 150rpm, and the ball milling time is 31 hours;
loading the ball-milled carbon material and potassium hydroxide into a nickel reactor, and activating the carbon material and potassium hydroxide for 3 hours in an argon atmosphere at the temperature of 700 ℃;
after the activation treatment, the alkali component was neutralized with hydrochloric acid having a volume molar concentration of 0.1mol/L, and washed with distilled water 6 times, and after washing, dried at 150℃for 18 hours, to obtain a porous activated carbon powder for use.
Preparation example 6
Carbonizing 2kg coal tar pitch in nitrogen atmosphere at 800 ℃ for 2 hours to obtain carbonized carbon material, wherein the coal tar pitch is medium-temperature pitch No. 1;
the carbonized carbon material and sodium hydroxide are mixed according to the weight ratio of 1:2, mixing, crushing by using a dry ball milling process, wherein zirconia balls are used in the ball milling process, the average diameter of the zirconia balls is 4.2mm, the rotating speed of the ball mill is 140rpm, and the ball milling time is 37 hours;
loading the ball-milled carbon material and potassium hydroxide into a nickel reactor, and activating the carbon material and potassium hydroxide for 12 hours in an argon atmosphere at 750 ℃;
after the activation treatment, the alkali component was neutralized with hydrochloric acid having a volume molar concentration of 0.1mol/L, and washed with distilled water 5 times, and after washing, dried at 130℃for 22 hours, to obtain a porous activated carbon powder for use.
Preparation example 7
Carbonizing 2kg of petroleum coke in a nitrogen atmosphere at 850 ℃ for 2 hours to obtain carbonized carbon material, wherein the carbon content in the petroleum coke is 90wt%;
the carbonized carbon material and potassium hydroxide are mixed according to the weight ratio of 1:4, mixing, crushing by using a dry ball milling process, wherein zirconia balls are used in the ball milling process, the average diameter of the zirconia balls is 3.9mm, the rotating speed of the ball mill is 150rpm, and the ball milling time is 44 hours;
loading the carbon material after ball milling and potassium hydroxide into a nickel reactor, and activating for 10 hours in an argon atmosphere at the temperature of 650 ℃;
after the activation treatment, the alkali component was neutralized with hydrochloric acid having a volume molar concentration of 0.1mol/L, and washed with distilled water 5 times, and after washing, dried at 150℃for 24 hours, to obtain a porous activated carbon powder for use.
Preparation example 8
Carbonizing 2kg of petroleum coke in a nitrogen atmosphere at 900 ℃ for 2 hours to obtain carbonized carbon material, wherein the petroleum coke is the same as the petroleum coke in preparation example 7;
the carbonized carbon material and potassium hydroxide are mixed according to the weight ratio of 1:4, mixing, crushing by using a dry ball milling process, wherein zirconia balls are used in the ball milling process, the average diameter of the zirconia balls is 3.5mm, the rotating speed of the ball mill is 150rpm, and the ball milling time is 50 hours;
loading the ball-milled carbon material and potassium hydroxide into a nickel reactor, and activating the carbon material and potassium hydroxide for 7 hours in an argon atmosphere at the temperature of 850 ℃;
after the activation treatment, the alkali component was neutralized with hydrochloric acid having a volume molar concentration of 0.1mol/L, and washed with distilled water 4 times, and after washing, dried at 150℃for 24 hours, to obtain a porous activated carbon powder for use.
The specific surface areas and the average layer spacing of the porous activated carbon powders obtained in preparation examples 1 to 8 are shown in the following table 1.
TABLE 1
Preparation examples 9 to 24 are preparation of nanocomposite materials
Preparation example 9
Mixing 0.2g of the porous activated carbon powder prepared in preparation example 1 with 30ml of nitric acid with a volume molar concentration of 1mol/L to oxidize the porous activated carbon powder to obtain an oxidized porous activated carbon solution;
ni (NO) 3 ) 2 Dissolving in deionized water to obtain nickel nitrate solution with volume molar concentration of 1mol/L, mixing 3ml of nickel nitrate solution with the oxidized porous activated carbon solution to prepare a mixed solution;
dripping a potassium hydroxide aqueous solution with the volume molar concentration of 1mol/L into the mixed solution, adjusting the pH value of the mixed solution to 10, and separating out an activated carbon-nickel hydroxide precipitate from the mixed solution;
the mixed solution was subjected to filtration treatment to separate out a precipitate, the precipitate was washed 5 times with distilled water, and then dried at 80 ℃ for 24 hours to obtain a nanocomposite, and high resolution transmission electron microscope (HR-TEM) photographs of the nanocomposite are shown in fig. 3 and 4.
Preparation example 10
Mixing 0.6g of the porous activated carbon powder prepared in preparation example 2 with 40ml of hydrochloric acid with a volume molar concentration of 5mol/L to oxidize the porous activated carbon powder to obtain an oxidized porous activated carbon solution;
MnCl is added to 2 Dissolving in deionized water to obtain MnCl with the volume molar concentration of 5mol/L 2 Aqueous solution, 3ml MnCl 2 Mixing the aqueous solution with the oxidized porous activated carbon solution to prepare a mixed solution;
dropping lithium hydroxide aqueous solution with the volume molar concentration of 5mol/L into the mixed solution, adjusting the pH value of the mixed solution to 12, and separating out active carbon-manganese hydroxide precipitate in the mixed solution;
filtering the mixed solution, separating out precipitate, washing the precipitate with distilled water for 5 times, and drying at 70deg.C for 24 hr to obtain nanocomposite.
PREPARATION EXAMPLE 11
Mixing 0.32g of the porous activated carbon powder prepared in preparation example 3 with 35ml of sulfuric acid with a volume molar concentration of 3.5mol/L to oxidize the porous activated carbon powder to obtain an oxidized porous activated carbon solution;
copper carbonate is dissolved in deionized water to obtain a copper carbonate solution with the volume molar concentration of 3.5mol/L, and 2ml of copper carbonate solution is mixed with the oxidized porous activated carbon solution to prepare a mixed solution;
dropwise adding a potassium hydroxide aqueous solution with the volume molar concentration of 3.5mol/L into the mixed solution, adjusting the pH value of the mixed solution to 9, and separating out an activated carbon-copper hydroxide precipitate from the mixed solution;
filtering the mixed solution, separating out precipitate, washing the precipitate with distilled water for 4 times, and drying at 60deg.C for 24 hr to obtain nanocomposite.
Preparation example 12
Mixing 0.5g of the porous activated carbon powder prepared in preparation example 4 with 30ml of nitric acid with a volume molar concentration of 4.2mol/L to oxidize the porous activated carbon powder to obtain an oxidized porous activated carbon solution;
dissolving ferric carbonate in deionized water to obtain ferric carbonate solution with the volume molar concentration of 4.2mol/L, and mixing 1.5ml of ferric carbonate solution with oxidized porous activated carbon solution to prepare a mixed solution;
dropping sodium hydroxide aqueous solution with the volume molar concentration of 4.2mol/L into the mixed solution, adjusting the pH value of the mixed solution to 10, and separating out active carbon-ferric hydroxide precipitate from the mixed solution;
filtering the mixed solution, separating out precipitate, washing the precipitate with distilled water for 5 times, and drying at 90 deg.C for 20 hr to obtain the nanometer composite material.
Preparation example 13
Mixing 0.28g of the porous activated carbon powder obtained in preparation example 5 with 30ml of nitric acid with a volume molar concentration of 2.6mol/L to oxidize the porous activated carbon powder to obtain an oxidized porous activated carbon solution;
zinc nitrate is dissolved in deionized water to obtain zinc nitrate solution with volume molar concentration of 2.6mol/L, and 3ml of zinc nitrate solution is mixed with oxidized porous activated carbon solution to prepare mixed solution;
dropwise adding a potassium hydroxide aqueous solution with the volume molar concentration of 2.6mol/L into the mixed solution, adjusting the pH value of the mixed solution to 10, and separating out an active carbon-zinc hydroxide precipitate in the mixed solution;
filtering the mixed solution, separating out precipitate, washing the precipitate with distilled water for 5 times, and drying at 100deg.C for 18 hr to obtain nanocomposite.
PREPARATION EXAMPLE 14
Mixing 0.22g of the porous activated carbon powder prepared in preparation example 6 with 40ml of hydrochloric acid with a volume molar concentration of 1.4mol/L to oxidize the porous activated carbon powder to obtain an oxidized porous activated carbon solution;
dissolving silver nitrate in deionized water to obtain a silver nitrate solution with the volume molar concentration of 1.4mol/L, and mixing 4ml of the silver nitrate solution with the oxidized porous activated carbon solution to obtain a mixed solution;
dripping a potassium hydroxide aqueous solution with the volume molar concentration of 1.4mol/L into the mixed solution, adjusting the pH value of the mixed solution to 12, and separating out an active carbon-silver hydroxide precipitate in the mixed solution;
filtering the mixed solution, separating out precipitate, washing the precipitate with distilled water for 5 times, and drying at 80deg.C for 24 hr to obtain nanocomposite.
Preparation example 15
Mixing 0.08g of the porous activated carbon powder obtained in preparation example 7 with 40ml of hydrochloric acid with a volume molar concentration of 0.1mol/L to oxidize the porous activated carbon powder to obtain an oxidized porous activated carbon solution;
TiCl is added to the mixture 4 Dissolving in deionized water to obtain TiCl with volume molar concentration of 0.1mol/L 4 Solution, 5ml TiCl 4 Mixing the solution with the oxidized porous activated carbon solution to prepare a mixed solution;
dropping ammonia water with the volume molar concentration of 0.1mol/L into the mixed solution, adjusting the pH value of the mixed solution to 9, and separating out active carbon-titanium hydroxide precipitate from the mixed solution;
filtering the mixed solution, separating out precipitate, washing the precipitate with distilled water for 5 times, and drying at 85deg.C for 22 hr to obtain nanocomposite.
PREPARATION EXAMPLE 16
Mixing 0.1g of the porous activated carbon powder obtained in preparation example 8 with 25ml of sulfuric acid having a volume molar concentration of 0.6mol/L to oxidize the porous activated carbon powder, thereby obtaining an oxidized porous activated carbon solution;
copper sulfate is dissolved in deionized water to obtain a copper sulfate solution with the volume molar concentration of 0.6mol/L, and 5ml of the copper sulfate solution is mixed with the oxidized porous activated carbon solution to prepare a mixed solution;
dropping sodium hydroxide with the volume molar concentration of 0.6mol/L into the mixed solution, adjusting the pH value of the mixed solution to 9, and separating out activated carbon-copper hydroxide precipitate from the mixed solution;
filtering the mixed solution, separating out precipitate, washing the precipitate with distilled water for 6 times, and drying at 85deg.C for 22 hr to obtain nanocomposite.
Preparation example 17
Mixing 0.25g of the porous activated carbon powder obtained in preparation example 7 with 30ml of nitric acid with a volume molar concentration of 1.8mol/L to oxidize the porous activated carbon powder to obtain an oxidized porous activated carbon solution;
dissolving vanadium nitrate in deionized water to obtain a vanadium nitrate solution with the volume molar concentration of 1mol/L, and mixing 3ml of the vanadium nitrate solution with the oxidized porous activated carbon solution to prepare a mixed solution;
dropping sodium hydroxide with the volume molar concentration of 1mol/L into the mixed solution, adjusting the pH value of the mixed solution to 10, and separating out active carbon-vanadium hydroxide precipitate from the mixed solution;
filtering the mixed solution, separating out precipitate, washing the precipitate with distilled water for 5 times, and drying at 80deg.C for 24 hr to obtain nanocomposite.
PREPARATION EXAMPLE 18
Mixing 0.22g of the porous activated carbon powder obtained in preparation example 7 with 35ml of nitric acid with a volume molar concentration of 2.1mol/L to oxidize the porous activated carbon powder to obtain an oxidized porous activated carbon solution;
dissolving chromium nitrate in deionized water to obtain a chromium nitrate solution with the volume molar concentration of 2.1mol/L, and mixing 3ml of the chromium nitrate solution with the oxidized porous activated carbon solution to obtain a mixed solution;
dropwise adding potassium hydroxide with the volume molar concentration of 2.1mol/L into the mixed solution, adjusting the pH value of the mixed solution to 11, and separating out active carbon-chromium hydroxide precipitate from the mixed solution;
filtering the mixed solution, separating out precipitate, washing the precipitate with distilled water for 5 times, and drying at 90 deg.C for 20 hr to obtain the nanometer composite material.
Preparation example 19
Mixing 0.31g of the porous activated carbon powder prepared in preparation example 1 with 35ml of hydrochloric acid with a volume molar concentration of 3mol/L to oxidize the porous activated carbon powder to obtain an oxidized porous activated carbon solution;
AuCl is to be made 3 Dissolving in deionized water to obtain AuCl with volume mole concentration of 3mol/L 3 Solution, 1.8ml AuCl 3 Mixing the solution with the oxidized porous activated carbon solution to prepare a mixed solution;
dropwise adding potassium hydroxide with the volume molar concentration of 3mol/L into the mixed solution, adjusting the pH value of the mixed solution to 10.5, and separating out active carbon-gold hydroxide precipitate from the mixed solution;
filtering the mixed solution, separating out precipitate, washing the precipitate with distilled water for 5 times, and drying at 90 deg.C for 20 hr to obtain the nanometer composite material.
Preparation example 20
Mixing 0.57g of the porous activated carbon powder obtained in preparation example 2 with 30ml of nitric acid having a volume molar concentration of 4.8mol/L to oxidize the porous activated carbon powder, thereby obtaining an oxidized porous activated carbon solution;
dissolving palladium nitrate in deionized water to obtain a palladium nitrate solution with the volume molar concentration of 4.8mol/L, and mixing 1.2ml of the palladium nitrate solution with the oxidized porous activated carbon solution to prepare a mixed solution;
dropwise adding potassium hydroxide with the volume molar concentration of 4.8mol/L into the mixed solution, adjusting the pH value of the mixed solution to 10.5, and separating out an activated carbon-palladium hydroxide precipitate in the mixed solution;
filtering the mixed solution, separating out precipitate, washing the precipitate with distilled water for 5 times, and drying at 75deg.C for 24 hr to obtain nanocomposite.
Preparation example 21
Mixing 0.1g of the porous activated carbon powder prepared in preparation example 3 with 20ml of nitric acid with a volume molar concentration of 0.5mol/L to oxidize the porous activated carbon powder to obtain an oxidized porous activated carbon solution;
dissolving platinum nitrate into deionized water to obtain a platinum nitrate solution with the volume molar concentration of 0.5mol/L, and mixing 5ml of the platinum nitrate solution with the oxidized porous activated carbon solution to prepare a mixed solution;
dropping ammonia water with the volume molar concentration of 0.5mol/L into the mixed solution, adjusting the pH value of the mixed solution to 8, and separating out active carbon-platinum hydroxide precipitate from the mixed solution;
filtering the mixed solution, separating out precipitate, washing the precipitate with distilled water for 5 times, and drying at 75deg.C for 24 hr to obtain nanocomposite.
PREPARATION EXAMPLE 22
Mixing 0.25g of the porous activated carbon powder obtained in preparation example 4 with 30ml of sulfuric acid having a volume molar concentration of 1.8mol/L to oxidize the porous activated carbon powder, thereby obtaining an oxidized porous activated carbon solution;
CdSO is processed into 4 Dissolving in deionized water to obtain CdSO with volume mole concentration of 0.5mol/L 4 Solution, 1.8ml CdSO 4 Mixing the solution with the oxidized porous activated carbon solution to prepare a mixed solution;
dripping lithium hydroxide with the volume molar concentration of 0.5mol/L into the mixed solution, adjusting the pH value of the mixed solution to 10, and separating out active carbon-cadmium hydroxide precipitate from the mixed solution;
filtering the mixed solution, separating out precipitate, washing the precipitate with distilled water for 5 times, and drying at 80deg.C for 24 hr to obtain nanocomposite.
Preparation example 23
Mixing 0.3g of the porous activated carbon powder prepared in preparation example 4 with 40ml of hydrochloric acid with a volume molar concentration of 2.9mol/L to oxidize the porous activated carbon powder to obtain an oxidized porous activated carbon solution;
dissolving ruthenium chloride in deionized water to obtain a ruthenium chloride solution with the volume molar concentration of 2.9mol/L, and mixing 2.9ml of the ruthenium chloride solution with the oxidized porous activated carbon solution to prepare a mixed solution;
dropping ammonia water with the volume molar concentration of 2.9mol/L into the mixed solution, adjusting the pH value of the mixed solution to 11, and separating out active carbon-ruthenium hydroxide precipitate from the mixed solution;
filtering the mixed solution, separating out precipitate, washing the precipitate with distilled water for 5 times, and drying at 80deg.C for 24 hr to obtain nanocomposite.
PREPARATION EXAMPLE 24
Mixing 0.55g of the porous activated carbon powder prepared in preparation example 5 with 35ml of sulfuric acid having a volume molar concentration of 4.5mol/L to oxidize the porous activated carbon powder, thereby obtaining an oxidized porous activated carbon solution;
dissolving cobalt sulfate in deionized water to obtain a cobalt sulfate solution with the volume molar concentration of 4.5mol/L, and mixing 1.5ml of ruthenium chloride solution with the oxidized porous activated carbon solution to prepare a mixed solution;
dropping lithium hydroxide with the volume molar concentration of 4.5mol/L into the mixed solution, adjusting the pH value of the mixed solution to 12, and separating out active carbon-cobalt hydroxide precipitate from the mixed solution;
filtering the mixed solution, separating out precipitate, washing the precipitate with distilled water for 5 times, and drying at 90 deg.C for 20 hr to obtain the nanometer composite material.
Examples 1 to 16 are preparation of electrode materials for super capacitor
Example 1
The nanocomposite prepared in preparation example 9, the conductive material, the adhesive and the dispersing agent are mixed according to the weight ratio of 10:0.2:0.2:0.1, and the mixture is mixed for 1 hour by adopting a planetary mixer to prepare the supercapacitor electrode material for standby.
Wherein the conductive material is conductive carbon black Super-P in termi high belgium, the adhesive is a mixture of carboxymethyl cellulose and styrene-butadiene rubber mixed according to the weight ratio of 17:1, the dispersing agent is ethanol, and the purity of the ethanol is 95%.
Example 2
The nanocomposite prepared in preparation example 10, the conductive material, the adhesive and the dispersing agent are mixed according to the weight ratio of 10:1:1:5, and the mixture is mixed for 2 hours by adopting a planetary mixer to prepare the supercapacitor electrode material for standby.
Wherein the conductive material is natural graphite, the adhesive is polytetrafluoroethylene, the dispersing agent is acetone, and the purity of the acetone is 96%.
Example 3
The nanocomposite prepared in preparation example 11, the conductive material, the adhesive and the dispersing agent are mixed according to the weight ratio of 10:0.7:0.7:10, and the mixture is mixed for 5 hours by adopting a planetary mixer to prepare the supercapacitor electrode material for standby.
Wherein the conductive material is artificial graphite, the adhesive is polyvinylidene fluoride, the dispersant is isopropanol, and the purity of the isopropanol is 99%.
Example 4
The nanocomposite, conductive material, binder and dispersant prepared in preparation example 12 were mixed in a weight ratio of 10:1.5:1.5:20, mixing for 4 hours by adopting a planetary mixer to prepare the electrode material of the super capacitor for standby.
Wherein the conductive material is carbon black, the adhesive is polyvinyl alcohol, the dispersing agent is N-methyl pyrrolidone, and the purity of the N-methyl pyrrolidone is 95%.
Example 5
The nanocomposite, conductive material, binder and dispersant prepared in preparation example 13 were mixed in a weight ratio of 10:2:2:30, mixing for 8 hours by adopting a planetary mixer to prepare the electrode material of the super capacitor for standby.
Wherein the conductive material is acetylene black, the adhesive is polyvinyl butyral, the dispersing agent is propylene glycol, and the purity of the propylene glycol is 99%.
Example 6
The nanocomposite, conductive material, binder and dispersant prepared in preparation example 14 were mixed in a weight ratio of 10:2:2:30, mixing for 8 hours by adopting a planetary mixer to prepare the electrode material of the super capacitor for standby.
Wherein the conductive material is acetylene black, the adhesive is polyvinyl butyral, the dispersing agent is propylene glycol, and the purity of the propylene glycol is 99%.
Example 7
The nanocomposite, conductive material, binder and dispersant prepared in preparation example 15 were mixed in a weight ratio of 10:1.8:1.8:25, mixing for 6 hours by adopting a planetary mixer to prepare the electrode material of the super capacitor for standby.
Wherein the conductive material is ketjen black, the adhesive is polyvinyl butyral, the dispersing agent is propylene glycol, and the purity of the propylene glycol is 99%.
Example 8
The nanocomposite, conductive material, binder and dispersant prepared in preparation example 16 were mixed in a weight ratio of 10:1.1:1.1:9, mixing, namely mixing for 5 hours by adopting a planetary mixer to prepare the electrode material of the super capacitor for standby.
Wherein the conductive material is carbon fiber, the adhesive is poly-N-vinyl pyrrolidone, the dispersing agent is propylene glycol, and the purity of the propylene glycol is 99%.
Example 9
The nanocomposite, conductive material, binder and dispersant prepared in preparation example 17 were mixed in a weight ratio of 10:1.3:1.3:14, mixing for 5.5 hours by adopting a planetary mixer to prepare the electrode material of the super capacitor for standby.
Wherein the conductive material is copper powder, the adhesive is polyamide imide, the dispersing agent is ethanol, and the purity of the ethanol is 95%.
Example 10
The nanocomposite, conductive material, binder and dispersant prepared in preparation example 18 were mixed in a weight ratio of 10:0.7:0.7: and 6, mixing, namely mixing for 5.5 hours by using a planetary mixer to prepare the electrode material of the supercapacitor for later use.
Wherein the conductive material is copper powder, the adhesive is polyamide imide, the dispersing agent is ethanol, and the purity of the ethanol is 95%.
Example 11
The nanocomposite, conductive material, binder and dispersant prepared in preparation example 19 were mixed in a weight ratio of 10:0.7:0.7: and 6, mixing, namely mixing for 5.5 hours by using a planetary mixer to prepare the electrode material of the supercapacitor for later use.
Wherein the conductive material is nickel powder, the adhesive is polyimide, the dispersing agent is acetone, and the purity of the acetone is 96%.
Example 12
The nanocomposite, conductive material, binder and dispersant prepared in preparation example 20 were mixed in a weight ratio of 10:0.7:0.7: and 6, mixing, namely mixing for 5.5 hours by using a planetary mixer to prepare the electrode material of the supercapacitor for later use.
Wherein the conductive material is aluminum powder, the adhesive is carboxymethyl cellulose, the dispersing agent is acetone, and the purity of the acetone is 96%.
Example 13
The nanocomposite, conductive material, binder and dispersant prepared in preparation example 21 were mixed in a weight ratio of 10:0.7:0.7: and 6, mixing, namely mixing for 5.5 hours by using a planetary mixer to prepare the electrode material of the supercapacitor for later use.
Wherein the conductive material is carbon black, the adhesive is polyvinyl alcohol, the dispersing agent is acetone, and the purity of the acetone is 96%.
Example 14
The nanocomposite, conductive material, binder and dispersant prepared in preparation example 22 were mixed in a weight ratio of 10:0.7:0.7: and 6, mixing, namely mixing for 5.5 hours by using a planetary mixer to prepare the electrode material of the supercapacitor for later use.
Wherein the conductive material is acetylene black, the adhesive is polyvinyl alcohol, the dispersing agent is acetone, and the purity of the acetone is 96%.
Example 15
The nanocomposite, conductive material, binder and dispersant prepared in preparation example 23 were mixed in a weight ratio of 10:0.7:0.7: and 6, mixing, namely mixing for 5.5 hours by using a planetary mixer to prepare the electrode material of the supercapacitor for later use.
Wherein the conductive material is acetylene black, the adhesive is polyvinyl alcohol, the dispersing agent is acetone, and the purity of the acetone is 96%.
Example 16
The nanocomposite, conductive material, binder and dispersant prepared in preparation example 24 were mixed in a weight ratio of 10:0.7:0.7: and 6, mixing, namely mixing for 5.5 hours by using a planetary mixer to prepare the electrode material of the supercapacitor for later use.
Wherein the conductive material is acetylene black, the adhesive is polyvinyl alcohol, the dispersing agent is acetone, and the purity of the acetone is 96%.
The supercapacitor electrode material prepared in example 1 was coated on a titanium foil in an area of 1cm×1cm, and then dried at a temperature of 120 ℃ for 2 hours to prepare a supercapacitor electrode. A three-electrode cell was constructed using a platinum electrode as a counter electrode, the supercapacitor electrode prepared from the electrode material of example 1 as a working electrode, a saturated calomel electrode as a reference electrode, and a three-electrode cell mounted in a beaker having a capacity of 250ml and using a potassium hydroxide solution having a molar concentration of 6mol/L as an electrolyte, and fig. 5 is a cyclic voltammogram of an electrode current value when the electrode potential of the three-electrode cell was kept constant at a constant potential scan rate change within a constant potential window.
As can be seen from fig. 5, when the potential sweep rate was increased from 1mV/s to 30mV/s, the pseudocapacitor behavior of the supercapacitor electrode fabricated according to example 1 remained intact, while it can be seen that the pseudocapacitor behavior of the supercapacitor electrode fabricated according to example 1 was very reversible; the supercapacitor electrode prepared according to example 1 had a specific capacitance of 265.8F/g at a potential sweep rate of 1mV/s and decreased to 188.2F/g when the potential sweep rate was increased to 30 mV/s; the reduction rate was confirmed to be 29.2%, indicating that the supercapacitor electrode prepared in example 1 has excellent electrochemical properties.
The supercapacitor electrode materials prepared in examples 1 to 8 were coated on corresponding aluminum etched foils and dried at 120℃for 2 hours, the dried product was punched into cylindrical supercapacitor electrodes having a bottom diameter of 12mm and a height of 1.2mm, the supercapacitor electrodes prepared were used as anodes and cathodes to manufacture supercapacitors in the form of button cells having a bottom diameter of 20mm and a height of 3.2mm, the electrolyte was a mixed solution of propylene carbonate and tetraethylammonium tetrafluoroborate, the volumetric molar concentration of tetraethylammonium tetrafluoroborate was 1mol/L, and the separator was TF4035 manufactured by Japanese NKK; the supercapacitor in the form of a coin cell prepared as described above was aged by applying a voltage of 2.7V at 70 ℃ and measuring the capacity by charging and discharging to 2.7V, and the volume ratio capacity was obtained by dividing the measured capacity by the sum of the volumes of the positive electrode and the negative electrode, as shown in table 2 below.
TABLE 2
From the test results in Table 2, it is apparent that the volumetric capacitance of the super capacitor prepared by using the super capacitor electrode materials obtained in examples 1 to 8 is higher than 21F/cc, and higher than that of the existing super capacitor electrode, so that the practical requirements can be better satisfied.
The foregoing are all preferred embodiments of the present application, and are not intended to limit the scope of the present application in any way, therefore: all equivalent changes in structure, shape and principle of this application should be covered in the protection scope of this application.
Claims (10)
1. The preparation method of the supercapacitor electrode material is characterized by comprising the following steps of:
s1, preparing porous activated carbon powder, wherein the specific surface area of the porous activated carbon powder is 300-1300 m 2 And/g, wherein the average interlayer spacing of the porous activated carbon powder is 3.385-4.445 nm;
s2, oxidizing the porous activated carbon powder in an acid solution to obtain an oxidized porous activated carbon solution;
s3, adding the transition metal aqueous solution into the oxidized porous activated carbon solution to prepare a mixed solution;
s4, dripping the alkaline solution into the mixed solution, and adjusting the pH value of the mixed solution to 8-12 to separate out a precipitate in the mixed solution;
s5, filtering the mixed solution to obtain a precipitate, and washing and drying the precipitate to obtain the nanocomposite;
s6, mixing the nanocomposite, the conductive material, the adhesive and the dispersing agent according to the weight ratio of 10: (0.2-2): (0.2-2): (0.1-30) and mixing to obtain the supercapacitor electrode material.
2. The method for preparing the supercapacitor electrode material according to claim 1, wherein in the step S1, the method for preparing the porous activated carbon powder comprises the steps of:
step one, carbonizing a carbon material under the condition of atmosphere protection;
step two, activating the carbonized carbon material;
and thirdly, washing and drying the activated carbon material to obtain the porous activated carbon powder.
3. The method for preparing the supercapacitor electrode material according to claim 2, wherein in the first step, the protective atmosphere is nitrogen or argon, and the carbonization treatment temperature is 550-900 ℃.
4. The method for preparing the supercapacitor electrode material according to claim 2, wherein in the first step, the carbon material is selected from one of petroleum pitch, coal pitch, petroleum coke and coal coke.
5. The method for preparing the supercapacitor electrode material according to claim 2, wherein in the second step, the activation treatment is performed by: the carbonized carbon material and potassium hydroxide or sodium hydroxide are mixed according to the weight ratio of 1: (1-5) mixing, grinding, and heating for 0.16-12 hours in a protective atmosphere at 600-900 ℃ to obtain the activated carbon material.
6. The method for preparing an electrode material for a supercapacitor according to claim 1, wherein in the step S2, the weight of the porous activated carbon powder is 0.1 to 0.3g, the volume of the acidic solution is 20 to 40ml, the molar concentration of the acidic solution is 0.1 to 5mol/L, and the acidic solution is one selected from nitric acid, hydrochloric acid and sulfuric acid.
7. The method for producing an electrode material for a supercapacitor according to claim 6, wherein in the step S3, the amount of the aqueous solution of the transition metal added is 1 to 5ml, and the volume molar concentration of the aqueous solution of the transition metal is 0.1 to 5mol/L.
8. The method for preparing the supercapacitor electrode material according to claim 1, wherein in the step S3, the method for preparing the aqueous transition metal solution comprises the following steps: dissolving a transition metal source in deionized water, wherein the transition metal source has a chemical formula of M (NO 3 ) n ，M(CO 3 ) n/2 ，M(SO 4 ) n/2 Or MCl n Wherein M is selected from one of Ti, V, cr, mn, fe, co, ni, cu, cd, zn, ru, pd, ag, pt and Au, and the value of n is matched with the valence of the metal M.
9. The method for preparing an electrode material for a supercapacitor according to claim 1, wherein in the step S4, the alkaline solution is selected from one of an aqueous lithium hydroxide solution, an aqueous sodium hydroxide solution, an aqueous potassium hydroxide solution, and aqueous ammonia, and the volume molar concentration of the alkaline solution is 0.1 to 10 mol/L.
10. A supercapacitor electrode material prepared by the method for preparing the supercapacitor electrode material according to claim 1.
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