CN116623250A - Formation foil for aluminum electrolytic capacitor and preparation method thereof - Google Patents
Formation foil for aluminum electrolytic capacitor and preparation method thereof Download PDFInfo
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- CN116623250A CN116623250A CN202310644613.8A CN202310644613A CN116623250A CN 116623250 A CN116623250 A CN 116623250A CN 202310644613 A CN202310644613 A CN 202310644613A CN 116623250 A CN116623250 A CN 116623250A
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- foil
- phosphate
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- 239000011888 foil Substances 0.000 title claims abstract description 174
- 230000015572 biosynthetic process Effects 0.000 title claims abstract description 54
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 title claims abstract description 25
- 229910052782 aluminium Inorganic materials 0.000 title claims abstract description 24
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 239000003990 capacitor Substances 0.000 title claims abstract description 13
- 239000007788 liquid Substances 0.000 claims abstract description 78
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims abstract description 39
- WNLRTRBMVRJNCN-UHFFFAOYSA-N adipic acid Chemical compound OC(=O)CCCCC(O)=O WNLRTRBMVRJNCN-UHFFFAOYSA-N 0.000 claims abstract description 26
- 229910019142 PO4 Inorganic materials 0.000 claims abstract description 19
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 claims abstract description 19
- 239000010452 phosphate Substances 0.000 claims abstract description 19
- 239000001361 adipic acid Substances 0.000 claims abstract description 13
- 235000011037 adipic acid Nutrition 0.000 claims abstract description 13
- 238000009835 boiling Methods 0.000 claims abstract description 13
- 229920001529 polyepoxysuccinic acid Polymers 0.000 claims abstract description 13
- BTBUEUYNUDRHOZ-UHFFFAOYSA-N Borate Chemical compound [O-]B([O-])[O-] BTBUEUYNUDRHOZ-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000011248 coating agent Substances 0.000 claims abstract description 5
- 238000000576 coating method Methods 0.000 claims abstract description 5
- 238000004506 ultrasonic cleaning Methods 0.000 claims abstract description 5
- 238000000034 method Methods 0.000 claims description 49
- 230000008569 process Effects 0.000 claims description 31
- 238000005245 sintering Methods 0.000 claims description 26
- 238000006243 chemical reaction Methods 0.000 claims description 22
- 239000000126 substance Substances 0.000 claims description 22
- 238000004140 cleaning Methods 0.000 claims description 19
- LFVGISIMTYGQHF-UHFFFAOYSA-N ammonium dihydrogen phosphate Chemical compound [NH4+].OP(O)([O-])=O LFVGISIMTYGQHF-UHFFFAOYSA-N 0.000 claims description 17
- 229910000387 ammonium dihydrogen phosphate Inorganic materials 0.000 claims description 17
- 235000019837 monoammonium phosphate Nutrition 0.000 claims description 17
- 239000006012 monoammonium phosphate Substances 0.000 claims description 16
- 229910021538 borax Inorganic materials 0.000 claims description 13
- UQGFMSUEHSUPRD-UHFFFAOYSA-N disodium;3,7-dioxido-2,4,6,8,9-pentaoxa-1,3,5,7-tetraborabicyclo[3.3.1]nonane Chemical compound [Na+].[Na+].O1B([O-])OB2OB([O-])OB1O2 UQGFMSUEHSUPRD-UHFFFAOYSA-N 0.000 claims description 13
- 239000004328 sodium tetraborate Substances 0.000 claims description 13
- 235000010339 sodium tetraborate Nutrition 0.000 claims description 13
- 238000001035 drying Methods 0.000 claims description 12
- 239000001488 sodium phosphate Substances 0.000 claims description 12
- 229910000162 sodium phosphate Inorganic materials 0.000 claims description 12
- 235000011008 sodium phosphates Nutrition 0.000 claims description 12
- RYFMWSXOAZQYPI-UHFFFAOYSA-K trisodium phosphate Chemical compound [Na+].[Na+].[Na+].[O-]P([O-])([O-])=O RYFMWSXOAZQYPI-UHFFFAOYSA-K 0.000 claims description 12
- OTRAYOBSWCVTIN-UHFFFAOYSA-N OB(O)O.OB(O)O.OB(O)O.OB(O)O.OB(O)O.N.N.N.N.N.N.N.N.N.N.N.N.N.N.N Chemical group OB(O)O.OB(O)O.OB(O)O.OB(O)O.OB(O)O.N.N.N.N.N.N.N.N.N.N.N.N.N.N.N OTRAYOBSWCVTIN-UHFFFAOYSA-N 0.000 claims description 10
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 claims description 9
- 239000004327 boric acid Substances 0.000 claims description 9
- 238000005238 degreasing Methods 0.000 claims description 9
- 239000002270 dispersing agent Substances 0.000 claims description 8
- 239000000853 adhesive Substances 0.000 claims description 7
- 230000001070 adhesive effect Effects 0.000 claims description 7
- 239000011268 mixed slurry Substances 0.000 claims description 6
- 239000003960 organic solvent Substances 0.000 claims description 6
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 5
- 239000000243 solution Substances 0.000 claims description 5
- 239000011259 mixed solution Substances 0.000 claims description 4
- LWIHDJKSTIGBAC-UHFFFAOYSA-K tripotassium phosphate Chemical compound [K+].[K+].[K+].[O-]P([O-])([O-])=O LWIHDJKSTIGBAC-UHFFFAOYSA-K 0.000 claims description 4
- 229920002125 Sokalan® Polymers 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
- 229920000058 polyacrylate Polymers 0.000 claims description 3
- 239000004584 polyacrylic acid Substances 0.000 claims description 3
- 239000012298 atmosphere Substances 0.000 claims description 2
- 235000014113 dietary fatty acids Nutrition 0.000 claims description 2
- 239000000194 fatty acid Substances 0.000 claims description 2
- 229930195729 fatty acid Natural products 0.000 claims description 2
- 150000004665 fatty acids Chemical class 0.000 claims description 2
- 150000002632 lipids Chemical class 0.000 claims description 2
- 229920002401 polyacrylamide Polymers 0.000 claims description 2
- 229920002635 polyurethane Polymers 0.000 claims description 2
- 239000004814 polyurethane Substances 0.000 claims description 2
- 229910000160 potassium phosphate Inorganic materials 0.000 claims description 2
- 235000011009 potassium phosphates Nutrition 0.000 claims description 2
- FQENQNTWSFEDLI-UHFFFAOYSA-J sodium diphosphate Chemical compound [Na+].[Na+].[Na+].[Na+].[O-]P([O-])(=O)OP([O-])([O-])=O FQENQNTWSFEDLI-UHFFFAOYSA-J 0.000 claims description 2
- 229940048086 sodium pyrophosphate Drugs 0.000 claims description 2
- 235000019818 tetrasodium diphosphate Nutrition 0.000 claims description 2
- 239000001577 tetrasodium phosphonato phosphate Substances 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims 3
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 claims 1
- 150000001298 alcohols Chemical group 0.000 claims 1
- 239000003822 epoxy resin Substances 0.000 claims 1
- 229920001568 phenolic resin Polymers 0.000 claims 1
- 239000005011 phenolic resin Substances 0.000 claims 1
- 229920000647 polyepoxide Polymers 0.000 claims 1
- 238000005755 formation reaction Methods 0.000 description 46
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 15
- 229910052751 metal Inorganic materials 0.000 description 13
- 239000002184 metal Substances 0.000 description 13
- 238000005406 washing Methods 0.000 description 13
- 230000000052 comparative effect Effects 0.000 description 8
- 230000008439 repair process Effects 0.000 description 8
- VZCYOOQTPOCHFL-OWOJBTEDSA-N Fumaric acid Chemical compound OC(=O)\C=C\C(O)=O VZCYOOQTPOCHFL-OWOJBTEDSA-N 0.000 description 6
- 239000002002 slurry Substances 0.000 description 6
- 238000012360 testing method Methods 0.000 description 6
- 150000003013 phosphoric acid derivatives Chemical class 0.000 description 5
- 239000000843 powder Substances 0.000 description 5
- 239000002904 solvent Substances 0.000 description 5
- 229940067597 azelate Drugs 0.000 description 4
- VGTPKLINSHNZRD-UHFFFAOYSA-N oxoborinic acid Chemical compound OB=O VGTPKLINSHNZRD-UHFFFAOYSA-N 0.000 description 4
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 3
- 238000005452 bending Methods 0.000 description 3
- 229910052799 carbon Inorganic materials 0.000 description 3
- 230000007547 defect Effects 0.000 description 3
- 238000005265 energy consumption Methods 0.000 description 3
- 239000001530 fumaric acid Substances 0.000 description 3
- 239000001257 hydrogen Substances 0.000 description 3
- 229910052739 hydrogen Inorganic materials 0.000 description 3
- VZCYOOQTPOCHFL-UHFFFAOYSA-N trans-butenedioic acid Natural products OC(=O)C=CC(O)=O VZCYOOQTPOCHFL-UHFFFAOYSA-N 0.000 description 3
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 description 2
- -1 ammonium azelate hydrogen Chemical class 0.000 description 2
- 239000011230 binding agent Substances 0.000 description 2
- 239000000835 fiber Substances 0.000 description 2
- 239000002923 metal particle Substances 0.000 description 2
- BDJRBEYXGGNYIS-UHFFFAOYSA-N nonanedioic acid Chemical compound OC(=O)CCCCCCCC(O)=O BDJRBEYXGGNYIS-UHFFFAOYSA-N 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 238000002791 soaking Methods 0.000 description 2
- 239000012085 test solution Substances 0.000 description 2
- 239000010936 titanium Substances 0.000 description 2
- 229910052719 titanium Inorganic materials 0.000 description 2
- XNWFRZJHXBZDAG-UHFFFAOYSA-N 2-METHOXYETHANOL Chemical compound COCCO XNWFRZJHXBZDAG-UHFFFAOYSA-N 0.000 description 1
- 239000004593 Epoxy Substances 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000006978 adaptation Effects 0.000 description 1
- 125000003158 alcohol group Chemical group 0.000 description 1
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 238000010000 carbonizing Methods 0.000 description 1
- 238000005253 cladding Methods 0.000 description 1
- 239000006255 coating slurry Substances 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 125000004435 hydrogen atom Chemical class [H]* 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 125000004108 n-butyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 description 1
- 239000011858 nanopowder Substances 0.000 description 1
- 229910052758 niobium Inorganic materials 0.000 description 1
- 239000010955 niobium Substances 0.000 description 1
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 description 1
- IJGRMHOSHXDMSA-UHFFFAOYSA-N nitrogen Substances N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N phenol group Chemical group C1(=CC=CC=C1)O ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 229910052715 tantalum Inorganic materials 0.000 description 1
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
- C25D11/02—Anodisation
- C25D11/04—Anodisation of aluminium or alloys based thereon
- C25D11/12—Anodising more than once, e.g. in different baths
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
- C25D11/02—Anodisation
- C25D11/04—Anodisation of aluminium or alloys based thereon
- C25D11/06—Anodisation of aluminium or alloys based thereon characterised by the electrolytes used
- C25D11/08—Anodisation of aluminium or alloys based thereon characterised by the electrolytes used containing inorganic acids
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
- C25D11/02—Anodisation
- C25D11/04—Anodisation of aluminium or alloys based thereon
- C25D11/06—Anodisation of aluminium or alloys based thereon characterised by the electrolytes used
- C25D11/10—Anodisation of aluminium or alloys based thereon characterised by the electrolytes used containing organic acids
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
- C25D11/02—Anodisation
- C25D11/04—Anodisation of aluminium or alloys based thereon
- C25D11/16—Pretreatment, e.g. desmutting
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G9/00—Electrolytic capacitors, rectifiers, detectors, switching devices, light-sensitive or temperature-sensitive devices; Processes of their manufacture
- H01G9/004—Details
- H01G9/04—Electrodes or formation of dielectric layers thereon
- H01G9/048—Electrodes or formation of dielectric layers thereon characterised by their structure
- H01G9/052—Sintered electrodes
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G9/00—Electrolytic capacitors, rectifiers, detectors, switching devices, light-sensitive or temperature-sensitive devices; Processes of their manufacture
- H01G9/004—Details
- H01G9/04—Electrodes or formation of dielectric layers thereon
- H01G9/048—Electrodes or formation of dielectric layers thereon characterised by their structure
- H01G9/055—Etched foil electrodes
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/13—Energy storage using capacitors
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Power Engineering (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Inorganic Chemistry (AREA)
- Chemical Treatment Of Metals (AREA)
Abstract
The invention discloses a formation foil for an aluminum electrolytic capacitor and a preparation method thereof, wherein the preparation method comprises the following steps: placing the basic sintered foil into a first treatment liquid for ultrasonic cleaning, roasting at 550-580 ℃, boiling the obtained roasted foil in a second treatment liquid to obtain a second treatment foil, and carrying out formation treatment to obtain a formation foil; wherein the first treatment liquid comprises citric acid, polyepoxysuccinic acid and adipic acid with the concentration of 1-5g/L, 0.2-0.4g/L and 0.3-0.8g/L respectively; the second treatment liquid comprises phosphate and borate with the concentration of 0.05-0.5g/L and 0.1-1.0 g/L. The invention solves the problem of carbide residue in the preparation of the sintered foil by the wet coating, and the obtained formed foil can further obtain the anode foil of the aluminum electrolytic capacitor with high specific volume and low leakage current.
Description
Technical Field
The invention relates to the technical field of aluminum electrolytic capacitors, in particular to the technical field of sintered foils of aluminum electrolytic capacitors.
Background
The aluminum electrolytic capacitor is widely used in the fields of communication equipment, consumer electronics, instruments and meters, energy-saving illumination and the like. Anode foil is a key material of aluminum electrolytic capacitor products, which restricts the performance of the capacitor. The current market adopts a sintering process anode foil. The preparation process comprises the following steps: the metal powder, the adhesive, the dispersing agent and the solvent are prepared into slurry, the slurry is coated on the surface of the aluminum foil, and then the high-capacity anode foil is obtained through drying degreasing, sintering and formation. The metal powder mainly comprises valve metals such as aluminum, titanium, niobium, tantalum and the like, and most commonly aluminum and titanium. In the preparation process of the sintered foil, the oxide formed by the valve metal is used as a dielectric medium to restrict the performance of the anode foil, meanwhile, after sintering, a part of residual carbide formed by a dispersant and a binder dissolved in a solvent is attached to the surface of the valve metal and even filled among gaps of metal particles, so that the surface area of the anode foil is greatly reduced, and the formation of an oxidation dielectric layer is blocked in the subsequent formation step, so that a series of problems of high formation energy consumption, increased oxide film defects, high leakage current, long boosting time and the like are caused.
Aiming at the problems, a part of the prior art adopts an improvement scheme, for example, patent document CN108461294B discloses a method for obtaining a sintered foil by taking an anodic oxidation bath solution as a carbon layer source, carbonizing the tunnel aperture and the surface of a corrosion foil at high temperature to form fiber metal carbon wires, and cladding and combining the fiber metal carbon wires with nano powder; patent document CN 110648849B discloses a process of sintering valve metal powder at 620 ℃ for 40 hours under an alkane-nitrogen mixed gas, or preparing valve metal powder, a solvent, and organic resins of different contents into slurry, and sintering; patent document CN111463016B discloses a process of sintering aluminum powder at a higher temperature by adding specific valve metal particles. However, although the above technology reduces the content of residual carbide to a certain extent by modifying the carbide morphology, reasonably constructing powder and sintering at high temperature, more carbide remains on the valve metal surface in practice, so that the performance of the sintered foil cannot be further improved.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide a novel sintered foil for an aluminum electrolytic capacitor and a preparation method thereof, wherein the preparation method can effectively solve the problem of carbide residues in the preparation of the sintered foil by wet coating, reduce energy consumption in the preparation and prepare the anode foil with high capacity, low leakage current and short boosting time by adding a formation pretreatment process between a sintering process and a formation process.
The technical scheme of the invention is as follows:
a method for preparing a formed foil for an aluminum electrolytic capacitor, comprising:
placing the base sintered foil obtained after the sintering process into a first treatment liquid with the pH value controlled at 4-6, and performing ultrasonic cleaning at 60-80 ℃ to obtain a first treatment foil;
cleaning the first treated foil, and roasting at 550-580 ℃ for 1.5-2.5min to obtain a first roasted foil;
placing the first baked foil into a second treatment liquid with the pH value controlled between 5 and 6 to be boiled, so as to obtain a second treatment foil;
carrying out formation treatment on the second treatment foil to obtain a formation foil;
wherein the first treatment liquid comprises: citric acid with the concentration of 1-5g/L, polyepoxysuccinic acid with the concentration of 0.2-0.4g/L and adipic acid with the concentration of 0.3-0.8 g/L; the second treatment liquid includes: phosphate with a concentration of 0.05-0.5g/L and borate with a concentration of 0.1-1.0 g/L.
According to some preferred embodiments of the invention, the time of the ultrasonic cleaning is 1-3min.
According to some preferred embodiments of the invention, the calcination time is 1.5-2.5min.
According to some preferred embodiments of the invention, the boiling time is 5-8min.
According to some preferred embodiments of the present invention, the phosphate comprises a first phosphate and a second phosphate, the first phosphate being monoammonium phosphate, the concentration of which in the second treatment fluid is 0.05-0.15g/L; and in the second treatment liquid, the concentration of the second phosphate is 0.1-0.3g/L, and the concentration of the borate is 0.1-0.8g/L.
According to some preferred embodiments of the present invention, the phosphate salt comprises a first phosphate salt and a second phosphate salt, the first phosphate salt being monoammonium phosphate, the second phosphate salt being selected from one or more of sodium phosphate, potassium phosphate, sodium pyrophosphate, monoammonium phosphate; the borate is selected from ammonium pentaborate and/or sodium tetraborate.
According to some preferred embodiments of the invention, the borate is selected from ammonium pentaborate and/or sodium tetraborate.
According to some preferred embodiments of the invention, the chemical conversion treatment comprises: and (3) placing the second treatment foil into a boric acid solution with the mass percentage of 15%, and carrying out formation at the voltage of 500-540 v.
According to some preferred embodiments of the invention, the chemical conversion treatment comprises: and (3) placing the second treatment foil into a mixed solution of 10 mass percent of boric acid and 5 mass percent of ammonium pentaborate, and carrying out formation at a voltage of 500-540 v.
According to some preferred embodiments of the invention, the chemical conversion process is a four-stage chemical conversion process.
According to some preferred embodiments of the invention, the base sintered foil is obtained by the following preparation process:
mixing titanium powder, an adhesive, a dispersing agent and an organic solvent to obtain mixed slurry;
coating the mixed slurry on the surface of a first aluminum foil after degreasing and drying, covering a second aluminum foil after degreasing and drying on the mixed slurry, bonding up and down, and drying and degreasing at 150 ℃ for 1-2 hours to obtain a presintered foil;
and carrying out heat treatment on the pre-sintered foil for 10-24 hours at 500-580 ℃ in an inert atmosphere to obtain the basic sintered foil.
According to some preferred embodiments of the invention, the binder is selected from one or more of epoxy, phenolic, polyurethane, polyacrylate.
According to some preferred embodiments of the invention, the dispersant is selected from one or more of polyacrylic acid, fatty acid, polyacrylamide.
According to some preferred embodiments of the invention, the organic solvent is selected from alcohol and/or lipid organic solvents.
The invention further provides the formed foil prepared by the preparation method, which does not contain residual carbide attached to the holes after sintering and has high capacity, high power-up efficiency and low leakage current.
In the preparation method, the first treatment liquid and the second treatment liquid can sufficiently clean and expand the pore of the residual carbide after sintering, and the formed oxide film has compact structure and excellent performance, and improves the capacity of the formed foil and the power-on efficiency.
Aiming at the problems of slow time for forming an oxide film, high energy consumption, multiple defects of the formed oxide film and the like in the subsequent formation process caused by the fact that valve metal wet coating is carried out on an aluminum foil in the prior art, dispersing agents and adhesive in a solvent are sintered, and residual carbide is attached to the surface of the valve metal, the invention reduces the residual carbide on the surface of the valve metal by designing a special formation pretreatment process, fully exerts the potential of a high dielectric layer of valve metal oxide, and obtains the anode foil with high specific volume.
Detailed Description
The present invention will be described in detail with reference to the following examples, but it should be understood that the examples are only illustrative of the present invention and are not intended to limit the scope of the present invention in any way. All reasonable variations and combinations that are included within the scope of the inventive concept fall within the scope of the present invention.
The base sintered foils used in the following examples were all obtained by the following procedure:
(1) Performing alkaline washing, acid washing and degreasing on the aluminum foil, and drying;
(2) Mixing titanium powder, an adhesive, a dispersing agent polyacrylic acid and a solvent ethylene glycol methyl ether, and uniformly stirring to obtain a viscous slurry, wherein the adhesive is a mixture of n-butyl titanate and polyacrylate in a volume ratio of 1:2.5;
(3) Coating slurry on one surface of the dried aluminum foil, trowelling, covering the slurry with another aluminum foil, enabling the slurry to be attached to the surfaces of the aluminum foil up and down, putting a sample into a drying furnace after finishing, and drying and degreasing at 150 ℃ for 1-2 hours to obtain a presintered foil;
(4) And (3) carrying out heat treatment on the pre-sintered foil for 10-24 hours at 500-580 ℃ under the protection of inert gas to obtain the basic sintered foil.
Example 1
The formation foil for aluminum electrolytic capacitor is prepared by the steps of:
(1) Placing the base sintered foil obtained after the sintering process into a first treatment liquid with the pH value controlled at 4-6, and ultrasonically cleaning for 3min at 85 ℃, wherein the first treatment liquid contains 1g/L citric acid, 0.2g/L polyepoxysuccinic acid and 0.3g/L adipic acid;
(2) Washing the treated foil obtained in the step (1) by flowing water, and roasting at 580 ℃ for 2.5min;
(3) Boiling the baked foil obtained in the step (2) in a second treatment liquid with the pH value controlled at 5-6 for 8min, wherein the second treatment liquid contains 0.15g/L monoammonium phosphate, 0.2g/L sodium phosphate and 0.5g/L sodium tetraborate;
(4) Performing four-stage formation treatment on the treated foil obtained in the step (3) to obtain a formed foil; the four-stage formation treatment specifically comprises:
and (3) primary formation: placing the foil treated in the step (3) into a primary formation liquid for formation treatment, wherein the primary formation liquid comprises 1-2.5g/L triethanolamine, 1-3g/L metaboric acid, 1.5-5g/L ammonium pentaborate, 4-6g/L ammonium azelate and 6-8g/L fumaric acid, the temperature of the bath liquid is controlled at 80-90 ℃, the voltage is 150-200v, and the current density is 0.3-0.5A/cm 2 The time is 5-10min;
and (3) secondary formation: processing the primary productThe foil is put into a secondary formation liquid for formation treatment, the secondary formation liquid comprises 0.5-2g/L triethanolamine, 5-10g/L ammonium pentaborate, 3-5g/L ammonium azelate hydrogen, 3-6g/L fumaric acid and 10-25g/L metaboric acid, the temperature of the bath liquid is controlled at 80-90 ℃, the voltage is 300-350v, and the current density is 0.3-0.5A/cm 2 The time is 5-10min;
cleaning: placing the foil subjected to the secondary formation treatment into a cleaning tank for cleaning;
and (3) three-stage formation: placing the cleaned foil into a three-stage formation liquid for formation treatment, wherein the three-stage formation liquid comprises 30-50g/L metaboric acid, 1-5g/L fumaric acid, 2-4g/L ammonium azelate hydrogen, the temperature of the bath liquid is controlled at 80-90 ℃, the voltage is 400-450v, and the current density is 0.3-0.5A/cm 2 The time is 5-10min;
four-stage formation: placing the foil subjected to the three-stage formation treatment into a four-stage formation liquid for formation treatment, wherein the four-stage formation liquid comprises 50-60g/L metaboric acid and 2-4g/L ammonium azelate hydrogen ammonium, the temperature of the bath liquid is controlled at 80-90 ℃, the voltage is 530v, and the current density is 0.3-0.5A/cm 2 The time is 10-15min;
(5) Cleaning the obtained formed foil, and then placing the cleaned foil into a roasting furnace to be roasted for 2min at 520-550 ℃ to obtain a first roasted foil;
(6) The first baked foil is put into a four-stage formation liquid for repair treatment, and the first repair foil is obtained, wherein in the repair treatment, the formation liquid temperature is controlled to be 80-90 ℃, the voltage is 530v, and the current density is 0.3-0.5A/cm 2 The time is 5-10min;
(7) Placing the first repair foil into 10 mass percent phosphoric acid, soaking for 150-180s, and cleaning;
(8) Putting the cleaned foil obtained in the step (7) into a four-stage formation liquid for restoration treatment to obtain a second restoration foil, wherein the formation liquid is controlled at 80-90 ℃ and has the voltage of 530v and the current density of 0.3-0.5A/cm 2 The time is 5-10min;
(9) Cleaning the second repair foil, and then placing the cleaned second repair foil into a roasting furnace to be roasted for 2min at 430-500 ℃ to obtain a second roasted foil;
(10) Putting the second baked foil into a four-stage formation liquid for repair treatment to obtainThird repairing foil, in repairing treatment, the temperature of the formation liquid is controlled at 80-90deg.C, the voltage is 530v, and the current density is 0.3-0.5A/cm 2 The time is 5-10min;
(11) Adding the third repair foil into ammonium dihydrogen phosphate post-treatment liquid with the concentration of 0.5g/L, and soaking at 50-60 ℃ for 6min to obtain a post-treatment foil;
(12) And (5) placing the post-treatment foil into a drying box, and drying at 200 ℃ to obtain the formed foil.
The capacity of the resulting formed foil was tested to be 20% higher than that obtained by conventional processes.
Example 2
The formed foil is prepared by the steps of:
(1) Placing the base sintered foil obtained after the sintering process into a first treatment liquid with the pH value controlled at 4-6, and ultrasonically cleaning for 3min at 85 ℃, wherein the first treatment liquid contains 3g/L citric acid, 0.3g/L polyepoxysuccinic acid and 0.5g/L adipic acid;
(2) Washing the treated foil obtained in the step (1) by flowing water, and roasting at 580 ℃ for 2.5min;
(3) Boiling the baked foil obtained in the step (2) in a second treatment liquid with the pH value controlled at 5-6 for 8min, wherein the second treatment liquid contains 0.15g/L monoammonium phosphate, 0.2g/L sodium phosphate and 0.5g/L sodium tetraborate;
(4) The treated foil obtained in step (3) was subjected to a chemical conversion treatment in accordance with the procedures (4) to (12) in example 1, to obtain a chemical conversion foil.
Example 3
The formed foil is prepared by the steps of:
(1) Placing the base sintered foil obtained after the sintering process into a first treatment liquid with the pH value controlled at 4-6, and ultrasonically cleaning for 3min at 85 ℃, wherein the first treatment liquid contains 5g/L citric acid, 0.4g/L polyepoxysuccinic acid and 0.7g/L adipic acid;
(2) Washing the treated foil obtained in the step (1) by flowing water, and roasting at 580 ℃ for 2.5min;
(3) Boiling the baked foil obtained in the step (2) in a second treatment liquid with the pH value controlled at 5-6 for 8min, wherein the second treatment liquid contains 0.15g/L monoammonium phosphate, 0.2g/L sodium phosphate and 0.5g/L sodium tetraborate;
(4) The treated foil obtained in step (3) was subjected to a chemical conversion treatment in accordance with the procedures (4) to (12) in example 1, to obtain a chemical conversion foil.
Example 4
The formed foil is prepared by the steps of:
(1) Placing the base sintered foil obtained after the sintering process into a first treatment liquid with the pH value controlled at 4-6, and ultrasonically cleaning for 3min at 85 ℃, wherein the first treatment liquid contains 3g/L citric acid, 0.3g/L polyepoxysuccinic acid and 0.5g/L adipic acid;
(2) Washing the treated foil obtained in the step (1) by flowing water, and roasting at 580 ℃ for 2.5min;
(3) Boiling the baked foil obtained in the step (2) in a second treatment liquid with the pH value controlled at 5-6 for 8min, wherein the second treatment liquid contains 0.1g/L monoammonium phosphate, 0.1g/L sodium phosphate and 0.5g/L sodium tetraborate;
(4) The treated foil obtained in step (3) was subjected to a chemical conversion treatment in accordance with the procedures (4) to (12) in example 1, to obtain a chemical conversion foil.
Example 5
The formed foil is prepared by the steps of:
(1) Placing the base sintered foil obtained after the sintering process into a first treatment liquid with the pH value controlled at 4-6, and ultrasonically cleaning for 3min at 85 ℃, wherein the first treatment liquid contains 3g/L citric acid, 0.3g/L polyepoxysuccinic acid and 0.5g/L adipic acid;
(2) Washing the treated foil obtained in the step (1) by flowing water, and roasting at 580 ℃ for 2.5min;
(3) Boiling the baked foil obtained in the step (2) in a second treatment liquid with the pH value controlled at 5-6 for 8min, wherein the second treatment liquid contains 0.2g/L monoammonium phosphate, 0.3g/L sodium phosphate and 0.5g/L sodium tetraborate;
(4) The treated foil obtained in step (3) was subjected to a chemical conversion treatment in accordance with the procedures (4) to (12) in example 1, to obtain a chemical conversion foil.
Example 6
The formed foil is prepared by the steps of:
(1) Placing the base sintered foil obtained after the sintering process into a first treatment liquid with the pH value controlled at 4-6, and ultrasonically cleaning for 3min at 85 ℃, wherein the first treatment liquid contains 3g/L citric acid, 0.3g/L polyepoxysuccinic acid and 0.5g/L adipic acid;
(2) Washing the treated foil obtained in the step (1) by flowing water, and roasting at 580 ℃ for 2.5min;
(3) Boiling the baked foil obtained in the step (2) in a second treatment liquid with the pH value controlled at 5-6 for 8min, wherein the second treatment liquid contains 0.15g/L monoammonium phosphate, 0.2g/L sodium phosphate and 0.5g/L sodium tetraborate;
(4) The treated foil obtained in step (3) was subjected to a chemical conversion treatment in accordance with the procedures (4) to (12) in example 1, to obtain a chemical conversion foil.
Example 7
The formed foil is prepared by the steps of:
(1) Placing the base sintered foil obtained after the sintering process into a first treatment liquid with the pH value controlled at 4-6, and ultrasonically cleaning for 3min at 60 ℃, wherein the first treatment liquid contains 3g/L citric acid, 0.3g/L polyepoxysuccinic acid and 0.5g/L adipic acid;
(2) Washing the treated foil obtained in the step (1) by flowing water, and roasting at 550 ℃ for 2.5min;
(3) Boiling the baked foil obtained in the step (2) in a second treatment liquid with the pH value controlled at 5-6 for 6min, wherein the second treatment liquid contains 0.15g/L monoammonium phosphate, 0.2g/L sodium phosphate and 0.5g/L sodium tetraborate;
(4) The treated foil obtained in step (3) was subjected to a chemical conversion treatment in accordance with the procedures (4) to (12) in example 1, to obtain a chemical conversion foil.
Example 8
The formed foil is prepared by the steps of:
(1) Placing the base sintered foil obtained after the sintering process into a first treatment liquid with the pH value controlled at 4-6, and ultrasonically cleaning for 3min at 85 ℃, wherein the first treatment liquid contains 3g/L citric acid, 0.3g/L polyepoxysuccinic acid and 0.5g/L adipic acid;
(2) Washing the treated foil obtained in the step (1) by flowing water, and roasting at 550 ℃ for 2.5min;
(3) Boiling the baked foil obtained in the step (2) in a second treatment liquid with the pH value controlled at 5-6 for 8min, wherein the second treatment liquid contains 0.15g/L monoammonium phosphate, 0.2g/L sodium phosphate and 0.5g/L sodium tetraborate;
(4) And (3) placing the treated foil obtained in the step (3) into a boric acid solution with the mass percentage of 15%, and carrying out formation treatment at 520v to obtain the formed foil.
Example 9
The formed foil is prepared by the steps of:
(1) Placing the base sintered foil obtained after the sintering process into a first treatment liquid with the pH value controlled at 4-6, and ultrasonically cleaning for 3min at 85 ℃, wherein the first treatment liquid contains 3g/L citric acid, 0.3g/L polyepoxysuccinic acid and 0.5g/L adipic acid;
(2) Washing the treated foil obtained in the step (1) by flowing water, and roasting at 580 ℃ for 2.5min;
(3) Boiling the baked foil obtained in the step (2) in a second treatment liquid with the pH value controlled at 5-6 for 8min, wherein the second treatment liquid contains 0.15g/L monoammonium phosphate, 0.2g/L sodium phosphate and 0.5g/L sodium tetraborate;
(4) And (3) placing the treated foil obtained in the step (3) into a mixed solution of boric acid with the mass percentage of 10% and ammonium pentaborate with the mass percentage of 5%, and carrying out formation treatment at 520v voltage to obtain the formed foil.
Comparative example 1
The formed foil is prepared by the steps of:
(1) The basic sintered foil obtained after the sintering process is put into pure water to be boiled for 10min;
(2) The treated foil obtained in step (1) was subjected to a chemical conversion treatment in accordance with the procedures (4) to (12) in example 1, to obtain a chemical conversion foil.
Comparative example 2
The formed foil is prepared by the steps of:
(1) The basic sintered foil obtained after the sintering process is put into pure water to be boiled for 10min;
(2) And (3) placing the treated foil obtained in the step (1) into a boric acid solution with the mass percentage of 15%, and carrying out formation treatment at 520v to obtain the formed foil.
Comparative example 3
The formed foil is prepared by the steps of:
(1) The basic sintered foil obtained after the sintering process is put into pure water to be boiled for 10min;
(2) And (3) placing the treated foil obtained in the step (1) into a mixed solution of boric acid with the mass percentage of 10% and ammonium pentaborate with the mass percentage of 5%, and carrying out formation treatment at 520v voltage to obtain the formed foil.
Comparative example 4
The formed foil is prepared by the steps of:
(1) Placing the base sintered foil obtained after the sintering process into a first treatment liquid with the pH value controlled at 4-6, and ultrasonically cleaning for 3min at 85 ℃, wherein the first treatment liquid contains 1g/L citric acid, 0.2g/L polyepoxysuccinic acid and 0.3g/L adipic acid;
(2) Washing the treated foil obtained in the step (1) by flowing water, and roasting at 580 ℃ for 2.5min;
(3) The baked foil obtained in the step (2) was subjected to formation treatment in the procedures of (4) to (12) in example 1 to obtain a formed foil.
Comparative example 5
The formed foil is prepared by the steps of:
(1) Washing and cleaning the basic sintered foil obtained after the sintering process by flowing water, and roasting at 580 ℃ for 2.5min;
(2) Boiling the baked foil obtained in the step (1) in a second treatment liquid with the pH value controlled at 5-6 for 8min, wherein the second treatment liquid contains 0.15g/L monoammonium phosphate, 0.2g/L sodium phosphate and 0.5g/L sodium tetraborate;
(3) The treated foil obtained in the step (2) was subjected to a formation treatment in accordance with the procedures (4) to (12) in example 1, to obtain a formed foil.
The foils obtained in examples 1 to 9 and comparative examples 1 to 5 were tested. The test using apparatus includes: a foil-forming TV characteristic tester, a foil-forming LCR tester, a bending machine and a measuring tank with the capacity of 1000 ml.
The leakage current, the withstand voltage and the withstand voltage boosting time are tested by a TV characteristic tester, the test temperature is 85 ℃, the test solution is 1000ml containing 70g boric acid, the resistivity is 7.5+/-0.3 KΩ & cm, the pH value is 3.2, and the test current is 2.0+/-0.2 mA. In the test, the time from the start of energization to the 90% voltage (Vr) of the rated film withstand voltage (Vf) was recorded as the rise time, and after the test for 3 minutes, the performance parameters such as the withstand voltage value, the withstand voltage boosting time, and the leakage current were read.
The capacity was measured by an LCR tester, the test solution was 1000ml of pure water containing 80g of ammonium pentaborate, the resistivity thereof was 30.+ -.5. Omega. Cm, the pH thereof was 7.4, and the test temperature thereof was 30 ℃.
The bending data are tested by a bending instrument.
The results are as follows:
table 1 comparative foil properties of examples and comparative examples
It can be seen that the foils of examples 1-9, which were pretreated and formed by the present invention, were higher in capacity than the foils prepared in the prior art, and had the advantages of shorter boost time and lower leakage current after removal of the carbide forming oxide film. And wherein the effects of example 1 and example 2 are more excellent. Meanwhile, the performance of the product treated by the two treatment liquids together is obviously better than that of the product treated by singly using any one of the treatment liquids
The above examples are only preferred embodiments of the present invention, and the scope of the present invention is not limited to the above examples. All technical schemes belonging to the concept of the invention belong to the protection scope of the invention. It should be noted that modifications and adaptations to the present invention may occur to one skilled in the art without departing from the principles of the present invention and are intended to be within the scope of the present invention.
Claims (10)
1. A method for producing a formed foil for an aluminum electrolytic capacitor, comprising:
(1) Placing the base sintered foil obtained after the sintering process into a first treatment liquid with the pH value controlled at 4-6, and performing ultrasonic cleaning at 60-80 ℃ to obtain a first treatment foil;
(2) Cleaning the first treated foil, and roasting at 550-580 ℃ for 1.5-2.5min to obtain a first roasted foil;
(3) Placing the first baked foil into a second treatment liquid with the pH value controlled between 5 and 6 to be boiled, so as to obtain a second treatment foil;
(4) Carrying out formation treatment on the second treatment foil to obtain a formation foil;
wherein the first treatment liquid comprises: citric acid with the concentration of 1-5g/L, polyepoxysuccinic acid with the concentration of 0.2-0.4g/L and adipic acid with the concentration of 0.3-0.8 g/L; the second treatment liquid includes: phosphate with a concentration of 0.05-0.5g/L and borate with a concentration of 0.1-1.0 g/L.
2. The method of claim 1, wherein the ultrasonic cleaning is for 1-3 minutes; and/or, the roasting time is 1.5-2.5min; and/or, the boiling time is 5-8min.
3. The method according to claim 1, wherein the phosphate comprises a first phosphate and a second phosphate, the first phosphate being monoammonium phosphate, and the concentration of the first phosphate in the second treatment liquid being 0.05-0.15g/L; and in the second treatment liquid, the concentration of the second phosphate is 0.1-0.3g/L, and the concentration of the borate is 0.1-0.8g/L.
4. The preparation method according to claim 1, wherein the phosphate comprises a first phosphate and a second phosphate, the first phosphate is monoammonium phosphate, and the second phosphate is one or more selected from sodium phosphate, potassium phosphate, sodium pyrophosphate, monoammonium phosphate; the borate is selected from ammonium pentaborate and/or sodium tetraborate.
5. The method of claim 1, wherein the chemical conversion process comprises: and (3) placing the second treatment foil into a boric acid solution with the mass percentage of 15%, and carrying out formation at the voltage of 500-540 v.
6. The method of claim 1, wherein the chemical conversion process comprises: and (3) placing the second treatment foil into a mixed solution of 10 mass percent of boric acid and 5 mass percent of ammonium pentaborate, and carrying out formation at a voltage of 500-540 v.
7. The method of claim 1, wherein the chemical conversion process is a four-stage chemical conversion process.
8. The method of manufacturing according to claim 1, characterized in that the base sintered foil is obtained by the following manufacturing process:
mixing titanium powder, an adhesive, a dispersing agent and an organic solvent to obtain mixed slurry;
coating the mixed slurry on the surface of a first aluminum foil after degreasing and drying, covering a second aluminum foil after degreasing and drying on the mixed slurry, bonding up and down, and drying and degreasing at 150 ℃ for 1-2 hours to obtain a presintered foil;
and carrying out heat treatment on the pre-sintered foil for 10-24 hours at 500-580 ℃ in an inert atmosphere to obtain the basic sintered foil.
9. The preparation method according to claim 1, wherein the adhesive is one or more selected from epoxy resin, phenolic resin, polyurethane and polyacrylate; the dispersing agent is one or more selected from polyacrylic acid, fatty acid and polyacrylamide; the organic solvent is selected from alcohols and/or lipid organic solvents.
10. A formed foil obtainable by the method according to any one of claims 1 to 9.
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| CN117524735B (en) * | 2024-01-05 | 2024-04-05 | 西安稀有金属材料研究院有限公司 | Preparation method of capacitor electrode material |
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