CN115172059A - Method for preparing aluminum electrolytic capacitor anode foil by combining aerosol spraying method - Google Patents
Method for preparing aluminum electrolytic capacitor anode foil by combining aerosol spraying method Download PDFInfo
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- CN115172059A CN115172059A CN202210951468.3A CN202210951468A CN115172059A CN 115172059 A CN115172059 A CN 115172059A CN 202210951468 A CN202210951468 A CN 202210951468A CN 115172059 A CN115172059 A CN 115172059A
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- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 title claims abstract description 196
- 229910052782 aluminium Inorganic materials 0.000 title claims abstract description 192
- 239000011888 foil Substances 0.000 title claims abstract description 138
- 238000005507 spraying Methods 0.000 title claims abstract description 89
- 238000000034 method Methods 0.000 title claims abstract description 69
- 239000003990 capacitor Substances 0.000 title claims abstract description 55
- 239000000443 aerosol Substances 0.000 title claims abstract description 43
- 239000000843 powder Substances 0.000 claims abstract description 38
- 238000011282 treatment Methods 0.000 claims abstract description 32
- 239000002131 composite material Substances 0.000 claims abstract description 30
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 24
- 238000005245 sintering Methods 0.000 claims abstract description 23
- 230000008569 process Effects 0.000 claims abstract description 22
- 238000009835 boiling Methods 0.000 claims abstract description 21
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 21
- 230000015572 biosynthetic process Effects 0.000 claims abstract description 15
- 239000011230 binding agent Substances 0.000 claims abstract description 14
- 239000002270 dispersing agent Substances 0.000 claims abstract description 13
- AZDRQVAHHNSJOQ-UHFFFAOYSA-N alumane Chemical class [AlH3] AZDRQVAHHNSJOQ-UHFFFAOYSA-N 0.000 claims abstract description 12
- 238000002156 mixing Methods 0.000 claims abstract description 7
- 238000010438 heat treatment Methods 0.000 claims description 37
- 239000000758 substrate Substances 0.000 claims description 35
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 21
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 claims description 14
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 8
- 230000003647 oxidation Effects 0.000 claims description 8
- 238000007254 oxidation reaction Methods 0.000 claims description 8
- 239000007787 solid Substances 0.000 claims description 7
- 239000007921 spray Substances 0.000 claims description 7
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 6
- 239000001856 Ethyl cellulose Substances 0.000 claims description 6
- ZZSNKZQZMQGXPY-UHFFFAOYSA-N Ethyl cellulose Chemical compound CCOCC1OC(OC)C(OCC)C(OCC)C1OC1C(O)C(O)C(OC)C(CO)O1 ZZSNKZQZMQGXPY-UHFFFAOYSA-N 0.000 claims description 6
- PRXRUNOAOLTIEF-ADSICKODSA-N Sorbitan trioleate Chemical compound CCCCCCCC\C=C/CCCCCCCC(=O)OC[C@@H](OC(=O)CCCCCCC\C=C/CCCCCCCC)[C@H]1OC[C@H](O)[C@H]1OC(=O)CCCCCCC\C=C/CCCCCCCC PRXRUNOAOLTIEF-ADSICKODSA-N 0.000 claims description 6
- 239000012298 atmosphere Substances 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 6
- 239000008367 deionised water Substances 0.000 claims description 6
- 229910021641 deionized water Inorganic materials 0.000 claims description 6
- 235000019325 ethyl cellulose Nutrition 0.000 claims description 6
- 229920001249 ethyl cellulose Polymers 0.000 claims description 6
- BNGXYYYYKUGPPF-UHFFFAOYSA-M (3-methylphenyl)methyl-triphenylphosphanium;chloride Chemical compound [Cl-].CC1=CC=CC(C[P+](C=2C=CC=CC=2)(C=2C=CC=CC=2)C=2C=CC=CC=2)=C1 BNGXYYYYKUGPPF-UHFFFAOYSA-M 0.000 claims description 5
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 claims description 5
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 claims description 5
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 claims description 5
- 239000005642 Oleic acid Substances 0.000 claims description 5
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 claims description 5
- DIZPMCHEQGEION-UHFFFAOYSA-H aluminium sulfate (anhydrous) Chemical compound [Al+3].[Al+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O DIZPMCHEQGEION-UHFFFAOYSA-H 0.000 claims description 5
- 239000004327 boric acid Substances 0.000 claims description 5
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 claims description 5
- 229920002678 cellulose Polymers 0.000 claims description 5
- 239000001913 cellulose Substances 0.000 claims description 5
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 claims description 5
- 238000009740 moulding (composite fabrication) Methods 0.000 claims description 5
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 claims description 5
- 229910052786 argon Inorganic materials 0.000 claims description 4
- IIZPXYDJLKNOIY-JXPKJXOSSA-N 1-palmitoyl-2-arachidonoyl-sn-glycero-3-phosphocholine Chemical compound CCCCCCCCCCCCCCCC(=O)OC[C@H](COP([O-])(=O)OCC[N+](C)(C)C)OC(=O)CCC\C=C/C\C=C/C\C=C/C\C=C/CCCCC IIZPXYDJLKNOIY-JXPKJXOSSA-N 0.000 claims description 3
- 239000004743 Polypropylene Substances 0.000 claims description 3
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 3
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 claims description 3
- YKTSYUJCYHOUJP-UHFFFAOYSA-N [O--].[Al+3].[Al+3].[O-][Si]([O-])([O-])[O-] Chemical compound [O--].[Al+3].[Al+3].[O-][Si]([O-])([O-])[O-] YKTSYUJCYHOUJP-UHFFFAOYSA-N 0.000 claims description 3
- COOGPNLGKIHLSK-UHFFFAOYSA-N aluminium sulfide Chemical compound [Al+3].[Al+3].[S-2].[S-2].[S-2] COOGPNLGKIHLSK-UHFFFAOYSA-N 0.000 claims description 3
- VXAUWWUXCIMFIM-UHFFFAOYSA-M aluminum;oxygen(2-);hydroxide Chemical compound [OH-].[O-2].[Al+3] VXAUWWUXCIMFIM-UHFFFAOYSA-M 0.000 claims description 3
- 239000000787 lecithin Substances 0.000 claims description 3
- 235000010445 lecithin Nutrition 0.000 claims description 3
- 229940067606 lecithin Drugs 0.000 claims description 3
- 229910052757 nitrogen Inorganic materials 0.000 claims description 3
- 229920000193 polymethacrylate Polymers 0.000 claims description 3
- -1 polypropylene Polymers 0.000 claims description 3
- 229920001155 polypropylene Polymers 0.000 claims description 3
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 3
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 claims description 2
- 238000005452 bending Methods 0.000 abstract description 12
- 239000011159 matrix material Substances 0.000 abstract description 8
- 230000001276 controlling effect Effects 0.000 abstract description 7
- 230000007797 corrosion Effects 0.000 abstract description 6
- 238000005260 corrosion Methods 0.000 abstract description 6
- 238000004519 manufacturing process Methods 0.000 abstract description 6
- 230000001105 regulatory effect Effects 0.000 abstract description 6
- 238000004804 winding Methods 0.000 abstract description 5
- 239000002994 raw material Substances 0.000 abstract description 4
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 abstract description 3
- 239000002360 explosive Substances 0.000 abstract description 3
- 231100000331 toxic Toxicity 0.000 abstract description 3
- 230000002588 toxic effect Effects 0.000 abstract description 3
- 238000005516 engineering process Methods 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 5
- 238000002360 preparation method Methods 0.000 description 5
- 238000005096 rolling process Methods 0.000 description 5
- 238000000231 atomic layer deposition Methods 0.000 description 4
- 238000010146 3D printing Methods 0.000 description 3
- 125000005619 boric acid group Chemical group 0.000 description 3
- 238000000576 coating method Methods 0.000 description 3
- 230000005684 electric field Effects 0.000 description 3
- 239000002244 precipitate Substances 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000000151 deposition Methods 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 239000002002 slurry Substances 0.000 description 2
- 230000003068 static effect Effects 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000007740 vapor deposition Methods 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- 239000002253 acid Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 239000010405 anode material Substances 0.000 description 1
- 238000000277 atomic layer chemical vapour deposition Methods 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 238000005238 degreasing Methods 0.000 description 1
- 230000032798 delamination Effects 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000006056 electrooxidation reaction Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 230000036571 hydration Effects 0.000 description 1
- 238000006703 hydration reaction Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 238000007747 plating Methods 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000007639 printing Methods 0.000 description 1
- FZUJWWOKDIGOKH-UHFFFAOYSA-N sulfuric acid hydrochloride Chemical compound Cl.OS(O)(=O)=O FZUJWWOKDIGOKH-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G9/00—Electrolytic capacitors, rectifiers, detectors, switching devices, light-sensitive or temperature-sensitive devices; Processes of their manufacture
- H01G9/004—Details
- H01G9/04—Electrodes or formation of dielectric layers thereon
- H01G9/042—Electrodes or formation of dielectric layers thereon characterised by the material
- H01G9/045—Electrodes or formation of dielectric layers thereon characterised by the material based on aluminium
-
- 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
-
- 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
Landscapes
- Engineering & Computer Science (AREA)
- Power Engineering (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Chemical & Material Sciences (AREA)
- Materials Engineering (AREA)
- Application Of Or Painting With Fluid Materials (AREA)
Abstract
The invention discloses a method for preparing an aluminum electrolytic capacitor anode foil by combining an aerosol spraying method, which comprises the following steps: 1. mixing a hydrochloric acid solution, aluminum salt powder and pure water, reacting to prepare an aluminum sol, and then adding a binder and a dispersing agent to obtain a composite aluminum sol; 2. spraying the composite alumina sol on the surface of the aluminum foil matrix and then curing; 3. and sequentially carrying out sintering, water boiling and formation treatment to obtain the anode foil of the aluminum electrolytic capacitor. The porosity and the thickness of the powder layer electronic aluminum foil are controlled by regulating and controlling the spraying parameters, so that the bending strength, the specific capacitance and the winding performance of the aluminum electrolytic capacitor anode foil are adjusted, different use requirements of the specific aluminum electrolytic capacitor anode foil are met, the production process is simple, the operation is easy, the porosity and the thickness of the powder layer electronic aluminum foil are effectively controlled, a complicated corrosion process is omitted, the cost is low, the efficiency is high, flammable and explosive or toxic raw materials are not needed, and the method is safe and environment-friendly.
Description
Technical Field
The invention belongs to the technical field of aluminum electrolytic capacitors, and particularly relates to a method for preparing an aluminum electrolytic capacitor anode foil by combining an aerosol spraying method.
Background
The aluminum electrolytic capacitor is one of the most important basic electronic elements, can be used as a filter and a bypass of an electronic circuit, and can also play roles in coupling, decoupling and the like. Because of its wide usability, aluminum electrolytic capacitors are widely used in fields such as electrical equipment, communication equipment, automotive equipment, and aerospace. The high-voltage anode electronic aluminum foil is an important component of an aluminum electrolytic capacitor, is a barrier type oxide film which grows on the surface of an aluminum electrode foil through anodic oxidation and is used as a dielectric layer of the aluminum electrolytic capacitor. At present, the high-voltage anode electronic aluminum foil is mainly obtained by carrying out electrochemical corrosion or chemical corrosion on the surface of an aluminum foil with a high cubic texture by using sulfuric acid-hydrochloric acid. The corrosion process of the high-voltage anode electronic aluminum foil is generally complex, and mainly relates to the technical processes of aluminum foil raw material, aluminum foil pretreatment, a first stage (aluminum foil hole forming stage), a second stage (aluminum foil hole forming stage), post-treatment, cleaning, drying and the like. The complex preparation process of the high-voltage anode electronic aluminum foil not only increases the processing cost, but also is difficult to reduce the cost for maintaining the quality stability, and simultaneously, the treatment of harmful substances such as waste acid, waste alkali and the like generated in the preparation process of the high-voltage anode electronic aluminum foil is difficult. Different from the traditional corrosion process, a method (powder layer electronic aluminum foil technology) for preparing the high-voltage anode electronic aluminum foil of the aluminum electrolytic capacitor by adopting a sintering method appears in the market at present, and the aluminum powder is sintered on the surface of an aluminum matrix to form a sandwich structure with a porous structure. The method saves the traditional corrosion link, and has the characteristics of simple process, low processing cost and environmental protection.
At present, the method for forming an aluminum film on the surface of an aluminum foil substrate mainly comprises the following steps: coating method, rolling method, electric field driven micro-scale 3D printing technology jetting method and gas phase deposition method. In the patent CN 112038099A, an aluminum film is printed on the surface of an aluminum foil substrate by adopting an electric field driving microscale 3D printing technology jet method; in patent CN 111804920A, aluminum powder particles are rolled to the surface of an aluminum foil matrix by a rolling method; in the patent CN 110718393A, an aluminum paste is coated on the surface of an aluminum foil substrate by a coating method to form an aluminum film; the patent CN 113436889A uses a vapor deposition method (atomic layer deposition method, chemical vapor deposition method and plasma enhanced atomic layer deposition method) to deposit a conductive metal film on the surface of the aluminum electrolytic capacitor anode foil dielectric layer. Among the above aluminum film production methods, the coating method is the most common film production method, and the operation method is simple, but the prepared slurry is difficult to store for a long time, and is easy to delaminate and precipitate, so that the aluminum film production method has a problem that it is difficult to use for a long time. The rolling method is generally considered as a simple film-making method, however, the difficulty of precisely controlling the rolling parameters in the rolling process so as to keep proper pores among aluminum powders exists; in addition, the aluminum powder is rolled on the surface of the aluminum film, and the aluminum film is likely to have powder falling phenomenon due to the absence of a binder. The electric field driving microscale 3D printing technology is an expensive technology, has high printing cost and low manufacturing efficiency, and is difficult to popularize and use at present. Also, vapor deposition methods (atomic layer deposition, chemical vapor deposition, and plasma-enhanced atomic layer deposition) have low plating efficiency, and the reaction source involved in the deposition and the residual gas after the reaction are flammable, explosive, or toxic, and the operator needs high protection requirements.
Disclosure of Invention
The technical problem to be solved by the present invention is to provide a method for preparing an aluminum electrolytic capacitor anode foil by combining an aerosol spraying method, aiming at the defects of the prior art. The method adopts an aerosol spraying method to spray and prepare the powder layer electronic aluminum foil, controls the porosity and the thickness of the powder layer electronic aluminum foil by regulating and controlling spraying parameters, further realizes the adjustment of the bending strength, the specific capacitance and the winding performance of the anode foil of the aluminum electrolytic capacitor, meets different use requirements of the anode foil of the specific aluminum electrolytic capacitor, and solves the defects of the prior preparation technology.
In order to solve the technical problems, the technical scheme adopted by the invention is as follows: a method for preparing aluminum electrolytic capacitor anode foil by combining aerosol spraying is characterized by comprising the following steps:
step one, mixing a hydrochloric acid solution, aluminum salt powder and pure water, reacting to prepare an aluminum sol, and uniformly dissolving a binder and a dispersant in the aluminum sol to obtain a composite aluminum sol;
step two, spraying the composite aluminum sol obtained in the step one on the surface of an aluminum foil matrix by adopting an aerosol spraying method, and then curing to obtain a cured aluminum foil; the aerosol spraying method comprises the following spraying parameters: the spraying pressure is 0.05MPa to 0.2MPa, the flow is 50 mu L/min to 300 mu L/min, the platform speed is 5mm/s to 30mm/s, and the height of the spray head from the base is 10cm to 25cm;
and step three, sequentially sintering, boiling and forming the cured aluminum foil obtained in the step two to obtain the aluminum electrolytic capacitor anode foil.
The invention firstly mixes and reacts hydrochloric acid solution, aluminum salt powder and pure water, and adds a binder and a dispersant, wherein the mass ratio of hydrochloric acid to aluminum salt is generally controlled to be 0.5 to 2.2: preparing composite aluminum sol which is not easy to precipitate and delaminate, spraying the composite aluminum sol by an aerosol spraying method to prepare an aerosol layer, and forming a powder layer electronic aluminum foil on the surface of the aluminum foil through curing, sintering, water boiling and formation treatment to obtain the anode foil of the aluminum electrolytic capacitor. In the preparation process, spraying parameters of an aerosol spraying method, namely spraying pressure, flow, platform speed and the height of a nozzle from a substrate, are regulated and controlled, specifically, the porosity of the powder layer electronic aluminum foil is reduced along with the increase of the spraying pressure, the thickness of the powder layer electronic aluminum foil is increased along with the increase of the flow, and the thickness of the powder layer electronic aluminum foil is reduced along with the increase of the platform speed, so that the porosity and the thickness of the powder layer electronic aluminum foil are effectively controlled, and by utilizing the characteristic that the porosity of the powder layer electronic aluminum foil is in positive correlation with the bending strength and in negative correlation with the specific capacity, and the characteristic that the thickness of the powder layer electronic aluminum foil is in negative correlation with the bending strength and in positive correlation with the specific capacity, the bending strength, the specific capacitance and the winding performance of the aluminum electrolytic capacitor anode foil are further regulated, and the aluminum electrolytic capacitor anode foil meeting specific use requirements is obtained.
The method for preparing the anode foil of the aluminum electrolytic capacitor by combining the aerosol spraying method is characterized in that in the step one, the mass fraction of the hydrochloric acid solution is 15-20%, and the aluminum salt powder is one or more than two of aluminum chloride, aluminum sulfate, aluminum nitrate, aluminum silicate, aluminum sulfide and pseudo-boehmite. The invention obtains the aluminum sol with proper proportion of each component by controlling the mass fraction of the hydrochloric acid solution, and ensures the formation of the aluminum sol with the viscosity suitable for aerosol spraying by combining the control of the type of the aluminum salt powder.
The method for preparing the anode foil of the aluminum electrolytic capacitor by combining the aerosol spraying method is characterized in that in the first step, the binder is one or more than two of ethyl cellulose, polyvinyl alcohol, polymethacrylate, carboxyl cellulose and polypropylene, and the dispersant is one or more than two of lecithin, oleic acid, span-85 and triethanolamine. According to the invention, the dispersant of the above kind is adopted to promote the uniform dispersion of each component in the composite aluminum sol, so that the precipitation delamination of the composite aluminum sol is avoided, and meanwhile, the kind of the added binder is controlled, so that the composite aluminum sol has excellent rheological property, is not easy to delaminate and precipitate in a short time, and ensures that the composite aluminum sol is bonded on the surface of an aluminum foil matrix in the subsequent spraying process, and aluminum salt powder particles are easy to bond; in addition, the price of the binder and the dispersant is relatively low, so that the preparation cost is reduced.
The method for preparing the anode foil of the aluminum electrolytic capacitor by combining the aerosol spraying method is characterized in that the solid content of the composite aluminum sol in the step one is 10-60%. According to the invention, the solid content of the composite aluminum sol is controlled to be 10-60%, so that the composite aluminum sol has proper adhesive property and flow property, can be well combined with an aluminum foil matrix in the subsequent spraying process, has good leveling property after spraying, and effectively ensures the thickness and uniformity of a sprayed layer.
The method for preparing the anode foil of the aluminum electrolytic capacitor by combining the aerosol spraying method is characterized in that before the spraying in the second step, the aluminum foil substrate is soaked in NaOH solution with the mass concentration of 0.1-10% for removing the oxidation film. According to the invention, the aluminum foil substrate is soaked in NaOH solution with the mass concentration of 0.1-10% for oxidation film removal treatment, so that an oxidation layer on the surface of the aluminum foil substrate is removed, and the aluminum foil substrate has degreasing and dust removing effects, so that the aluminum foil substrate is easy to combine with a spraying layer, and an aluminum raw material is better combined on the surface of the aluminum foil substrate in a subsequent sintering process.
The method for preparing the anode foil of the aluminum electrolytic capacitor by combining the aerosol spraying method is characterized in that in the second step, the thickness of the aluminum foil substrate is 30-60 mu m, and the spraying thickness of the composite aluminum sol is 60-80 mu m. According to the invention, by controlling the thickness of the aluminum foil substrate, the thickness of the spraying layer is increased, the use of the aluminum foil substrate is reduced, the cost is saved, and meanwhile, the problems that the mechanical strength is not favorable for curling and winding of the anode foil of the aluminum electrolytic capacitor due to the excessively thin aluminum foil substrate and the specific capacitance of the anode foil of the aluminum electrolytic capacitor is influenced due to the excessively thick aluminum foil substrate are avoided; according to the invention, by controlling the spraying thickness of the composite alumina sol, the thickness of the electronic aluminum foil of the powder layer is ensured to be 130-200 μm, and the problem that the subsequent use function is influenced because the specific capacitance performance cannot be ensured when the thickness is too small is avoided.
The method for preparing the aluminum electrolytic capacitor anode foil by combining the aerosol spraying method is characterized in that the curing temperature in the second step is 80-200 ℃. The invention controls the curing temperature to ensure that the composite alumina sol is primarily solidified, thereby facilitating the subsequent sintering.
The method for preparing the anode foil of the aluminum electrolytic capacitor by combining the aerosol spraying method is characterized in that the sintering treatment process in the third step is as follows: firstly, heating a cured aluminum foil to 250-300 ℃ at a heating rate of 5-20 ℃/min, preserving heat for 1h-4h, then heating to 350-500 ℃ at a heating rate of 5-20 ℃/min, preserving heat for 2h-8h, then heating to 600-650 ℃ at a heating rate of 5-20 ℃/min, preserving heat for 1h-24h, and then cooling along with a furnace; and the atmosphere in the furnace in the sintering treatment process is nitrogen, argon or vacuum. The invention adopts a three-stage heating sintering procedure, wherein the residual binder and dispersant in the solidified aluminum foil are removed at a lower temperature in the first two stages, and the electronic aluminum foil of the powder layer on the surface of the aluminum foil substrate is fully combined with the aluminum foil substrate at a higher temperature in the third stage, so that the structural strength of the anode foil of the aluminum electrolytic capacitor is enhanced.
The method for preparing the anode foil of the aluminum electrolytic capacitor by combining the aerosol spraying method is characterized in that deionized water is adopted for boiling treatment in the third step, and the boiling time is 10min to 20min. According to the invention, the deionized water is adopted for boiling to prevent other impurities from being introduced, and the boiling time is controlled to form a hydration film with proper thickness on the surface of the anode foil, so that the subsequent formation treatment is facilitated.
The method for preparing the anode foil of the aluminum electrolytic capacitor by combining the aerosol spraying method is characterized in that the solution adopted in the formation treatment in the third step is boric acid solution with the mass concentration of 10%, and the formation voltage is 520V. According to the invention, the oxide film is formed on the surface of the anode material through the formation treatment of the parameters, so that the anode foil of the aluminum electrolytic capacitor is obtained, and the specific capacitance performance of the anode foil of the aluminum electrolytic capacitor is improved.
Compared with the prior art, the invention has the following advantages:
1. the powder layer electronic aluminum foil is prepared by spraying by adopting an aerosol spraying method, the porosity and the thickness of the powder layer electronic aluminum foil are controlled by regulating and controlling spraying parameters, and the bending strength, the specific capacitance and the winding performance of the anode foil of the aluminum electrolytic capacitor are regulated by utilizing the relevant characteristics of the porosity, the bending strength and the specific capacity of the powder layer electronic aluminum foil and the relevant characteristics of the thickness, the bending strength and the specific capacity of the powder layer electronic aluminum foil, so that different use requirements of the anode foil of the specific aluminum electrolytic capacitor are met.
2. According to the invention, the hydrochloric acid solution, the aluminum salt powder and the pure water are mixed and then react, and the binder and the dispersing agent are added to prepare the composite aluminum sol which is not easy to precipitate and delaminate, so that the problems that the slurry obtained by the traditional method is easy to delaminate and precipitate and is difficult to store for a long time are solved.
3. Compared with the existing method for forming the aluminum film on the surface of the aluminum foil substrate, the method has the advantages of simple production process, easy operation, effective control of the porosity and the thickness of the electronic aluminum foil of the powder layer, omission of a complicated corrosion process, low cost, high efficiency, no need of flammable and explosive or toxic raw materials, and safety and environmental protection.
4. The powder layer electronic aluminum foil is prepared by spraying by adopting an aerosol spraying method, and due to the controllability of spraying parameters, the uniformity of aluminum powder dispersion in the spraying process is ensured, so that the thickness consistency and the performance stability of the powder layer electronic aluminum foil are ensured.
The technical solution of the present invention is further described in detail by examples below.
Detailed Description
Example 1
The embodiment comprises the following steps:
step one, mixing and reacting a hydrochloric acid solution with a mass fraction of 15%, aluminum chloride powder and pure water according to a mass ratio of 0.5; the solid content of the composite aluminum sol is 10%;
step two, spraying the composite aluminum sol obtained in the step one on the surface of an aluminum foil matrix by adopting an aerosol spraying method, and then curing at 150 ℃ to obtain a cured aluminum foil; before the spraying, the aluminum foil substrate is soaked in NaOH solution with the mass concentration of 0.1% to carry out oxidation film removing treatment; the aerosol spraying method comprises the following spraying parameters: the spraying pressure is 0.05MPa, the flow is 300 mu L/min, the platform speed is 15mm/s, and the height between the spray head and the substrate is 15cm; the thickness of the aluminum foil substrate is 30 micrometers, and the spraying thickness of the composite aluminum sol is 80 micrometers;
step three, sequentially sintering, boiling and forming the cured aluminum foil obtained in the step two to obtain an aluminum electrolytic capacitor anode foil; the sintering treatment process comprises the following steps: firstly, heating the solidified aluminum foil to 250 ℃ at the heating rate of 20 ℃/min and preserving heat for 1h, then heating to 400 ℃ at the heating rate of 20 ℃/min and preserving heat for 2h, then heating to 600 ℃ at the heating rate of 20 ℃/min and preserving heat for 24h, and then cooling along with the furnace; in the sintering treatment process, the furnace atmosphere is argon; the water boiling treatment adopts deionized water, and the boiling time is 15min; the solution adopted in the formation treatment is boric acid solution with the mass concentration of 10%, and the formation voltage is 520V.
The aluminum salt powder in this embodiment may be replaced with one or more of aluminum chloride, aluminum sulfate, aluminum nitrate, aluminum silicate, aluminum sulfide, and pseudo-boehmite in addition to the aluminum chloride powder; the binder in the embodiment may be replaced by one or more of ethyl cellulose other than ethyl cellulose, polyvinyl alcohol, polymethacrylate, carboxyl cellulose and polypropylene, and the dispersant may be replaced by one or more of lecithin other than span-85, oleic acid, span-85 and triethanolamine; in the process of sintering treatment in this embodiment, the furnace atmosphere may also be vacuum.
Comparative example 1
The comparative example comprises the following steps:
step one, mixing and reacting a hydrochloric acid solution with a mass fraction of 15%, aluminum chloride powder and pure water according to a mass ratio of 0.5; the solid content of the aluminum sol is 10 percent;
step two, spraying the aluminum sol obtained in the step one on the surface of an aluminum foil substrate by adopting an aerosol spraying method, and then curing at 150 ℃ to obtain a cured aluminum foil; before the spraying, the aluminum foil substrate is soaked in NaOH solution with the mass concentration of 0.1% to carry out oxidation film removing treatment; the aerosol spraying method comprises the following spraying parameters: the spraying pressure is 0.05MPa, the flow is 300 mu L/min, the platform speed is 15mm/s, and the height between the spray head and the substrate is 15cm; the thickness of the aluminum foil substrate is 30 micrometers, and the spraying thickness of the aluminum sol is 80 micrometers;
step three, sequentially sintering, boiling and forming the cured aluminum foil obtained in the step two to obtain an aluminum electrolytic capacitor anode foil; the sintering treatment process comprises the following steps: firstly, heating the solidified aluminum foil to 250 ℃ at the heating rate of 20 ℃/min and preserving heat for 1h, then heating to 400 ℃ at the heating rate of 20 ℃/min and preserving heat for 2h, then heating to 600 ℃ at the heating rate of 20 ℃/min and preserving heat for 24h, and then cooling along with a furnace; in the sintering treatment process, the furnace atmosphere is argon; the water boiling treatment adopts deionized water, and the boiling time is 15min; the solution adopted in the formation treatment is boric acid solution with the mass concentration of 10%, and the formation voltage is 520V.
Example 2
The present embodiment differs from embodiment 1 in that: in the first step, the aluminum salt powder is prepared by mixing aluminum sulfate and aluminum nitrate in a mass ratio of 1:1, and the solid content of the composite aluminum sol is 15 percent
Example 3
The present embodiment differs from embodiment 1 in that: in the first step, the binder is ethyl cellulose and carboxyl cellulose, the dispersant is oleic acid and span-85, the mass ratio of ethyl cellulose to carboxyl cellulose to oleic acid to span-85 is 2.
Example 4
The embodiment comprises the following steps:
step one, mixing and reacting 20% by mass of hydrochloric acid solution, aluminum chloride, aluminum sulfate, aluminum nitrate powder and pure water according to a mass ratio of 2.3; the solid content of the composite aluminum sol is 60 percent;
step two, spraying the composite aluminum sol obtained in the step one on the surface of an aluminum foil substrate by adopting an aerosol spraying method, and then curing at 80 ℃ to obtain a cured aluminum foil; before the spraying, the aluminum foil substrate is soaked in a NaOH solution with the mass concentration of 5% for removing an oxidation film; the aerosol spraying method comprises the following spraying parameters: the spraying pressure is 0.2MPa, the flow is 50 mu L/min, the platform speed is 5mm/s, and the height between the spray head and the substrate is 10cm; the thickness of the aluminum foil substrate is 40 micrometers, and the spraying thickness of the composite aluminum sol is 70 micrometers;
thirdly, sequentially sintering, boiling and forming the cured aluminum foil obtained in the second step to obtain an aluminum electrolytic capacitor anode foil; the sintering treatment process comprises the following steps: firstly, heating a solidified aluminum foil to 300 ℃ at a heating rate of 5 ℃/min and preserving heat for 2h, then heating to 350 ℃ at a heating rate of 5 ℃/min and preserving heat for 8h, then heating to 630 ℃ at a heating rate of 5 ℃/min and preserving heat for 10h, and then cooling along with a furnace; the furnace atmosphere in the sintering treatment process is nitrogen; the water boiling treatment adopts deionized water, and the boiling time is 10min; the solution adopted in the formation treatment is boric acid solution with the mass concentration of 10%, and the formation voltage is 520V.
Example 5
The present embodiment differs from embodiment 4 in that: step two, the mass concentration of NaOH solution adopted in the oxide film removing treatment is 10 percent; the aerosol spraying method comprises the following spraying parameters: spraying pressure is 0.1MPa, flow is 200 mu L/min, platform speed is 30mm/s, and the height of the spray head from the substrate is 25cm; the thickness of the aluminum foil matrix is 60 micrometers, and the spraying thickness of the composite aluminum sol is 60 micrometers; the curing temperature was 200 ℃.
Example 6
The present embodiment differs from embodiment 4 in that: the sintering treatment process in the third step comprises the following steps: firstly, heating the solidified aluminum foil to 280 ℃ at the heating rate of 10 ℃/min and preserving heat for 4h, then heating to 500 ℃ at the heating rate of 10 ℃/min and preserving heat for 2h, then heating to 650 ℃ at the heating rate of 10 ℃/min and preserving heat for 1h, and then cooling along with the furnace; the boiling time of the water boiling treatment is 20min.
The anode foils for aluminum electrolytic capacitors prepared in examples 1 to 6 of the present invention and comparative example 1 were tested using an LCR meter and an aluminum foil bending tester, and the obtained static specific capacities and the number of times of bending were as shown in table 1.
As can be seen from table 1, the anode foils for aluminum electrolytic capacitors prepared in examples 1 to 6 of the present invention have lower static specific capacities, all of which are smaller than comparative example 1, and more bending times, all of which are greater than comparative example 1, which indicates that the composite aluminum sol prepared by adding the binder and the dispersant according to the present invention, which is not easy to precipitate and delaminate, has better adhesion performance with the aluminum foil substrate after spraying, effectively controls the porosity of the sprayed layer, and improves the bending strength and specific capacitance of the anode foil for aluminum electrolytic capacitors.
The above description is only for the preferred embodiment of the present invention, and is not intended to limit the present invention in any way. Any simple modification, change and equivalent changes of the above embodiments according to the technical essence of the invention are still within the protection scope of the technical solution of the invention.
Claims (10)
1. A method for preparing aluminum electrolytic capacitor anode foil by combining aerosol spraying is characterized by comprising the following steps:
step one, mixing a hydrochloric acid solution, aluminum salt powder and pure water, reacting to prepare an aluminum sol, and then uniformly dissolving a binder and a dispersant in the aluminum sol to obtain a composite aluminum sol;
step two, spraying the composite aluminum sol obtained in the step one on the surface of an aluminum foil substrate by adopting an aerosol spraying method, and then curing to obtain a cured aluminum foil; the aerosol spraying method comprises the following spraying parameters: spraying pressure is 0.05MPa to 0.2MPa, flow is 50 mu L/min to 300 mu L/min, platform speed is 5mm/s to 30mm/s, and the height of a spray head from a substrate is 10cm to 25cm;
and step three, sequentially sintering, boiling and forming the cured aluminum foil obtained in the step two to obtain the aluminum electrolytic capacitor anode foil.
2. The method for preparing the anode foil of the aluminum electrolytic capacitor by combining the aerosol spraying method according to claim 1, wherein the mass fraction of the hydrochloric acid solution in the step one is 15-20%, and the aluminum salt powder is one or more than two of aluminum chloride, aluminum sulfate, aluminum nitrate, aluminum silicate, aluminum sulfide and pseudo-boehmite.
3. The method for preparing the anode foil of the aluminum electrolytic capacitor by combining the aerosol spraying method as claimed in claim 1, wherein the binder in the first step is one or more of ethyl cellulose, polyvinyl alcohol, polymethacrylate, carboxyl cellulose and polypropylene, and the dispersant is one or more of lecithin, oleic acid, span-85 and triethanolamine.
4. The method for preparing the anode foil of the aluminum electrolytic capacitor by combining the aerosol spraying method according to claim 1, wherein the solid content of the composite aluminum sol in the first step is 10-60%.
5. The method for preparing the anode foil of the aluminum electrolytic capacitor by combining the aerosol spraying method according to claim 1, wherein before the spraying in the second step, the aluminum foil substrate is soaked in a NaOH solution with a mass concentration of 0.1-10% for removing the oxidation film.
6. The method for preparing the anode foil of the aluminum electrolytic capacitor by combining the aerosol spraying method according to claim 1, wherein the thickness of the aluminum foil substrate in the second step is 30 to 60 μm, and the spraying thickness of the composite aluminum sol is 60 to 80 μm.
7. The method for preparing the anode foil of the aluminum electrolytic capacitor by combining the aerosol spraying method according to claim 1, wherein the curing temperature in the second step is 80 ℃ to 200 ℃.
8. The method for preparing the anode foil of the aluminum electrolytic capacitor by combining the aerosol spraying method according to claim 1, wherein the sintering process in the third step is as follows: firstly, heating a cured aluminum foil to 250-300 ℃ at a heating rate of 5-20 ℃/min, preserving heat for 1h-4h, then heating to 350-500 ℃ at a heating rate of 5-20 ℃/min, preserving heat for 2h-8h, then heating to 600-650 ℃ at a heating rate of 5-20 ℃/min, preserving heat for 1h-24h, and then cooling along with a furnace; the atmosphere in the furnace in the sintering treatment process is nitrogen, argon or vacuum.
9. The method for preparing the anode foil of the aluminum electrolytic capacitor by combining the aerosol spraying method as claimed in claim 1, wherein the water boiling treatment in the third step is deionized water, and the boiling time is 10min to 20min.
10. The method for preparing the anode foil of the aluminum electrolytic capacitor by combining the aerosol spraying method according to claim 1, wherein the solution used in the formation treatment in the third step is a boric acid solution with a mass concentration of 10%, and the formation voltage is 520V.
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