CN101483103B - Corrosion method for aluminum electrolysis capacitor anode foil - Google Patents
Corrosion method for aluminum electrolysis capacitor anode foil Download PDFInfo
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- CN101483103B CN101483103B CN2009100953001A CN200910095300A CN101483103B CN 101483103 B CN101483103 B CN 101483103B CN 2009100953001 A CN2009100953001 A CN 2009100953001A CN 200910095300 A CN200910095300 A CN 200910095300A CN 101483103 B CN101483103 B CN 101483103B
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Abstract
The present invention relates to an anode foil corrosion method for aluminum electrolytic capacitor, belonging to the manufacture field of aluminum electrolytic capacitor. Through the method, not only the middle-and high-voltage anode foil corrosion problem is solved, but also the anode foil has good mechanical high strength and saved cost on the premise of specific volume. The method includes: performing pretreatment to the aluminum optical foil; performing a first stage direct current electrolytic corrosion to the aluminum foil after pretreatment in the mixed solution of 3-10wt% of hydrochloric acid and 0.6-6wt% of sulfuric acid; subsequently performing a second stage chemical corrosion in a mixed solution of 3 - 10wt% of hydrochloric acid, 0.01-0.5wt% of phosphoric acid and 0.1-0.2wt% of polyethylene glycol (whose molecular weight is 20000); finally soaking in 0.2-3wt% of nitric acid aqueous solution. The process increases the surface expansion rate of aluminum foil, substantially increases its specific volume, and simultaneously has no loss of mechanical strength.
Description
Technical field
The present invention relates to a kind of caustic solution of anode foil for aluminum electrolytic capacitor, belong to aluminium electrolytic capacitor and make the field.
Background technology
Anode foil for aluminum electrolytic capacitor in order to improve specific volume, generally adopts electrochemical etching method to increase the effective surface area of aluminium foil, wherein mainly comprises the initiation of initial pit of aluminium foil surface and the counter-boring techniques of aluminium foil pit.The research of relevant corrosion reaming aspect has many reports, and the past caustic solution is the electricity consumption chemical enlargement, and the present invention adopts the chemical corrosion reaming.
The caustic solution of recent Chinese patent application (200410041286.4) 63WV～100WV high specific volume anode foil: this caustic solution carries out pre-treatment with optical aluminum foil, then at concentration 0.1～1wt% sulfuric acid, carry out communication pre-corrosion in 5～20wt% hydrochloric acid mixed solution, then at concentration 10～25wt% hydrochloric acid, 0.1 soak in the mixed solution of～1wt% sulfuric acid and 0.01～10ppm copper ion, again at concentration 0.1～1wt% sulfuric acid, 10～25wt% hydrochloric acid, 0.01～1wt% thiocarbamide, 0.01～1wt% oxalic acid, 0.2 carry out AC corrosion in the mixed solution of～5wt% alchlor, in the aqueous solution of nitric acid of concentration 1～10wt%, soak at last.This caustic solution caustic solution in the past can improve the area expanding rate of aluminium foil, but this caustic solution can only corrode at the low-voltage anode foil of 63WV～100WV, and relatively poor for the corrosive effect of the high-voltage anode paper tinsel that surpasses 100WV.Adopt AC corrosion, because the corrosion aperture is less, high pressure easily stops up when forming.
Summary of the invention
The caustic solution that the present invention is directed to existing anode foils can only corrode and can't corrode the caustic solution that existing defective provides a kind of mesohigh anode foils to the anode foils of mesohigh the anode foils of low pressure; Not only solved the etching problem of mesohigh anode foils by this method, anode foils is obtaining to have good mechanical strength under the high specific volume prerequisite, and saves cost.
Above-mentioned technical problem of the present invention is implemented by the following technical programs: a kind of caustic solution of aluminum electrolysis capacitor anode foil, and this method may further comprise the steps:
A, pre-treatment: aluminium foil is placed in the mixed solution of 0.6～6wt% sulfuric acid and 3～10wt% hydrochloric acid and soaked 2～3 minutes;
B, the corrosion of one-level dc electrolysis: the mixed solution that above-mentioned aluminium foil through pre-treatment is put into 0.6～6wt% sulfuric acid and 3～10wt% hydrochloric acid carries out the corrosion of one-level dc electrolysis;
C, secondary chemical corrosion: the mixed solution that above-mentioned aluminium foil through the corrosion of one-level dc electrolysis is put into hydrochloric acid, 0.01～0.5wt% phosphoric acid and the 0.1～0.2wt% polyethylene glycol of 3～10wt% carries out the secondary chemical corrosion;
D, reprocessing: above-mentioned aluminium foil through the secondary chemical corrosion was soaked 4～6 minutes in the aqueous solution of nitric acid of, 0.2～3wt%.
The caustic solution of above-mentioned aluminum electrolysis capacitor anode foil, as preferably, in pre-treatment, aluminium foil in mixed solution soaking temperature at 60～75 ℃.
The caustic solution of above-mentioned aluminum electrolysis capacitor anode foil, as preferably, in the corrosion of one-level dc electrolysis, current density is 25～35A/dm
2, electric weight is 1900～2600C/dm
2
The caustic solution of above-mentioned aluminum electrolysis capacitor anode foil, as preferably, in the corrosion of one-level dc electrolysis, the temperature of described mixed solution is 70 ℃～85 ℃.
The caustic solution of above-mentioned aluminum electrolysis capacitor anode foil, as preferably, in the secondary chemical corrosion, the temperature of described mixed solution is 60 ℃～90 ℃.
The caustic solution of above-mentioned aluminum electrolysis capacitor anode foil, as preferably, in the corrosion of secondary dc electrolysis, the molecular weight of described polyethylene glycol is 20000～30000.
The caustic solution of above-mentioned aluminum electrolysis capacitor anode foil, as preferably, in reprocessing, aluminium foil in aqueous solution of nitric acid soaking temperature at 50 ℃～80 ℃.
Pre-treatment main purpose of the present invention is to remove the greasy dirt of aluminium foil surface, impurity, makes the paper tinsel surface evenly, forms equally distributed initial pit when helping the corrosion of one-level dc electrolysis.
One-level dc electrolysis of the present invention corrosion main purpose is to cause initial pit at aluminium foil surface, and make the pit aperture size reasonable, be evenly distributed.It is bigger that employing DC power supply ratio employing AC power is corroded formed aperture, and pit is difficult for obstruction when forming.
The purpose of secondary chemical corrosion of the present invention is reaming on the basis of initial pit, makes the aperture of etch pit satisfy the requirement that mesohigh changes into.
Reprocessing purpose of the present invention is to remove aluminium foil surface metal remained impurity, through aluminium foil surface metal impurities residual quantity≤1mg/m after the reprocessing
2
In sum: the present invention compares with prior art has following advantage:
Adopt caustic solution of the present invention not only to solve the etching problem of mesohigh anode foils, improved the area expanding rate of aluminium foil, the mesohigh anode foils is obtaining to have good mechanical strength under the high specific volume prerequisite, and cost reduces.
Embodiment
Below by embodiment, technical scheme of the present invention is described in further detail; But the present invention is not limited to these embodiment.
Embodiment 1
Many and paper tinsel corrodes and it is changed into to 110 μ m Xinjiang to adopt caustic solution of the present invention, and concrete operating process is as follows:
1, pre-treatment:
With aluminium foil (Xinjiang many and 110 μ m paper tinsels) be placed on soak 2 minutes in the mixed solution that 65 ℃, concentration are 5wt% sulfuric acid and 4wt% hydrochloric acid after, taking-up.
2, one-level dc electrolysis corrosion:
To be placed on temperature through the aluminium foil after the pre-treatment be 80 ℃ with above-mentioned, and concentration is to carry out the corrosion of one-level dc electrolysis in the sulfuric acid of 5wt% and the 4wt% hydrochloric acid mixed solution, and current density is 25A/dm
2, electric weight is 2000C/dm
2
3, secondary chemical corrosion:
Above-mentioned aluminium foil through the corrosion of secondary dc electrolysis is placed in the mixed solution that concentration is 4wt% hydrochloric acid, 0.02wt% phosphoric acid and 0.1wt% polyethylene glycol (molecular weight is 20000) carries out the secondary chemical corrosion, the parameters of mixed solution is:
Temperature: 80 ℃
Time: 20 minutes.
4, reprocessing:
Is that 60 ℃, concentration are to soak in the aqueous solution of nitric acid of 1wt% to change in 5 minutes with above-mentioned aluminium foil through the secondary chemical corrosion in temperature;
Wherein the condition of changing into is:
90 ℃ of 0.05A/dm of 10% boric acid
2Vfe=200V 610V
Be respectively through 110 μ m Xinjiang of embodiment 1 and chemical synthesizing method production every performance many and that paper tinsel reaches:
C
200Vf=2.35～2.45 μ F/cm
2C
610Vf=0.52～0.53 μ F/cm
2Tensile strength=21.0N/cm.
Embodiment 2
Adopt caustic solution of the present invention that 115 μ m Mitsubishi paper tinsels are corroded and it is changed into, concrete operating process is as follows:
1, pre-treatment:
With aluminium foil (115 μ m Mitsubishi paper tinsel) be placed on soak 2 minutes in the mixed solution that 67 ℃, concentration are 6wt% sulfuric acid and 3wt% hydrochloric acid after, take out.
2, one-level dc electrolysis corrosion:
To be placed on temperature through the aluminium foil after the pre-treatment be 79 ℃ with above-mentioned, and concentration is to carry out the corrosion of one-level dc electrolysis in the sulfuric acid of 6wt% and the 3wt% hydrochloric acid mixed solution, and current density is 26A/dm
2, electric weight is 2100C/dm
2
3, secondary chemical corrosion:
Above-mentioned aluminium foil through the corrosion of one-level dc electrolysis is placed in the mixed solution that concentration is 3wt% hydrochloric acid, 0.12wt% phosphoric acid and 0.2wt% polyethylene glycol (molecular weight is 20000) carries out the secondary chemical corrosion, the parameters of mixed solution is:
Temperature: 80 ℃
Time: 21 minutes
4, reprocessing:
Is that 65 ℃, concentration are to soak in the aqueous solution of nitric acid of 2wt% to change in 6 minutes with above-mentioned aluminium foil through the secondary chemical corrosion in temperature;
Wherein the condition of changing into is:
90 ℃ of 0.05A/dm of 10% boric acid
2Vfe=200V 610V
Every performance that 150 μ m Mitsubishi paper tinsels of process embodiment 2 and chemical synthesizing method production reach is respectively:
C
200Vf=2.60～2.65 μ F/cm
2C
610Vf=0.55～0.57 μ F/cm
2Tensile strength=21.0N/cm.
Specific embodiment described herein only is that the present invention's spirit is illustrated.The technical staff of the technical field of the invention can do various modifications or replenishes or adopt similar mode to substitute described specific embodiment, but can't depart from spirit of the present invention or surmount the defined scope of appended claims.
Claims (3)
1. the caustic solution of an aluminum electrolysis capacitor anode foil, this method may further comprise the steps:
A, pre-treatment: aluminium foil is placed in the mixed solution of 0.6～6wt% sulfuric acid and 3～10wt% hydrochloric acid and soaked 2～3 minutes;
B, the corrosion of one-level dc electrolysis: the mixed solution that above-mentioned aluminium foil through pre-treatment is put into 0.6～6wt% sulfuric acid and 3～10wt% hydrochloric acid carries out the corrosion of one-level dc electrolysis, and current density is 25～35A/dm
2, electric weight is 1900～2600C/dm
2, the temperature of described mixed solution is 70 ℃～85 ℃;
C, secondary chemical corrosion: the mixed solution that above-mentioned aluminium foil through the corrosion of one-level dc electrolysis is put into hydrochloric acid, 0.01～0.5wt% phosphoric acid and the 0.1～0.2wt% polyethylene glycol of 3～10wt% carries out the secondary chemical corrosion, the temperature of described mixed solution is 60 ℃～90 ℃, and the molecular weight of described polyethylene glycol is 20000～30000;
D, reprocessing: above-mentioned aluminium foil through the secondary chemical corrosion was soaked in the aqueous solution of nitric acid of 0.2～3wt% 4～6 minutes.
2. the caustic solution of aluminum electrolysis capacitor anode foil according to claim 1 is characterized in that: in pre-treatment, aluminium foil in mixed solution soaking temperature at 60～75 ℃.
3. the caustic solution of aluminum electrolysis capacitor anode foil according to claim 1 is characterized in that: in reprocessing, aluminium foil in aqueous solution of nitric acid soaking temperature at 50 ℃～80 ℃.
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| CN2009100953001A CN101483103B (en) | 2009-01-08 | 2009-01-08 | Corrosion method for aluminum electrolysis capacitor anode foil |
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| CN2009100953001A CN101483103B (en) | 2009-01-08 | 2009-01-08 | Corrosion method for aluminum electrolysis capacitor anode foil |
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| CN101483103A CN101483103A (en) | 2009-07-15 |
| CN101483103B true CN101483103B (en) | 2011-03-02 |
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Families Citing this family (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101645354B (en) * | 2009-08-27 | 2011-01-26 | 南通华冠电子科技有限公司 | Preparation method of high pressure anode foil for aluminum electrolytic capacitor |
| CN101964256A (en) * | 2010-11-04 | 2011-02-02 | 南通华冠电子科技有限公司 | Method for manufacturing medium and high-voltage anodic aluminum foil |
| CN102426930A (en) * | 2011-08-17 | 2012-04-25 | 佛山科学技术学院 | Corrosion method of high-voltage low-specific-volume anode foil |
| CN102723205A (en) * | 2012-06-30 | 2012-10-10 | 佛山科学技术学院 | Corrosion method of middle-high-voltage anode foil of aluminum electrolytic capacitor |
| CN105374561A (en) * | 2015-11-30 | 2016-03-02 | 新疆西部宏远电子有限公司 | Composite chemical etching technology of anode foil for high voltage aluminum electrolytic capacitor |
| CN108004547A (en) * | 2017-11-20 | 2018-05-08 | 湖北富奕达电子科技有限公司 | A kind of aluminium electrolytic capacitor cathode aluminium foil corrosion new process |
| CN108010723A (en) * | 2017-12-08 | 2018-05-08 | 南通海星电子股份有限公司 | A kind of method that the middle-high voltage electrode foil containing complex oxide film is prepared using magnetron sputtering |
| CN109097817B (en) * | 2018-09-25 | 2023-12-19 | 乳源县立东电子科技有限公司 | Method and device for improving wave edge of low-voltage anode foil |
| CN109537040A (en) * | 2018-12-31 | 2019-03-29 | 陈建君 | The process of mesohigh Fabrication of High Specific Capacitance aluminium foil corrosion |
| CN110289171B (en) * | 2019-05-14 | 2021-10-01 | 乳源瑶族自治县东阳光化成箔有限公司 | Method for manufacturing non-phosphorus hole-expanding aluminum electrolytic capacitor electrode foil |
| CN111979504A (en) * | 2020-08-20 | 2020-11-24 | 博罗冠业电子有限公司 | Aluminum foil manufacturing method and electrolytic capacitor negative electrode foil |
| CN113862765A (en) * | 2021-08-20 | 2021-12-31 | 扬州宏远电子股份有限公司 | Anode foil acid treatment direct-current corrosion process for high-voltage aluminum electrolytic capacitor |
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| US5143591A (en) * | 1991-06-11 | 1992-09-01 | U.S. Philips Corporation | Method of producing ultra stable aluminum oxide for high volt electrolytic capacitors and product thereof |
| JP2005264288A (en) * | 2004-03-22 | 2005-09-29 | Matsushita Electric Ind Co Ltd | Method for manufacturing etched foil for aluminum electrolytic capacitor, the etched foil, and chemical foil thereof |
| CN101205618A (en) * | 2007-12-14 | 2008-06-25 | 横店集团东磁有限公司 | Corrosion method of anode aluminum foil for middle-high voltage electrolytic capacitor |
| CN101250744A (en) * | 2008-02-27 | 2008-08-27 | 横店集团东磁有限公司 | Method for erosion of supervoltage high specific volume anode foil |
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2009
- 2009-01-08 CN CN2009100953001A patent/CN101483103B/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5143591A (en) * | 1991-06-11 | 1992-09-01 | U.S. Philips Corporation | Method of producing ultra stable aluminum oxide for high volt electrolytic capacitors and product thereof |
| JP2005264288A (en) * | 2004-03-22 | 2005-09-29 | Matsushita Electric Ind Co Ltd | Method for manufacturing etched foil for aluminum electrolytic capacitor, the etched foil, and chemical foil thereof |
| CN101205618A (en) * | 2007-12-14 | 2008-06-25 | 横店集团东磁有限公司 | Corrosion method of anode aluminum foil for middle-high voltage electrolytic capacitor |
| CN101250744A (en) * | 2008-02-27 | 2008-08-27 | 横店集团东磁有限公司 | Method for erosion of supervoltage high specific volume anode foil |
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