CN100532648C - Corrosion method of anode aluminum foil for middle-high voltage electrolytic capacitor - Google Patents
Corrosion method of anode aluminum foil for middle-high voltage electrolytic capacitor Download PDFInfo
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- CN100532648C CN100532648C CNB2007101943169A CN200710194316A CN100532648C CN 100532648 C CN100532648 C CN 100532648C CN B2007101943169 A CNB2007101943169 A CN B2007101943169A CN 200710194316 A CN200710194316 A CN 200710194316A CN 100532648 C CN100532648 C CN 100532648C
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Abstract
The invention relates to an anode aluminium foil corrosion method for middle and high voltage aluminum electrolytic capacitor, which comprising of: a preliminary treatment; primary direct current corrosion; chemical treatment; post treatment; and other steps. The invention solves the contradiction between the effective surface area of the anode aluminium foil and the mechanical strength, then provides the manufacturing method of electrolytic capacitor electrolytic capacitor corrosion foil which improves the area expanding rate, greatly improves the specific capacitance; meanwhile guarantees that the anode of the electrolytic capacitor with certain mechanical strength.
Description
Technical field
The present invention relates to a kind of medium-high voltage aluminum electrolytic capacitor anodic aluminum corrosion technology.
Background technology
The electrolytic condenser anode foils by enlarging its effective surface area, increases the electrostatic capacity of unit surface, generally handles aluminium foil with electrochemistry or chemical corrosion.Therefore, the relevant research that improves the area expanding rate aspect also had a lot of reports, etching process in the past, when hole density increases, also be accompanied by the dissolving of aluminium foil surface, not only reduced the effective surface area of etched foil, also reduce its physical strength, limited its Application Areas.
Summary of the invention
The invention solves the above-mentioned technical problem of existing in prior technology, a kind of medium-high voltage aluminum electrolytic capacitor anode aluminum foil erosion method is provided.
The objective of the invention is to overcome and solve effective surface area and physical strength contradiction between the two, proposed a kind of raising area expanding rate then, promote specific volume significantly, guarantee the manufacture method of the electrolytic capacitor anode etched foil of certain physical strength simultaneously.
Above-mentioned technical purpose of the present invention solves by the following technical programs: the medium-high voltage aluminum electrolytic capacitor anode aluminum foil erosion method may further comprise the steps:
Pre-treatment: aluminium foil is placed on containing in 1wt%-8wt% hydrochloric acid and the 10wt%-40wt% vitriolic mixing solutions of 65 ℃-85 ℃ of temperature soaked 0.5-3 minute; Above-mentioned concentration is mixed total concn.
The one-level dc corrosion: the aluminium foil of pre-treatment is placed on 70 ℃-90 ℃ of temperature, and 1wt%-8% hydrochloric acid carries out the dc electrolysis corrosion in the 10wt%-40wt% vitriolic mixed solution;
Chemical treatment: the aluminium foil that dc electrolysis was corroded is placed on 80 ℃-88 ℃ of temperature, 1.5wt%-5wt% hydrochloric acid and contain in the mixed solution of 0-25ppm cupric ion and carry out chemical treatment, and the time is 15-30 minute;
Aftertreatment: it is 10 ℃-40 ℃ that the aluminium foil of chemical treatment is placed on temperature, soaks 1-6 minute in the salpeter solution of 3wt%-30wt%.
Details are as follows for various processes:
1. pre-treatment
The main effect of pre-treatment is exactly to remove aluminium foil surface greasy dirt, impurity and natural oxide film, and aluminium foil surface is evenly activated, and forms the initial pit that is evenly distributed when helping pre-treatment.Concrete grammar is aluminium foil to be placed on containing in 1wt%-8wt% hydrochloric acid and the 10wt%-40wt% vitriolic mixing solutions of 65 ℃-85 ℃ of temperature soaked 0.5-3 minute.
As preferably, described pre-treatment is to contain 2wt%-6wt% hydrochloric acid with what aluminium foil was placed on 65 ℃-85 ℃ of temperature, and soak time is 0.5-2 minute in the 12wt%-35wt% sulfuric acid mixed solution.
As preferably, described pre-treatment be with aluminium foil at 2wt%-6wt% hydrochloric acid, soak in the 12wt%-35wt% sulfuric acid mixed solution, its treatment temp is 70 ℃-83 ℃.
Concentration of hydrochloric acid is lower than 2wt%, and treatment effect is not good, if concentration surpasses 6wt%, aluminium foil surface dissolving aggravation does not reach the corrosive effect of expection, so concentration of hydrochloric acid is best at 2wt%-6wt%.
Sulfuric acid concentration is lower than 12wt%, and treatment effect is not good, if concentration surpasses 35wt%, aluminium foil surface dissolving aggravation does not reach the corrosive effect of expection, so sulfuric acid concentration is best at 12wt%-35wt%.
Treatment time is lower than 0.5 minute, and treatment effect is not good, if the time is higher than 2 minutes, aluminium foil dissolves comprehensively, so the pre-treatment time is controlled at 0.5-2 minute for best.
Treatment temp is lower than 70 ℃, and treatment effect is not obvious, if temperature surpasses 83 ℃, aluminium foil dissolves comprehensively, so the pre-treatment temperature is controlled at 70 ℃-83 ℃ for best.
2. one-level dc corrosion
The one-level dc corrosion is the key point of whole etching process, and main purpose is the initial pit that forms certain depth and aperture at aluminium foil surface, still has the tunnel hole of imitating area after mesohigh forms so that subsequent corrosion can make to grow up into.
The one-level dc corrosion is that the aluminium foil with pre-treatment is placed on 70 ℃-88 ℃ of temperature, and 1wt%-8% hydrochloric acid carries out the dc electrolysis corrosion in the 10wt%-40wt% vitriolic mixed solution;
As preferably, described one-level dc corrosion be the aluminium foil with pre-treatment to be placed on temperature be 72 ℃-85 ℃, 2wt%-6wt% hydrochloric acid carries out the dc electrolysis corrosion in the 12wt%-35wt% vitriolic mixed solution, its current density is 0.3-0.7A/cm
2, electric weight is 25-80C/cm
2
Concentration of hydrochloric acid is lower than 2wt%, and corrosive effect is not good, if concentration surpasses 6wt%, aluminium foil surface dissolving aggravation does not reach the corrosive effect of expection, so concentration of hydrochloric acid is best at 2wt%-6wt%.
Sulfuric acid concentration is lower than 12wt%, and corrosive effect is not good, if concentration surpasses 35wt%, aluminium foil surface dissolving aggravation does not reach the corrosive effect of expection, so sulfuric acid concentration is best at 12wt%-35wt%.
One-level dc electrolysis corrosive fluid temperature is lower than 72 ℃, and corrosion speed is slow partially, and corrosive effect is not quite obvious, if temperature surpasses 85 ℃, the corrosion speed aggravation is difficult to control, so one-level dc electrolysis corrosive fluid temperature is controlled at 72 ℃-85 ℃ for best.
Current density is lower than 0.3A/cm
2, first pit density is not enough, if current density surpasses 0.7A/cm
2, first pit density is too close, and causes the local dissolution of aluminium foil surface, so current density is controlled at 0.3-0.7A/cm
2Be the best.
The corrosion electric weight is lower than 25C/cm
2, corrosive effect is not obvious, if the corrosion electric weight surpasses 80C/cm
2, then can cause the local dissolution of aluminium foil surface, so corrode electric energy control at 25-80C/cm
2Be the best.
1. chemical treatment
Chemically treated purpose is to allow initial pit further enlarge and intensification on original basis, makes the final aperture and the degree of depth satisfy mesohigh and changes into requirement.
Chemical treatment method is that the aluminium foil that dc electrolysis corroded is placed on 80 ℃-88 ℃ of temperature, carries out chemical treatment in the mixed solution of 1.5wt%-5wt% hydrochloric acid soln and 0-25ppm cupric ion, and the time is 15-30 minute;
As preferably, described chemical treatment is that the aluminium foil after the corrosion of one-level dc electrolysis is immersed in temperature is 82 ℃-86 ℃, and in the mixed solution of 1.5wt%-5wt% hydrochloric acid and 3-20ppm cupric ion, the time is 15-25 minute.
Concentration of hydrochloric acid is lower than 1.5wt%, and corrosive effect is not good, if concentration surpasses 5wt%, aluminium foil surface dissolving aggravation does not reach the corrosive effect of expection, so concentration of hydrochloric acid is best at 1.5wt%-5wt%.
Cupric ion is lower than 3ppm, and speed of response is too slow, can't allow initial pit further enlarge and intensification, if cupric ion surpasses 20ppm, speed of response is fast, is difficult to control, causes specific volume to descend, and is best so cupric ion is controlled at 3-20ppm.
Treatment temp is lower than 82 ℃, and speed of response is slow, if temperature surpasses 86 ℃, speed of response is fast, so treatment temp is best at 82 ℃-86 ℃.
Treatment time is lower than 15 minutes, and treatment effect is not good, if the time surpasses 25 minutes, aluminium foil dissolves comprehensively, so the treatment time was best at 15-25 minute.
4, aftertreatment
Aftertreatment mainly is to remove residual harmful chemical substance and exposed metallic impurity in remaining oxide film, surface and the hole, guarantees to form densification and the oxide film of excellent electrical properties when changing into.
Described aftertreatment be the aluminium foil with chemical treatment to be placed on temperature be 10 ℃-40 ℃, soaked 1-6 minute in the salpeter solution of 3wt%-30wt%.
As preferably, described aftertreatment is that the aluminium foil after the chemical treatment is placed on temperature is 10 ℃-40 ℃, soaks 2-5 minute in the salpeter solution of 5wt%-25wt%.
Concentration of nitric acid is lower than 3wt%, and treatment effect is not obvious, if concentration surpasses 25wt%, then can make the aluminium foil dissolving, so concentration of nitric acid is controlled at 3wt%-25wt% for best.
The nitric acid temperature is lower than 10 ℃, and treatment effect is not obvious, if concentration surpasses 40 ℃, then can make the aluminium foil dissolving, so the nitric acid temperature is controlled at 10 ℃-40 ℃ for best.
The nitric acid time is lower than 2 minutes, and treatment effect is not obvious, if the time surpasses 5 minutes, then can make the aluminium foil dissolving, so the nitric acid time is controlled at 2-5 minute for best.
Embodiment
Embodiment 1:
1. pre-treatment
With aluminium foil be placed on 76 ℃ of temperature, concentration is 2.5wt% hydrochloric acid, soaks in the 30wt% sulfuric acid mixed solution 2 minutes, take out.
2. one-level dc corrosion
It is 76 ℃, 2.5wt% hydrochloric acid that the aluminium foil of pre-treatment is placed on temperature, carries out the dc electrolysis corrosion in the 30wt% vitriolic mixed solution, and its current density is 0.45A/cm
2, electric weight is 40C/cm
2
3. chemical treatment
In temperature is 84 ℃, soaks in the mixed solution of 3wt% hydrochloric acid and 12ppm cupric ion after 20 minutes, takes out.
4. aftertreatment
35 ℃ of temperature, soak in the salpeter solution of 7wt% after 4 minutes, take out.
Embodiment 2:
1. pre-treatment
With aluminium foil be placed on 77 ℃ of temperature, concentration is 2.5wt% hydrochloric acid, soaks in the 30wt% sulfuric acid mixed solution 1.5 minutes, take out.
2. one-level dc corrosion
It is 77 ℃, 2.5wt% hydrochloric acid that the aluminium foil of pre-treatment is placed on temperature, carries out the dc electrolysis corrosion in the 30wt% vitriolic mixed solution, and its current density is 0.4A/cm
2, electric weight is 35C/cm
2
3. chemical treatment
In temperature is 86 ℃, soaks in the mixed solution of 2.5wt% hydrochloric acid and 15ppm cupric ion after 20 minutes, takes out.
4. aftertreatment
35 ℃ of temperature, soak in the salpeter solution of 7wt% after 4 minutes, take out.
Embodiment 3:
1. pre-treatment
With aluminium foil be placed on 75 ℃ of temperature, concentration is 3wt% hydrochloric acid, soaks in the 28wt% sulfuric acid mixed solution 1 minute, take out.
2. one-level dc corrosion
It is 75 ℃, 3wt% hydrochloric acid that aluminium foil after the pre-treatment is placed on temperature, carries out the dc electrolysis corrosion in the 28wt% sulfuric acid mixture liquid, and its current density is 0.5A/cm
2, electric weight is 35C/cm
2
3. chemical treatment
In temperature is 82 ℃, soaks in the mixed solution of 4wt% hydrochloric acid soln and 8ppm cupric ion after 22 minutes, takes out.
4. aftertreatment
30 ℃ of temperature, soak in the salpeter solution of 10wt% after 5 minutes, take out.
Embodiment 4:
1. pre-treatment
With aluminium foil be placed on 75 ℃ of temperature, concentration is 3wt% hydrochloric acid, soaks in the 28wt% sulfuric acid mixed solution 2 minutes, take out.
2. one-level dc corrosion
It is 75 ℃, 3wt% hydrochloric acid that aluminium foil after the pre-treatment is placed on temperature, carries out the dc electrolysis corrosion in the 28wt% sulfuric acid mixture liquid, and its current density is 0.43A/cm
2, electric weight is 35C/cm
2
3. chemical treatment
In temperature is 84 ℃, soaks in the mixed solution of 4wt% hydrochloric acid soln and 5ppm cupric ion after 24 minutes, takes out.
4. aftertreatment
30 ℃ of temperature, soak in the salpeter solution of 10wt% after 5 minutes, take out.
Change into condition:
85 ℃ of 0.05A/cm of 10% boric acid
2Vfe=375v520v
The result is as follows:
C375vf＝1.05-1.15μF/cm
2 C520vf＝0.62-0.70μF/cm
2 F＝20N/cm
The mesohigh sun level paper tinsel of manufacturing of the present invention has high specific volume, physical strength preferably.
Claims (3)
1, medium-high voltage aluminum electrolytic capacitor anode aluminum foil erosion method may further comprise the steps:
Pre-treatment: aluminium foil is placed on containing in 2wt%-6wt% hydrochloric acid and the 12wt%-35wt% vitriolic mixing solutions of 70 ℃-83 ℃ of temperature soaked 0.5-2 minute;
The one-level dc corrosion: the aluminium foil of pre-treatment is placed on 72 ℃-85 ℃ of temperature, and 2wt%-6wt% hydrochloric acid carries out the dc electrolysis corrosion in the 12wt%-35wt% vitriolic mixed solution, and its current density is 0.3-0.7A/cm
2, electric weight is 25-80C/cm
2
Chemical treatment: the aluminium foil that dc electrolysis was corroded is placed on 82 ℃-86 ℃ of temperature, carries out chemical treatment in the mixed solution of 1.5wt%-5wt% hydrochloric acid soln and 3-20ppm cupric ion, and the time is 15-25 minute;
Aftertreatment: it is 10 ℃-40 ℃ that the aluminium foil of chemical treatment is placed on temperature, soaks 2-5 minute in the salpeter solution of 3wt%-25wt%.
2, medium-high voltage aluminum electrolytic capacitor anode aluminum foil erosion method according to claim 1, it is characterized in that: described one-level dc corrosion is that to be placed on temperature be 74 ℃-83 ℃ to the aluminium foil with pre-treatment, 2wt%-6wt% hydrochloric acid, carry out the dc electrolysis corrosion in the 12wt%-35wt% vitriolic mixed solution, its current density is 0.3-0.7A/cm
2, electric weight is 25-80C/cm
2
3, medium-high voltage aluminum electrolytic capacitor anode aluminum foil erosion method according to claim 1, it is characterized in that: described aftertreatment is that the aluminium foil after the chemical treatment is placed on temperature is 10 ℃-40 ℃, soaks 2-5 minute in the salpeter solution of 5wt%-25wt%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2007101943169A CN100532648C (en) | 2007-12-14 | 2007-12-14 | Corrosion method of anode aluminum foil for middle-high voltage electrolytic capacitor |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2007101943169A CN100532648C (en) | 2007-12-14 | 2007-12-14 | Corrosion method of anode aluminum foil for middle-high voltage electrolytic capacitor |
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| CN100532648C true CN100532648C (en) | 2009-08-26 |
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Families Citing this family (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101483103B (en) * | 2009-01-08 | 2011-03-02 | 横店集团东磁有限公司 | Corrosion method for aluminum electrolysis capacitor anode foil |
| CN101483102B (en) * | 2009-01-08 | 2011-03-02 | 横店集团东磁有限公司 | Anode aluminum corrosion method for media and high voltage aluminum electrolysis capacitor |
| CN101777432A (en) * | 2010-03-23 | 2010-07-14 | 扬州宏远电子有限公司 | Forming process of anode foils for extra-high voltage aluminium electrolytic capacitors |
| CN102013333A (en) * | 2010-09-21 | 2011-04-13 | 吕荣荣 | Method for etching anode foil of high-voltage aluminum electrolytic capacitor used for energy-saving lamp |
| CN105957717B (en) * | 2016-05-26 | 2018-11-30 | 乳源县立东电子科技有限公司 | The multiple hair engaging aperture method of the multistage of mesohigh anode foils |
| CN107502948A (en) * | 2017-07-15 | 2017-12-22 | 江苏国瑞科技有限公司 | A kind of new etched foil counter-boring techniques |
| CN107658471A (en) * | 2017-10-09 | 2018-02-02 | 山西沃特海默新材料科技股份有限公司 | A kind of chemical heat erosion preparation method of micropore battery aluminium foil |
| CN107699894B (en) * | 2017-10-09 | 2020-09-29 | 山西沃特海默新材料科技股份有限公司 | Chemical corrosion preparation method of microporous battery aluminum foil |
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