CN101483102B - Anode aluminum corrosion method for media and high voltage aluminum electrolysis capacitor - Google Patents
Anode aluminum corrosion method for media and high voltage aluminum electrolysis capacitor Download PDFInfo
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- CN101483102B CN101483102B CN2009100952992A CN200910095299A CN101483102B CN 101483102 B CN101483102 B CN 101483102B CN 2009100952992 A CN2009100952992 A CN 2009100952992A CN 200910095299 A CN200910095299 A CN 200910095299A CN 101483102 B CN101483102 B CN 101483102B
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Abstract
The present invention relates to an anode aluminum foil corrosion process for middle-and high-voltage aluminum-electrolytic capacitor. The present invention solves the existence technical problems in the prior art such as the mechanical strength is reduced in the anode aluminum foil corrosion process for the high-voltage aluminum-electrolytic capacitor, the invention provides an anode aluminum foil corrosion process which can simultaneously hold the mechanical strength while achieving the prior corrosion affection. The invention has main step of: a pretreatment of soaking the aluminum foil in a mixed solution of 1.5wt%-5wt% of hydrochloric acid and 20wt%-38wt% of sulfuric acid; a first stage direct current corrosion of performing direct current electrolytic corrosion to the aluminum foil after pretreatment in the mixed solution of 1.5wt%-5wt% of hydrochloric acid and 20wt%-38wt% of sulfuric acid; a second stage direct current corrosion of performing direct current electrolytic corrosion to the aluminum foil after first stage direct current corrosion in a 0.5wt%-4wt% hydrochloric acid solution; and a post-processing of putting the aluminum foil after the second stage direct current corrosion in a 2wt%-15wt% of nitric acid solution for immersion.
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 capacitor anode foils by enlarging its effective surface area, increases the static capacity of unit are, generally handles aluminium foil with electrochemistry or chemical corrosion.Etching process in the past when hole density increases, also is accompanied by the dissolving of aluminium foil surface, has not only reduced the effective surface area of etched foil, has also reduced its mechanical strength, has limited its application.
Summary of the invention
The invention solves technical problems such as having reduced its mechanical strength in the existing in prior technology anode aluminum foil for high-voltage aluminum electrolytic capacitor corrosion process, a kind of medium-high voltage aluminum electrolytic capacitor anode aluminum foil erosion method is provided, when making it reach original corrosive effect, kept mechanical strength.
The objective of the invention is to overcome and solve effective surface area and mechanical 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 mechanical 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 in the mixed solution of 1.5wt%-5wt% hydrochloric acid and 20wt%-38wt% sulfuric acid and soaked 0.5-3 minute, solution temperature is 60 ℃-75 ℃;
The one-level dc corrosion: the aluminium foil of pre-treatment is placed in the mixed solution of 1.5wt%-5wt% hydrochloric acid and 20wt%-38wt% sulfuric acid and carries out the dc electrolysis corrosion, solution temperature is 70 ℃-85 ℃;
The secondary dc corrosion: the aluminium foil that the one-level dc corrosion is crossed is placed in the solution of 0.5wt%-4wt% hydrochloric acid and carries out the dc electrolysis corrosion, and solution temperature is 70 ℃-87 ℃;
Reprocessing: the aluminium foil that the secondary dc corrosion is crossed is placed in the salpeter solution of 2wt%-15wt% and soaked 2-5 minute, and solution temperature is 20 ℃-45 ℃;
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 preliminary treatment.Concrete grammar is aluminium foil to be placed in the mixed solution of 1.5wt%-5wt% hydrochloric acid and 20wt%-38wt% sulfuric acid soaked 0.5-3 minute, and temperature is 60 ℃-75 ℃;
As preferably, described pre-treatment is aluminium foil to be placed on soak time is 1-2 minute in 1.8wt%-4wt% hydrochloric acid and the 25wt%-35wt% sulfuric acid mixed solution, 60 ℃-75 ℃ of temperature;
As preferably, described pre-treatment is aluminium foil to be placed in 1.8wt%-4wt% hydrochloric acid and the 25wt%-35wt% sulfuric acid mixed solution soak, and its treatment temperature is 65 ℃-70 ℃.
Concentration of hydrochloric acid is lower than 1.8wt%, and treatment effect is not good, if concentration surpasses 4wt%, aluminium foil surface dissolving aggravation does not reach the corrosive effect of expection, so concentration of hydrochloric acid is best at 1.8wt%-4wt%.
Sulfuric acid concentration is lower than 25wt%, 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 25wt%-35wt%.
Processing time is lower than 1 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 1-2 minute for best.
Treatment temperature is lower than 65 ℃, and treatment effect is not obvious, if temperature surpasses 70 ℃, aluminium foil dissolves comprehensively, so the pre-treatment temperature is controlled at 65 ℃-70 ℃ 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.
One-level dc corrosion: the aluminium foil of pre-treatment is placed in the mixed solution of 1.5wt%-5% hydrochloric acid and 20wt%-38wt% sulfuric acid and carries out the dc electrolysis corrosion, 70 ℃-85 ℃ of its temperature;
As preferably, described one-level dc corrosion is that the aluminium foil with pre-treatment is placed in the mixed liquor of 1.8wt%-4wt% hydrochloric acid and 25wt%-35wt% sulfuric acid and carries out the dc electrolysis corrosion, and its current density is 0.4-0.75A/cm
2, electric weight is 30-60C/cm
2, temperature is 72 ℃-83 ℃;
Concentration of hydrochloric acid is lower than 1.8wt%, and corrosive effect is not good, if concentration surpasses 4wt%, aluminium foil surface dissolving aggravation does not reach the corrosive effect of expection, so concentration of hydrochloric acid is best at 1.8wt%-4wt%.
Sulfuric acid concentration is lower than 25wt%, 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 25wt%-35wt%.
One-level dc electrolysis corrosive liquid temperature is lower than 72 ℃, and corrosion rate is slow partially, and corrosive effect is not quite obvious, if temperature surpasses 83 ℃, the corrosion rate aggravation is difficult to control, so one-level dc electrolysis corrosive liquid temperature is controlled at 72 ℃-83 ℃ for best.
Current density is lower than 0.4A/cm
2, first pit density is not enough, if current density surpasses 0.75/cm
2, comprehensive dissolving of aluminium foil surface is so current density is controlled at 0.4-0.75A/cm
2Be the best.
The corrosion electric weight is lower than 30C/cm
2, corrosive effect is not obvious, if the corrosion electric weight surpasses 60C/cm
2, then can cause the local dissolution of aluminium foil surface, so corrode electric energy control at 30-60C/cm
2Be the best.
3. secondary dc corrosion
The purpose of secondary dc corrosion 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.
The secondary dc corrosion: the aluminium foil that the one-level dc corrosion is crossed is placed in the solution of 0.5wt%-4wt% hydrochloric acid and carries out the dc electrolysis corrosion, and solution temperature is 70 ℃-87 ℃;
As preferably, described secondary dc corrosion is the aluminium foil after the corrosion of one-level dc electrolysis to be placed in the solution of 0.5wt%-3.5wt% hydrochloric acid carry out the dc electrolysis corrosion, and its current density is 0.05-0.2A/cm
2, electric weight is 20-90C/cm
2, 75 ℃-85 ℃ of temperature,
Concentration of hydrochloric acid is lower than 0.5wt%, and corrosive effect is not good, if concentration surpasses 3.5wt%, aluminium foil surface dissolving aggravation does not reach the corrosive effect of expection, so concentration of hydrochloric acid is best at 1wt%-3.5wt%.
Treatment temperature is lower than 75 ℃, and reaction speed is slow, if temperature surpasses 85 ℃, reaction speed is fast, is difficult to control, so treatment temperature is best at 75 ℃-85 ℃.
Current density is lower than 0.05A/cm
2, the reaming DeGrain is if current density surpasses 0.75A/cm
2, then can cause the local dissolution of aluminium foil surface, so current density is controlled at 0.4-0.75A/cm
2Be the best.
The corrosion electric weight is lower than 20C/cm
2, corrosive effect is not obvious, if the corrosion electric weight surpasses 90C/cm
2, then can cause the local dissolution of aluminium foil surface, so corrode electric energy control at 20-90C/cm
2Be the best.
4, reprocessing
Reprocessing mainly is to remove residual harmful chemical substance and exposed metal impurities in remaining oxide-film, surface and the hole, guarantees to form densification and the oxide-film of excellent electrical properties when changing into.
Described reprocessing is the aluminium foil that the secondary dc corrosion is crossed to be placed in the salpeter solution of 2wt%-15wt% soaked 2-5 minute, and solution temperature is 20 ℃-45 ℃;
As preferably, described reprocessing is the aluminium foil after the chemical treatment to be placed in the salpeter solution of 4wt%-10wt% soaked 2-4 minute, and temperature is 25 ℃-35 ℃;
Concentration of nitric acid is lower than 2wt%, and treatment effect is not obvious, if concentration surpasses 15wt%, then can make the aluminium foil dissolving, so concentration of nitric acid is controlled at 2wt%-15wt% for best.
The nitric acid temperature is lower than 25 ℃, and treatment effect is not obvious, if concentration surpasses 35 ℃, then can make the aluminium foil dissolving, so the nitric acid temperature is controlled at 25 ℃-35 ℃ for best.
The nitric acid time is lower than 2 minutes, and treatment effect is not obvious, if the time surpasses 4 minutes, then can make the aluminium foil dissolving, so the nitric acid time is controlled at 2-4 minute for best.
Material of the present invention compared with prior art has the following advantages:
The medium-high voltage aluminum electrolytic capacitor that the inventive method is made has high area expanding rate with anode aluminium foil, and specific volume promotes significantly, guarantees certain mechanical strength simultaneously.
Embodiment
Embodiment 1:
1. pre-treatment
Aluminium foil is placed on immersion taking-up after 1 minute in 2.4wt% hydrochloric acid and the 31wt% sulfuric acid mixed solution, and temperature is 63 ℃.
2. one-level dc corrosion
The aluminium foil of pre-treatment is placed in the mixed liquor of 2.4wt% hydrochloric acid and 31wt% sulfuric acid and carries out the dc electrolysis corrosion, its current density is 0.60A/cm
2, electric weight is 33C/cm
2, temperature is 76 ℃.
3. secondary dc corrosion
The aluminium foil that the one-level dc corrosion is crossed is placed in the solution of 3.8wt% hydrochloric acid and carries out the dc electrolysis corrosion, and its current density is 0.08A/cm
2, electric weight is 55C/cm
2, temperature is 80 ℃.
4. reprocessing
The aluminium foil that the secondary dc corrosion is crossed is placed on to soak after 4 minutes in the salpeter solution of 5.7wt% and takes out, and temperature is 35 ℃.
Change into condition:
85 ℃ of 0.05A/cm of 10% boric acid
2Vfe=375v 520v
Sun level paper tinsel The performance test results result after changing into is as follows:
C
375vf=1.10-1.15 μ F/cm
2C
520vf=0.67-0.74 μ F/cm
2Tensile strength F=20N/cm
The mesohigh sun level paper tinsel of manufacturing of the present invention has high specific volume, mechanical strength preferably.
Embodiment 2:
1. pre-treatment
Aluminium foil is placed on immersion taking-up after 2 minutes in 2.6wt% hydrochloric acid and the 30wt% sulfuric acid mixed solution, and temperature is 68 ℃.
2. one-level dc corrosion
The aluminium foil of pre-treatment is placed in the mixed liquor of 2.6wt% hydrochloric acid and 30wt% sulfuric acid and carries out the dc electrolysis corrosion, its current density is 0.65A/cm
2, electric weight is 36C/cm
2, temperature is 73 ℃.
3. secondary dc corrosion
The aluminium foil that the one-level dc corrosion is crossed is placed in the solution of 3.3wt% hydrochloric acid and carries out the dc electrolysis corrosion, and its current density is 0.10A/cm
2, electric weight is 67C/cm
2, temperature is 75 ℃.
4. reprocessing
The aluminium foil that the secondary dc corrosion is crossed is placed on to soak after 3.5 minutes in the salpeter solution of 8wt% and takes out, and temperature is 35 ℃.
Change into condition:
85 ℃ of 0.05A/cm of 10% boric acid
2Vfe=375v 520v
Sun level paper tinsel The performance test results result after changing into is as follows:
C
375vf=1.10-1.15 μ F/cm
2C
520vf=0.67-0.74 μ F/cm
2Tensile strength F=20N/cm
The mesohigh sun level paper tinsel of manufacturing of the present invention has high specific volume, mechanical strength preferably.
Embodiment 3:
1. pre-treatment
Aluminium foil is placed on 2.8wt% hydrochloric acid, soaks after 1 minute in the 29.8wt% sulfuric acid mixed solution and take out, temperature is 70 ℃.
2. one-level dc corrosion
The aluminium foil of pre-treatment is placed in the mixed liquor of 2.8wt% hydrochloric acid and 29.8wt% sulfuric acid and carries out the dc electrolysis corrosion, its current density is 0.55A/cm
2, electric weight is 35C/cm
2, temperature is 74 ℃.
3. secondary dc corrosion
The aluminium foil that the one-level dc corrosion is crossed is placed in the solution of 3wt% hydrochloric acid and carries out the dc electrolysis corrosion, and its current density is 0.08A/cm
2, electric weight is 60C/cm
2, temperature is 84 ℃.
4. reprocessing
The aluminium foil that the secondary dc corrosion is crossed is placed on to soak after 3 minutes in the salpeter solution of 6.8wt% and takes out, and temperature is 35 ℃.
Change into condition:
85 ℃ of 0.05A/cm of 10% boric acid
2Vfe=375v 520v
Sun level paper tinsel The performance test results result after changing into is as follows:
C
375vf=1.10-1.15 μ F/cm
2C
520vf=0.67-0.74 μ F/cm
2Tensile strength F=20N/cm
The mesohigh sun level paper tinsel of manufacturing of the present invention has high specific volume, mechanical strength preferably.
Specific embodiment described in the present invention only is that the present invention's spirit is illustrated.The technical staff of the technical field of the invention can make 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.
Although the present invention has been made detailed explanation and has quoted some instantiations as proof, to those skilled in the art, only otherwise leave that the spirit and scope of the present invention can be done various variations or correction is obvious.
Claims (1)
1. medium-high voltage aluminum electrolytic capacitor anode aluminum foil erosion method, its step comprises:
A) pre-treatment: aluminium foil is placed in the mixed solution soaked 1-2 minute, contain 1.8wt%-4wt% hydrochloric acid and 25wt%-35wt% sulfuric acid in the mixed solution, the mixed solution temperature is 65 ℃-70C;
B) one-level dc corrosion: the aluminium foil of pre-treatment is placed on carries out the dc electrolysis corrosion in the mixed solution, contain 1.8wt%-4wt% hydrochloric acid and 25wt%-35wt% sulfuric acid in the mixed solution, its current density is 0.4-0.75A/cm
2, electric weight is 30-60C/cm
2, the mixed solution temperature is 72 ℃-83 ℃;
C) secondary dc corrosion: the aluminium foil that the one-level dc corrosion is crossed is placed in the solution of 0.5wt%-3.5wt% hydrochloric acid and carries out the dc electrolysis corrosion, and its current density is 0.05-0.2A/cm
2, electric weight is 20-90C/cm
2, solution temperature is 75 ℃-85 ℃;
D) reprocessing: the aluminium foil that the secondary dc corrosion is crossed is placed in the salpeter solution of 4wt%-10wt% and soaked 2-4 minute, and solution temperature is 25 ℃-35 ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN2009100952992A CN101483102B (en) | 2009-01-08 | 2009-01-08 | Anode aluminum corrosion method for media and high voltage aluminum electrolysis capacitor |
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| CN2009100952992A CN101483102B (en) | 2009-01-08 | 2009-01-08 | Anode aluminum corrosion method for media and high voltage aluminum electrolysis capacitor |
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| CN101483102B true CN101483102B (en) | 2011-03-02 |
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Families Citing this family (11)
| 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 |
| 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 |
| CN102074379A (en) * | 2011-01-11 | 2011-05-25 | 江苏立富电极箔有限公司 | Production process of high-voltage anode foil for aluminum electrolytic capacitor |
| CN102094231A (en) * | 2011-01-11 | 2011-06-15 | 江苏立富电极箔有限公司 | Process for corroding anode foil for intermediate and high voltage aluminum electrolytic capacitor |
| 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 |
| CN103745830B (en) * | 2014-01-22 | 2016-06-29 | 广西贺州市桂东电子科技有限责任公司 | A kind of raising conforming two sections of current waveform caustic solutions of mesohigh anode aluminium foil tunnel hole length |
| CN105551805B (en) * | 2016-01-18 | 2018-01-12 | 南通海星电子股份有限公司 | The middle processing method of medium-high voltage aluminum electrolytic capacitor electrode foil |
| CN106098380B (en) * | 2016-05-26 | 2019-02-22 | 乳源县立东电子科技有限公司 | The hole shape control method of high-voltage anode foil secondary chambering |
| 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 |
| CN108396367B (en) * | 2018-05-31 | 2020-09-22 | 南通海星电子股份有限公司 | Method for manufacturing medium-high voltage corrosion foil for aluminum electrolytic capacitor |
| CN109727775B (en) * | 2018-12-28 | 2022-01-18 | 广西贺州市桂东电子科技有限责任公司 | Method for preparing medium-high voltage anode aluminum foil long and short hole structure by double-V pore corrosion |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1106475A (en) * | 1994-12-01 | 1995-08-09 | 西安交通大学 | Etching technique of anode Al foil of electrolysis capacitor |
| 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 |
-
2009
- 2009-01-08 CN CN2009100952992A patent/CN101483102B/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1106475A (en) * | 1994-12-01 | 1995-08-09 | 西安交通大学 | Etching technique of anode Al foil of electrolysis capacitor |
| 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 |
Non-Patent Citations (2)
| Title |
|---|
| JP平10-172869A 1998.06.26 |
| JP平6-53085A 1994.02.25 |
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