CN102983008A - Ultrahigh voltage anode foil corrosion method for aluminum electrolytic capacitor - Google Patents
Ultrahigh voltage anode foil corrosion method for aluminum electrolytic capacitor Download PDFInfo
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Abstract
Disclosed is an ultrahigh voltage anode foil corrosion method for an aluminum electrolytic capacitor. The method comprises steps of conducting pretreatment, conducting first direct current electrochemical corrosion, conducting first middle treatment, conducting second direct current electrochemical corrosion, conducting second middle treatment, conducting third direct current electrochemical corrosion, and conducting post treatment. By the aid of the method, produced anode foil can meet ultrahigh voltage requirements of 800 V to 1000 V, and produced products have the advantages of being low in drain current, quick in boost time and good in mechanical performance.
Description
Technical field
The present invention relates to a kind of aluminum electrolysis capacitor anode foil and make field, especially a kind of aluminium electrolytic capacitor extra-high voltage anode foil caustic solution.
Background technology
The ultra-high voltage aluminum electrolytic capacitor is because its voltage is high, energy storage is high, discharge and recharge in the field such as fast and generate heat low extensive use Aero-Space, vehicle frequency transformer and industrial frequency conversion and the industry.The report that extra-high voltage anode foil corrosion or chemical synthesizing method were also arranged in the present at home industry, but its voltage mostly is in 700V, superhigh pressure also rarely has report or patent application greater than the anode foil corrosion technology of 800V, electronic material ultra-high voltage aluminum electrolytic capacitor anode aluminum foil production technology also is in blank basically at home, and researching and developing and be applied to the production of ultra-high voltage aluminum electrolytic capacitor anode aluminum foil has larger facilitation to filling the domestic gaps with industry development.
Summary of the invention
Little in order to solve the anode foils hole that has corrosion technology production now, change into rear easy obstruction, specific volume is low, can only be used in the mesohigh anode foils and produce, and can not carry out the defective that superhigh pressure is produced with anode foils, the invention provides a kind of aluminium electrolytic capacitor extra-high voltage anode foil caustic solution.
The present invention is achieved through the following technical solutions above-mentioned purpose: a kind of aluminium electrolytic capacitor extra-high voltage anode foil caustic solution comprises the steps: light paper tinsel → pre-treatment → one-level the anodic etching method → middle processing 1 → secondary the anodic etching method → 2 → three grades of the anodic etching method → reprocessings of middle processing.
Extra-high voltage anode foil of the present invention is Vt 〉=800V.
A, pre-treatment: aluminium foil is placed on 50~70 ℃, and concentration is to soak in 2.0~6.0wt% hydrochloric acid solution 60~150 seconds,
B, one-level the anodic etching method: it is 65~85 ℃ that above-mentioned aluminium foil through pre-treatment is put into temperature, concentration is to carry out the anodic etching method in 3~10wt% hydrochloric acid, 20~35wt% sulfuric acid and the 0.1~0.5wt% phosphoric acid mixed liquor, and current density is 0.25~0.50A/cm
2, electric weight is 20~30C/cm
2,
C, middle processing 1: it is 65~85 ℃ that above-mentioned aluminium foil through the one-level the anodic etching method is put into temperature, and concentration is dc electrolysis corrosion in 2~6wt% hydrochloric acid and the 0.02~0.25wt% ethanedioic acid mixed liquor, and current density is 0.02~0.10A/cm
2, electric weight is 3~6C/cm
2,
D, secondary the anodic etching method: it is 65~80 ℃ that the aluminium foil of processing in the above-mentioned process is put into temperature, concentration is the anodic etching method in the mixed liquor of 3~15wt% nitric acid and 0.005~0.05wt% polyacrylamide, and current density is 0.06~0.15A/cm
2, electric weight is 18~45C/cm
2,
E, middle processing 2: it is 65~85 ℃ that above-mentioned aluminium foil through the secondary the anodic etching method is put into temperature, and concentration is dc electrolysis corrosion in 2~6wt% hydrochloric acid and the 0.02~0.25wt% ethanedioic acid mixed liquor, and current density is 0.02~0.10A/cm
2, electric weight is 3~6C/cm
2,
F, three grades of the anodic etching methods: it is 65~80 ℃ that the aluminium foil of processing in the above-mentioned process is put into temperature, concentration is secondary the anodic etching method in the mixed liquor of 3~15wt% nitric acid and 0.005~0.05wt% polyacrylamide, and current density is 0.04~0.12A/cm
2, electric weight is 12~36C/cm
2
G, reprocessing: to put into temperature through the aluminium foil behind three grades of the anodic etching methods be 60~80 ℃ with above-mentioned, and concentration is to soak in 5~12wt% salpeter solution 30~90 seconds.
The pre-treatment pure hydrochloric acid aqueous solution of the present invention effect is impurity, the greasy dirt of removing aluminium foil surface, uses the surface to be in the state of activation, is conducive to the one-level the anodic etching method to the hole of sending out of aluminium foil surface, is conducive to form equally distributed initial erosion point.
One-level the anodic etching method main purpose of the present invention is to cause the erosion point at aluminium foil surface, and the pit that uses the erosion point to form size reasonable, be evenly distributed.Adopt hydrochloric acid, sulfuric acid to add the homogenizing that the phosphoric acid corrosion system more is conducive to aluminium foil surface erosion point homogenizing and pit size.
Middle processing intent of the present invention is further pit to be enlarged after pit forms, and reduces the oxide-film that the hole inwall forms, and is conducive to the expansion of follow-up pit.
Secondary of the present invention, three grades of the anodic etching methods, its objective is the further reaming after higher level's operation is finished, final purpose is to use the aperture of etch pit to satisfy superhigh pressure (Vt 〉=800V) requirement of formation energy-endowing, and higher specific volume and the mechanical performance of maintenance.
Reprocessing purpose of the present invention is to remove the metal impurities on the inner residual chloride ion of aluminium foil, surface, through aluminium foil surface residual chlorine ion≤1mg/m after the reprocessing
2
Outstanding advantages of the present invention is: through after the improvement to pre-treatment, one-level the anodic etching method, middle processing, secondary the anodic etching method technique, the anode foils of producing can not only satisfy the demand that still changes into to 1000V superhigh pressure greater than 800V, and the product of output has the mechanical performance that leakage current is low, pressure rising time is fast and good.
Embodiment
Below by embodiment technical scheme of the present invention is further described in detail.
Adopt aluminium electrolytic capacitor of the present invention extra-high voltage anode foil caustic solution, unified clear and paper tinsel corrodes and it is changed into processing to 116 μ m Japan.
Embodiment 1
Aluminium electrolytic capacitor of the present invention extra-high voltage anode foil caustic solution comprises the steps:
1, pre-treatment:
Aluminium foil is placed on 70 ℃, and concentration is to soak 150 seconds in the 2.0wt% hydrochloric acid solution, takes out.
2, one-level the anodic etching method:
It is 85 ℃ that above-mentioned aluminium foil through pre-treatment is put into temperature, and concentration is to carry out the anodic etching method in 3wt% hydrochloric acid, 20wt% sulfuric acid and the 0.1wt% phosphoric acid mixed liquor, and current density is 0.5A/cm
2, electric weight is 30C/cm
2
3, middle processing 1:
It is 65 ℃ that above-mentioned aluminium foil through the one-level the anodic etching method is put into temperature, and concentration is dc electrolysis corrosion in 3.5wt% hydrochloric acid and the 0.08wt% ethanedioic acid mixed liquor, and current density is 0.02A/cm
2, electric weight is 3C/cm
2
4, secondary the anodic etching method:
It is 65 ℃ that the aluminium foil of processing in the above-mentioned process is put into temperature, and concentration is the anodic etching method in the mixed liquor of 3wt% nitric acid and 0.005wt% polyacrylamide, and current density is 0.10A/cm
2, electric weight is 30C/cm
2
5, middle processing 2:
It is 85 ℃ that above-mentioned aluminium foil through the one-level the anodic etching method is put into temperature, and concentration is dc electrolysis corrosion in the 4wt% hydrochloric acid 0.08wt% ethanedioic acid mixed liquor, and current density is 0.02A/cm
2, electric weight is 3.0C/cm
2
6, three grades of the anodic etching methods:
It is 65 ℃ that the aluminium foil of processing in the above-mentioned process is put into temperature, and concentration is the anodic etching method in the mixed liquor of 6wt% nitric acid and 0.005wt% polyacrylamide, and current density is 0.04A/cm
2, electric weight is 12C/cm
2
7, reprocessing
To put into temperature through the aluminium foil behind three grades of the anodic etching methods be 80 ℃ with above-mentioned, and concentration is to soak 30 seconds in the 12wt% salpeter solution.
Embodiment 2
Aluminium electrolytic capacitor of the present invention comprises the steps: with another embodiment of extra-high voltage anode foil caustic solution
1, pre-treatment:
Aluminium foil is placed on 65 ℃, and concentration is to soak 120 seconds in the 3.5wt% hydrochloric acid solution, takes out.
2, one-level the anodic etching method:
It is 80 ℃ that above-mentioned aluminium foil through pre-treatment is put into temperature, and concentration is to carry out the anodic etching method in 5wt% hydrochloric acid, 15wt% sulfuric acid and the 0.25wt% phosphoric acid mixed liquor, and current density is 0.4A/cm
2, electric weight is 30C/cm
2
3, middle processing 1:
It is 70 ℃ that above-mentioned aluminium foil through the one-level the anodic etching method is put into temperature, and concentration is dc electrolysis corrosion in 2wt% hydrochloric acid and the 0.02wt% ethanedioic acid mixed liquor, and current density is 0.05A/cm
2, electric weight is 6C/cm
2
4, secondary the anodic etching method:
It is 65 ℃ that the aluminium foil of processing in the above-mentioned process is put into temperature, and concentration is the anodic etching method in the mixed liquor of 6wt% nitric acid and 0.015wt% polyacrylamide, and current density is 0.12A/cm
2, electric weight is 36C/cm
2
5, middle processing 2:
It is 70 ℃ that above-mentioned aluminium foil through the one-level the anodic etching method is put into temperature, and concentration is dc electrolysis corrosion in 2wt% hydrochloric acid and the 0.02wt% ethanedioic acid mixed liquor, and current density is 0.05A/cm
2, electric weight is 6C/cm
2
6, three grades of the anodic etching methods:
It is 70 ℃ that the aluminium foil of processing in the above-mentioned process is put into temperature, and concentration is the anodic etching method in the mixed liquor of 3wt% nitric acid and 0.015wt% polyacrylamide, and current density is 0.08A/cm
2, electric weight is 24C/cm
2
7, reprocessing
To put into temperature through the aluminium foil behind three grades of the anodic etching methods be 70 ℃ with above-mentioned, and concentration is to soak 60 seconds in the 10wt% salpeter solution.
Embodiment 3
Aluminium electrolytic capacitor of the present invention comprises the steps: with the another embodiment of extra-high voltage anode foil caustic solution
1, pre-treatment:
Aluminium foil is placed on 60 ℃, and concentration is to soak 120 seconds in the 5wt% hydrochloric acid solution, takes out.
2, one-level the anodic etching method:
It is 75 ℃ that above-mentioned aluminium foil through pre-treatment is put into temperature, and concentration is to carry out the anodic etching method in 7.5wt% hydrochloric acid, 35wt% sulfuric acid and the 0.35wt% phosphoric acid mixed liquor, and current density is 0.35A/cm
2, electric weight is 25C/cm
2
3, middle processing 1:
It is 78 ℃ that above-mentioned aluminium foil through the one-level the anodic etching method is put into temperature, and concentration is dc electrolysis corrosion in 2wt% hydrochloric acid and the 0.14wt% ethanedioic acid mixed liquor, and current density is 0.075A/cm
2, electric weight is 5C/cm
2
4, secondary the anodic etching method:
It is 75 ℃ that the aluminium foil of processing in the above-mentioned process is put into temperature, and concentration is the anodic etching method in the mixed liquor of 10wt% nitric acid and 0.03wt% polyacrylamide, and current density is 0.15A/cm
2, electric weight is 45C/cm
2
5, middle processing 2:
It is 78 ℃ that above-mentioned aluminium foil through the one-level the anodic etching method is put into temperature, and concentration is dc electrolysis corrosion in 2wt% hydrochloric acid and the 0.14wt% ethanedioic acid mixed liquor, and current density is 0.075A/cm
2, electric weight is 5C/cm
2
6, three grades of the anodic etching methods:
It is 75 ℃ that the aluminium foil of processing in the above-mentioned process is put into temperature, and concentration is the anodic etching method in the mixed liquor of 10wt% nitric acid and 0.03wt% polyacrylamide, and current density is 0.12A/cm
2, electric weight is 36C/cm
2
7, reprocessing
To put into temperature through the aluminium foil behind three grades of the anodic etching methods be 75 ℃ with above-mentioned, and concentration is to soak 75 seconds in the 7.5wt% salpeter solution.
Embodiment 4
Aluminium electrolytic capacitor of the present invention comprises the steps: with another embodiment of extra-high voltage anode foil caustic solution
1, pre-treatment:
Aluminium foil is placed on 50 ℃, and concentration is to soak 60 seconds in the 6wt% hydrochloric acid solution, takes out.
2, one-level the anodic etching method:
It is 65 ℃ that above-mentioned aluminium foil through pre-treatment is put into temperature, and concentration is to carry out the anodic etching method in 10wt% hydrochloric acid, 20wt% sulfuric acid and the 0.5wt% phosphoric acid mixed liquor, and current density is 0.25A/cm
2, electric weight is 20C/cm
2
3, middle processing 1:
It is 85 ℃ that above-mentioned aluminium foil through the one-level the anodic etching method is put into temperature, and concentration is dc electrolysis corrosion in 6wt% hydrochloric acid and the 0.25wt% ethanedioic acid mixed liquor, and current density is 0.10A/cm
2, electric weight is 6C/cm
2
4, secondary the anodic etching method:
It is 80 ℃ that the aluminium foil of processing in the above-mentioned process is put into temperature, and concentration is the anodic etching method in the mixed liquor of 15wt% nitric acid and 0.05wt% polyacrylamide, and current density is 0.06A/cm
2, electric weight is 18C/cm
2
5, middle processing 2:
It is 85 ℃ that above-mentioned aluminium foil through the one-level the anodic etching method is put into temperature, and concentration is dc electrolysis corrosion in 6wt% hydrochloric acid and the 0.25wt% ethanedioic acid mixed liquor, and current density is 0.10A/cm
2, electric weight is 6C/cm
2
6, three grades of the anodic etching methods:
It is 80 ℃ that the aluminium foil of processing in the above-mentioned process is put into temperature, and concentration is the anodic etching method in the mixed liquor of 15wt% nitric acid and 0.05wt% polyacrylamide, and current density is 0.08A/cm
2, electric weight is 24C/cm
2
7, reprocessing
To put into temperature through the aluminium foil behind three grades of the anodic etching methods be 60 ℃ with above-mentioned, and concentration is to soak 90 seconds in the 5wt% salpeter solution.
Wherein embodiment 1~4 aluminium foil changes into condition and is: 90 ℃ of 0.05A/ ㎝ of 10% boric acid
2Vfe is 820V or 900V.
Change into rear aluminium foil properties such as table 1
Can find out according to upper table performance feature: use technique of the present invention to stablize to make the Vt value to reach the above anode etched foil of 850V, wherein the extra-high voltage anode foil electrical property among embodiment 1 and the embodiment 3 etc. has all reached higher level.
Specific embodiment of the present invention is only to the theory for example of the present invention's spirit; under the R﹠D personnel of technical field various modifications that described specific embodiment is done or replenish or adopt similar mode to substitute; but the improvement not departing from spirit of the present invention and doing all belongs to protection scope of the present invention.
Claims (1)
1. aluminium electrolytic capacitor extra-high voltage anode foil caustic solution is characterized in that the method may further comprise the steps:
A, pre-treatment: aluminium foil is placed on 50~70 ℃, and concentration is to soak in 2.0~6.0wt% hydrochloric acid solution 60~150 seconds,
B, one-level the anodic etching method: it is 65~85 ℃ that above-mentioned aluminium foil through pre-treatment is put into temperature, concentration is to carry out the anodic etching method in 3~10wt% hydrochloric acid, 20~35wt% sulfuric acid and the 0.1~0.5wt% phosphoric acid mixed liquor, and current density is 0.25~0.50A/cm
2, electric weight is 20~30C/cm
2,
C, middle processing 1: it is 65~85 ℃ that above-mentioned aluminium foil through the one-level the anodic etching method is put into temperature, and concentration is dc electrolysis corrosion in 2~6wt% hydrochloric acid and the 0.02~0.25wt% ethanedioic acid mixed liquor, and current density is 0.02~0.10A/cm
2, electric weight is 3~6C/cm
2,
D, secondary the anodic etching method: it is 65~80 ℃ that the aluminium foil of processing in the above-mentioned process is put into temperature, concentration is the anodic etching method in the mixed liquor of 3~15wt% nitric acid and 0.005~0.05wt% polyacrylamide, and current density is 0.06~0.15A/cm
2, electric weight is 18~45C/cm
2,
E, middle processing 2: it is 65~85 ℃ that above-mentioned aluminium foil through the secondary the anodic etching method is put into temperature, and concentration is dc electrolysis corrosion in 2~6wt% hydrochloric acid and the 0.02~0.25wt% ethanedioic acid mixed liquor, and current density is 0.02~0.10A/cm
2, electric weight is 3~6C/cm
2,
F, three grades of the anodic etching methods: it is 65~80 ℃ that the aluminium foil of processing in the above-mentioned process is put into temperature, concentration is secondary the anodic etching method in the mixed liquor of 3~15wt% nitric acid and 0.005~0.05wt% polyacrylamide, and current density is 0.04~0.12A/cm
2, electric weight is 12~36C/cm
2,
G, reprocessing: to put into temperature through the aluminium foil behind three grades of the anodic etching methods be 60~80 ℃ with above-mentioned, and concentration is to soak in 5~12wt% salpeter solution 30~90 seconds.
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CN103280321A (en) * | 2013-05-16 | 2013-09-04 | 陶荣燕 | Preparation method of electrode foil |
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