CN102360954B - Method capable of improving specific volume of anode foil of aluminum electrolytic capacitor - Google Patents
Method capable of improving specific volume of anode foil of aluminum electrolytic capacitor Download PDFInfo
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- CN102360954B CN102360954B CN 201110277211 CN201110277211A CN102360954B CN 102360954 B CN102360954 B CN 102360954B CN 201110277211 CN201110277211 CN 201110277211 CN 201110277211 A CN201110277211 A CN 201110277211A CN 102360954 B CN102360954 B CN 102360954B
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Abstract
The invention relates to an aluminum electrolytic capacitor, in particular to a method capable of improving specific volume of an anode foil of an aluminum electrolytic capacitor. The method comprises the following steps: (1) dipping an etched foil after primary and secondary alternating current (AC) corrosion treatment in specific solution with the aid of heating and ultrasonic treatment; (2) carrying out high-temperature heat treatment on the dipped aluminum foil so as to form a compound during the reaction process; and (3) anodizing the aluminum foil after heat treatment in electrolyte solution so as to finally form a composite membrane with high dielectric constant on the surface of the aluminum foil. Compared with the anode foil obtained by the traditional method, the specific capacitance of the aluminum anode foil obtained by the manufacturing method provided by the invention is improved by more than 15%, and the dielectric loss can meet the use requirements for the aluminum electrolytic capacitor. The manufacturing method provided by the invention has the advantages of simple process and low cost, and is convenient for operation and easy to control, thus being suitable for large-scale industrial production of the anode foils of various aluminum electrolytic capacitors.
Description
Technical field
The present invention relates to aluminium electrolytic capacitor, particularly a kind of method that improves the aluminum electrolysis capacitor anode foil specific volume.
Background technology
Along with developing rapidly of electronic industry, the sharply expansion of the produce markets such as computer, communication products and household electrical appliances, demand to aluminium electrolytic capacitor also sharply rises, at present, the aluminium electrolytic capacitor development trend is miniaturization, chip type, high temperature resistant and long-life, so Fabrication of High Specific Capacitance electrode foil manufacturing technology becomes the key of making the high-quality aluminum electrolytic capacitor.the ratio electric capacity of aluminium electrolytic capacitor is directly proportional to effective surface area and the dielectric constant of its dielectric layer, therefore, introduce high-k metal (pottery) base and form complex oxide film with aluminum substrate, the dielectric constant that improves dielectric layer is one of method that very effectively improves specific volume, in prior art by advancing one-level, electrode foil after the secondary corrosion floods in specific solution, by drying, heat treatment, the final composite membrane that obtains to contain high-k of the processes such as anodic oxidation, can increase substantially the anode foils specific volume by this kind process, yet in dipping process, it is inhomogeneous that etched foil surface-coated rete appears sometimes, surface coverage too much causes high dielectric material obstruction hole to cause specific area to reduce the unfavorable factors such as even specific volume reduction, these are also to improve the specific volume problem needing to overcome at anode foils surface preparation composite membrane at present.
Summary of the invention
Research purpose of the present invention is to overcome above-mentioned prior art and makes the defective that composite membrane exists, take ultrasonic processing and the water-bath of specific solution and auxiliary certain frequency in dipping process, solved in the unequal phenomenon of etched foil surface-coated, and by follow-up heat treatment, specific anodic oxidation, finally make Al
2O
3-TiO
2The complex oxide film electrode material, thus the specific volume of aluminum electrolysis capacitor anode foil improved.
Process of the present invention comprises the five steps such as colloidal sol preparation, impregnation process, dry processing, high-temperature heat treatment, anodized.Concrete steps are as follows:
A) colloidal sol preparation: add butyl titanate and constantly stir at absolute ethyl alcohol, drip simultaneously glacial acetic acid, and the pH value of controlling solution making the solution-stabilized existence of configuration in the 3-4 scope;
B) stabilizing solution that impregnation process: will be placed in steps A through the etched foil after one-level, secondary corrosion) prepares, in 30 ~ 70KHz ultrasound environments, dip time 10-120s, dipping temperature are 30 ~ 40 ℃;
C) the dry processing: the etched foil after flooding cleans up in the baking oven that is placed on 50-100 ℃ dry with deionized water;
D) heat treatment process: be to process 1-10 min under the hot conditions of 500-600 ℃ in pure oxygen atmosphere in temperature with dried etched foil in above-mentioned C;
E) anodized: the aluminium foil after processing in above-mentioned D is placed in ammonium adipate and phosphoric acid ammonia mixed aqueous solution carries out namely obtaining the composite anode paper tinsel after anodic oxidation.
Described steps A specific operation process is: butyl titanate is dissolved in absolute ethyl alcohol, wherein butyl titanate is 1.5mol/l in the molar concentration of absolute ethyl alcohol, stir 30min, make mixed liquor A, drip glacial acetic acid in mixed liquor A, continue to stir 30min, make mixed liquid B, the addition of glacial acetic acid is 1-2 times of mixed liquor A volume, adopts at last the pH value of glacial acetic acid adjusting mixed liquid B between 3-4, makes Stability of Sols.
Described step e Anodic Oxidation is completed in ammonium adipate and phosphoric acid ammonia mixed aqueous solution, ammonium adipate concentration is the 1-30%(mass fraction), phosphoric acid ammonia concentration is 0.01 mol/L-3mol/L, oxidizing temperature is between 80-90 ℃, oxidation voltage 10-50V, oxidization time 1-30min, electric current are 0.01 ~ 0.1A/cm
2
beneficial effect of the present invention is: by take ultrasonic auxiliary and suitable water-bath in the impregnation process process, ultrasonic wave forms pneumatics in colloidal sol, form a large amount of cavities, then be subject to normal pressure compressed, produce well differentiated cavitation bubble, when breaking, it can produce localized hyperthermia's high pressure, solia particle is suspended more even in colloidal sol, avoiding particulate to form reunites, on the other hand, the ultrasonic aluminium foil aperture that helps after further activation corrosion, should more be conducive to the combination of rete and carrier on the physical property, thereby form more uniform and smooth overlay, make the better of the aluminium of composite membrane and titanium combination.In addition, in heat treatment process, by processing, effectively guaranteed the compound of surface alumina oxide and titanium oxide in pure oxygen environment.Adopt at last ammonium adipate and phosphoric acid ammonia mixed liquor to carry out oxidation processes in anode oxidation process, thereby improve the specific volume of electrode foil, the electric property of intensifier electrode paper tinsel.
Embodiment
Embodiment 1:
1, under room temperature, the 0.015mol butyl titanate is dissolved in the 10ml absolute ethyl alcohol, stirs 30min, get mixed liquor A, drip the 20ml glacial acetic acid in A, continue to stir 30min, get mixed liquid B, the pH value with glacial acetic acid adjusting mixed liquid B is 3 at last, makes Stability of Sols;
2, be that 1cm * 5cm etched foil is placed in the above-mentioned stabilizing solution for preparing at 30 ℃ and floods 30S with one section area, whole dipping process is completed under auxiliary ultrasonic, and supersonic frequency is 60KHz;
3, the aluminium foil distilled water wash clean that above-mentioned dipping is good is put into subsequently 100 ℃ of baking ovens and is dried;
4, will dry good aluminium foil and heat-treat in pure oxygen environment, heat treatment temperature is 550 ℃, and the time is 8min;
5, the sample that heat treatment is good is placed in 15% ammonium adipate+0.1 mol/L phosphoric acid ammonia mixed aqueous solution at last, when temperature is 85 ℃, and anodic oxidation under the voltage of 20V, current density is 0.05 A/cm
-2, oxidization time 6min.
Comparative Examples 1:
1, under room temperature, the 0.015mol butyl titanate is dissolved in the 10ml absolute ethyl alcohol, stirs 30min, get mixed liquor A, drip the 20ml glacial acetic acid in A, continue to stir 30min, get mixed liquid B, the pH value with glacial acetic acid adjusting mixed liquid B is 3 at last, makes Stability of Sols;
2, be that 1cm * 5cm etched foil is placed in the above-mentioned stabilizing solution for preparing at 30 ℃ and floods 30S with one section area;
3, the aluminium foil distilled water wash clean that above-mentioned dipping is good is put into subsequently 100 ℃ of baking ovens and is dried;
4, will dry good aluminium foil and heat-treat in air atmosphere, heat treatment temperature is 550 ℃, and heat treatment time is 6min;
5, the sample that heat treatment is good is placed in the 15%(mass fraction at last) the ammonium adipate aqueous solution, in the time of 85 ℃, anodic oxidation under the voltage of 20V, current density is 0.05 A/cm
-2, oxidization time 8min.
Embodiment 2:
1, under room temperature, the 0.015mol butyl titanate is dissolved in the 10ml absolute ethyl alcohol, stirs 30min, get mixed liquor A, drip in A
15The ml glacial acetic acid continues to stir 30min, gets mixed liquid B, and the pH value with glacial acetic acid adjusting mixed liquid B is 4 at last, makes Stability of Sols;
2, be that 1cm * 5cm etched foil exists with one section area
40 ℃Be placed in the above-mentioned colloidal sol for preparing and flood 120S, whole dipping process is completed under ultrasonic assisting, and supersonic frequency is 30KHz;
3, the aluminium foil distilled water wash clean that above-mentioned dipping is good is put into subsequently 50 ℃ of baking ovens and is dried;
4, will dry good aluminium foil and heat-treat in pure oxygen environment, heat treatment temperature is 500 ℃, and heat treatment time is 10min;
5, the sample that heat treatment is good is placed at last
Ammonium adipate+2.8mol/L of 2%In phosphoric acid ammonia mixed aqueous solution, in the time of 90 ℃, anodic oxidation under the voltage of 50V, current density is 0.1 A/cm
-2, oxidization time 2min.
Comparative Examples 2:
1, under room temperature, the 0.015mol butyl titanate is dissolved in the 10ml absolute ethyl alcohol, stirs 30min, get mixed liquor A, drip the 15ml glacial acetic acid in A, continue to stir 30min, get mixed liquid B, the pH value with glacial acetic acid adjusting mixed liquid B is 4 at last, makes Stability of Sols;
2, be that 1cm * 5cm etched foil is placed in the above-mentioned colloidal sol for preparing at 40 ℃ and floods 120S with one section area.
3, the aluminium foil distilled water wash clean that above-mentioned dipping is good is put into subsequently 50 ℃ of baking ovens and is dried.
4, will dry good aluminium foil and heat-treat in air atmosphere, heat treatment temperature is 500 ℃, and heat treatment time is 10min.
5, the sample that heat treatment is good is placed in the 2%(mass fraction at last) the ammonium adipate aqueous solution, in the time of 90 ℃, anodic oxidation under the voltage of 50V, current density is 0.1A/cm
-2, oxidization time 2min.
Embodiment 3:
1, under room temperature, the 0.015mol butyl titanate is dissolved in the 10ml absolute ethyl alcohol, stirs 30min, get mixed liquor A, drip the 10ml glacial acetic acid in A, continue to stir 30min, get mixed liquid B, the pH value with glacial acetic acid adjusting mixed liquid B is 3 at last, makes Stability of Sols;
2, be that 1cm * 5cm etched foil is placed in the above-mentioned colloidal sol for preparing at 40 ℃ and floods 15S with one section area, whole dipping process is completed under auxiliary ultrasonic, and supersonic frequency is 70KHz;
3, the aluminium foil distilled water wash clean that above-mentioned dipping is good is put into subsequently 80 ℃ of baking ovens and is dried;
4, will dry good aluminium foil and heat-treat in pure oxygen environment, heat treatment temperature is 600 ℃, and heat treatment time is 2min;
5, the sample that heat treatment is good is placed in 25% ammonium adipate+1 mol/L phosphoric acid ammonia mixed aqueous solution at last, in the time of 90 ℃, and anodic oxidation under the voltage of 10V, current density is 0.01 A/cm
-2, oxidization time 10min.
Comparative Examples 3:
1, under room temperature, the 0.015mol butyl titanate is dissolved in the 10ml absolute ethyl alcohol, stirs 30min, get mixed liquor A, drip the 10ml glacial acetic acid in A, continue to stir 30min, get mixed liquid B, the pH value with glacial acetic acid adjusting mixed liquid B is 3 at last, makes Stability of Sols;
2, be that 1cm * 5cm etched foil is placed in the above-mentioned colloidal sol for preparing at 40 ℃ and floods 15S with one section area;
3, the aluminium foil distilled water wash clean that above-mentioned dipping is good is put into subsequently 80 ℃ of baking ovens and is dried.
4, will dry good aluminium foil and heat-treat in air atmosphere, heat treatment temperature is 600 ℃, and heat treatment time is 2min;
5, the sample that heat treatment is good is placed in the 25%(mass fraction at last) the ammonium adipate aqueous solution, in the time of 90 ℃, anodic oxidation under the voltage of 10V, current density is 0.01 A/cm
-2, oxidization time 10min.
Embodiment 4:
1, under room temperature, the 0.015mol butyl titanate is dissolved in the 10ml absolute ethyl alcohol, stirs 30min, get mixed liquor A, drip the 20ml glacial acetic acid in A, continue to stir 30min, get mixed liquid B, the pH value with glacial acetic acid adjusting mixed liquid B is 4 at last, makes Stability of Sols;
2, be that 1cm * 5cm etched foil is placed in the above-mentioned colloidal sol for preparing at 40 ℃ and floods 80S with one section area, whole dipping process is completed under auxiliary ultrasonic, and supersonic frequency is 40KHz;
3, the aluminium foil distilled water wash clean that above-mentioned dipping is good is put into subsequently 100 ℃ of baking ovens and is dried;
4, will dry good aluminium foil and heat-treat in pure oxygen environment, heat treatment temperature is 600 ℃, and heat treatment time is 3min;
5, the sample that heat treatment is good is placed in 30% ammonium adipate+0.01mol/L phosphoric acid ammonia mixed aqueous solution at last, in the time of 85 ℃, and anodic oxidation under the voltage of 40V, current density is 0.08 A/cm
-2, oxidization time 4min.
Comparative Examples 4:
1, under room temperature, the 0.015mol butyl titanate is dissolved in the 10ml absolute ethyl alcohol, stirs 30min, get mixed liquor A, drip the 20ml glacial acetic acid in A, continue to stir 30min, get mixed liquid B, the pH value with glacial acetic acid adjusting mixed liquid B is 4 at last, makes Stability of Sols;
2, be that 1cm * 5cm etched foil is placed in the above-mentioned colloidal sol for preparing at 40 ℃ and floods 80S with one section area;
3, the aluminium foil distilled water wash clean that above-mentioned dipping is good is put into subsequently 100 ℃ of baking ovens and is dried;
4, will dry good aluminium foil and heat-treat in air atmosphere, heat treatment temperature is 600 ℃, and heat treatment time is 3min;
5, the sample that heat treatment is good is placed in the 30%(mass fraction at last) the ammonium adipate aqueous solution, in the time of 85 ℃, anodic oxidation under the voltage of 40V, current density is 0.08 A/cm
-2, oxidization time 4min.
Embodiment 1 ~ 4th, specific embodiments of the present invention, and Comparative Examples 1 ~ 4th, the technique of originally taking, by respectively Waste Acid From Hua Cheng Foil being carried out than capacity measurement, during test result is listed in the table below:
Claims (3)
1. method that improves the aluminum electrolysis capacitor anode foil specific volume
,Concrete steps are:
A) colloidal sol preparation: add butyl titanate and constantly stir at absolute ethyl alcohol, drip simultaneously glacial acetic acid, and the pH value of controlling solution making the solution-stabilized existence of configuration in the 3-4 scope;
B) stabilizing solution that impregnation process: will be placed in steps A through the etched foil after one-level, secondary corrosion) prepares, in 30 ~ 70KHz ultrasound environments, dip time 10-120s, dipping temperature are 30 ~ 40 ℃;
C) the dry processing: the etched foil after flooding cleans up in the baking oven that is placed on 50-100 ℃ dry with deionized water;
D) high-temperature heat treatment: with step C), dried etched foil is to process 1-10 min under the hot conditions of 500-600 ℃ in pure oxygen atmosphere in temperature;
E) aluminium foil anodized: with above-mentioned D) after high-temperature heat treatment is placed in ammonium adipate and phosphoric acid ammonia mixed aqueous solution carries out namely obtaining the composite anode paper tinsel after anodic oxidation.
2. a kind of method that improves the aluminum electrolysis capacitor anode foil specific volume as claimed in claim 1, it is characterized in that: described steps A) specific operation process is: butyl titanate is dissolved in absolute ethyl alcohol, wherein butyl titanate is 1.5mol/l in the molar concentration of absolute ethyl alcohol, stir 30min, make mixed liquor A, drip glacial acetic acid in mixed liquor A, continue to stir 30min, make mixed liquid B, the addition of glacial acetic acid is 1-2 times of mixed liquor A volume, adopt at last the pH value of glacial acetic acid adjusting mixed liquid B between 3-4, make Stability of Sols.
3. a kind of method that improves the aluminum electrolysis capacitor anode foil specific volume as claimed in claim 1, it is characterized in that: described step e) Anodic Oxidation is completed in ammonium adipate and phosphoric acid ammonia mixed aqueous solution, ammonium adipate concentration is the 1-30%(mass fraction), phosphoric acid ammonia concentration is 0.01 mol/L-3mol/L, oxidizing temperature is between 80-90 ℃, oxidation voltage 10-50V, oxidization time 1-30min, electric current are 0.01 ~ 0.1A/cm
2
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103187176B (en) * | 2013-03-22 | 2015-12-02 | 常州大学 | A kind of etching process of anode aluminum foil of electrolytic capacitor |
| CN103601273B (en) * | 2013-11-13 | 2015-01-14 | 清华大学 | Nano titanium dioxide modification method of electric adsorption desalinization carbon electrode |
| CN105420803A (en) * | 2015-11-27 | 2016-03-23 | 广西贺州市桂东电子科技有限责任公司 | Method for ultrasonic-assisted corrosion of middle-high voltage anode aluminum foil |
| CN105862116A (en) * | 2016-04-10 | 2016-08-17 | 江苏荣生电子有限公司 | Method for manufacturing energy storage foil by utilizing ultrasonic treatment |
| CN106340404B (en) * | 2016-09-12 | 2018-11-27 | 肇庆华锋电子铝箔股份有限公司 | A kind of preparation method of the high dielectric nano complex oxide film anode foils of low-voltage aluminum electrolytic capacitor |
| CN113161150A (en) * | 2021-04-22 | 2021-07-23 | 湖南艾华集团股份有限公司 | Preparation method of anode foil composite film of aluminum electrolytic capacitor |
| CN117904690B (en) * | 2024-03-20 | 2024-06-04 | 南通江海电容器股份有限公司 | Preparation method and application of formed foil |
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| CN1391243A (en) * | 2002-07-24 | 2003-01-15 | 扬州宏远电子有限公司 | Process for preparing 35Vw and 50Vw anode foil with high specific capacity and low contact resistance |
| CN1873865A (en) * | 2006-04-05 | 2006-12-06 | 江苏中联科技集团有限公司 | Method for increasing specific volume of electrode foil for aluminum electrolytic capacitor |
| CN101425393A (en) * | 2008-07-29 | 2009-05-06 | 东莞市东阳光电容器有限公司 | Cathode foil manufacturing method for aluminum electrolysis capacitor |
| CN101736381A (en) * | 2009-12-28 | 2010-06-16 | 新疆众和股份有限公司 | Electrolyte and method for preparing aluminum oxide template with big hole pitch |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1391243A (en) * | 2002-07-24 | 2003-01-15 | 扬州宏远电子有限公司 | Process for preparing 35Vw and 50Vw anode foil with high specific capacity and low contact resistance |
| CN1873865A (en) * | 2006-04-05 | 2006-12-06 | 江苏中联科技集团有限公司 | Method for increasing specific volume of electrode foil for aluminum electrolytic capacitor |
| CN101425393A (en) * | 2008-07-29 | 2009-05-06 | 东莞市东阳光电容器有限公司 | Cathode foil manufacturing method for aluminum electrolysis capacitor |
| CN101736381A (en) * | 2009-12-28 | 2010-06-16 | 新疆众和股份有限公司 | Electrolyte and method for preparing aluminum oxide template with big hole pitch |
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