CN101425389A - Aluminum electrolysis capacitor anode foil manufacturing method - Google Patents
Aluminum electrolysis capacitor anode foil manufacturing method Download PDFInfo
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- CN101425389A CN101425389A CNA2008100298015A CN200810029801A CN101425389A CN 101425389 A CN101425389 A CN 101425389A CN A2008100298015 A CNA2008100298015 A CN A2008100298015A CN 200810029801 A CN200810029801 A CN 200810029801A CN 101425389 A CN101425389 A CN 101425389A
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Abstract
The invention relates to a preparation method of an anode foil for aluminum electrolytic capacitors. The preparation method comprises boiling in pure water, first-level formation, phosphating treatment, reformation treatment and post-treatment. The phosphating treatment plays a role in depolarization, effectively improves the electrical properties of filam, removes or dissolves the impurities in pores and irregular alumina hydrated film and effectively increases the specific surface area of foil. The invention adds the phosphating treatment after the first-level formation, which is favorable for improving the electrostatic capacity, mechanical strength and water resistance of the foil, thereby an anode foil for aluminum electrolytic capacitors with high specific volume, high intensity, little leakage current and good water resistance can be produced.
Description
Technical field:
The present invention relates to anode foil manufacturing method, especially refer to the manufacture method of the middle and high pressure anode foils of aluminium electrolytic capacitor.
Background technology:
It is the main material of making middle and high jewelling electrolytic capacitor that middle and high pressure is anodizing to paper tinsel, and the quality of its performance is the performance of decision capacitor product directly, is exactly that the etched foil surface generates one deck compact structure, the good crystal formation γ-Al of insulation property in the formation process
2O
3Oxide-film is as the working media of capacitor, thereby the electrical property of oxide-film and anti-hydrability are the keys of capacitor performance quality.At present, medium-high voltage aluminum electrolytic capacitor is such with the manufacture method of electrode foil: this etched foil is boiled 9min in pure water; Under 85 ℃ of temperature, in boric acid 10% and 0.1% the salicylic acid solution with 20mAcm
-2Current density carry out the first order and change into, voltage arrives constant voltage 9min behind the 110V; With boosting to constant voltage 9min behind the 219V under the same conditions; Constant voltage 35min after the same terms boosts to 365V; Heat treatment 2min in 500 ℃ of temperature; Add the ammonium citrate of 250ppm and the phosphoric acid of 750ppm in the boric acid of 5wt%, regulate pH to 6.0 with ammoniacal liquor, under 85 ℃ of temperature, 365V changes into 9min again; Under 60 ℃ of temperature, handle 3min in 5% the phosphoric acid; Under 85 ℃ of temperature, in the boric acid of 5wt%, add the ammonium citrate of 250ppm and the phosphoric acid of 750ppm, 365V changes into 9min again; Heat treatment 2min in 500 ℃ of temperature; Under 85 ℃ of temperature, 365V changes into 5min again; Under 50 ℃ of temperature, in the 1wt% ammonium phosphate solution, handle 2min.The electrode foil oxide-film poor water resistance of making in this way, capacity is little, leakage current is big, intensity difference.Thisly be anodizing to the electrolytic capacitor poor performance that paper tinsel is made, useful life is short, can not satisfy life at all and producing the demand more and more higher to the aluminium electrolytic capacitor performance requirement.
Summary of the invention:
Be the desirability of adaptation electrolytic capacitor high life performance and the development trend of miniaturization, a kind of high power capacity that the objective of the invention is to overcome above-mentioned weak point and provide, high strength, the medium-high voltage aluminum electrolytic capacitor of the high life manufacture method of electrode foil, comprise that boiling pure water, one-level change into, phosphatization is handled, change into again and reprocessing, one-level changes into the back phosphatization and handles, played unpolarized effect, improve the electrical property of oxide-film, can remove or dissolve impurity and irregular alumina hydration film in the hole, effectively increase the specific surface area of paillon foil.
The invention provides and a kind ofly comprise that boiling pure water, one-level change into, phosphatization is handled, change into the aluminum electrolysis capacitor anode foil manufacturing method with reprocessing again.Employing aluminium purity is 99.99% high pressure etched foil, and this etched foil is boiled 9min in pure water; Under 85 ℃ of temperature, in boric acid 10% and 0.1% the salicylic acid solution with 20mAcm
-2The close current density row first order of advancing of electric current change into, voltage arrives constant voltage 9min behind the 110V; One-level changes into the back and carries out the phosphatization processing with in phosphoric acid, phosphate or the organophosphor one or more, and content is 1wt%～20wt%, processing time 1min～10min, 20 ℃～70 ℃ of treatment temperatures; With one-level change into boost to 219V under the same terms after constant voltage 9min; With one-level change into the same terms boost to 365V after constant voltage 35min; Heat treatment 2min in 500 ℃ of temperature; Under 85 ℃ of temperature, in the boric acid of 5wt%, add the ammonium citrate of 250ppm and the phosphoric acid of 750ppm, regulate pH to 6.0 with ammoniacal liquor, under 85 ℃ of temperature, 365V changes into 9min again; Under 60 ℃ of temperature, handle 3min in 5% the phosphoric acid; Under 85 ℃ of temperature, in the boric acid of 5wt%, add the ammonium citrate of 250ppm and the phosphoric acid of 750ppm, regulate pH to 6.0 with ammoniacal liquor, 365V changes into 9min again; Heat treatment 2min in 500 ℃ of temperature; Under 85 ℃ of temperature, 365V changes into 5min again; Under 50 ℃ of temperature, in the 1wt% ammonium phosphate solution, handle 2min.
Used phosphate is ammonium dihydrogen phosphate in phosphatization is handled.
Beneficial effect of the present invention is: aluminum electrolysis capacitor anode foil manufacturing method comprises that boiling pure water, one-level change into, phosphatization is handled, changes into and reprocessing again.Phosphatization is handled and has been played unpolarized effect, can remove or dissolve impurity and irregular alumina hydration film in the hole, has effectively increased the specific surface area of paillon foil, improves the electrical property of paillon foil.
Embodiment:
Describe the present invention in detail below by embodiment:
Aluminium purity is 99.99% mesohigh etched foil, and the 375Vfe specific volume is 1.233ufcm
-2
Embodiment 1:
By weight percentage:
The first step: this etched foil is boiled 9min in pure water;
Second the step: under 85 ℃ of temperature, in boric acid 10% and 0.1% the salicylic acid solution with 20mA-cm
-2The current density row first order change into, voltage arrives constant voltage 9min behind the 110V;
The 3rd step: in 3% phosphoric acid solution, handle 4min under 55 ℃ of temperature;
The 4th step: constant voltage 9min after boosting to 219V under the step 2 reaction condition;
The 5th step: constant voltage 35min after boosting to 365V under the step 2 reaction condition;
The 6th step: heat treatment 2min in 500 ℃ of temperature;
The 7th step: in the boric acid of 5wt%, add the ammonium citrate of 250ppm and the phosphoric acid of 750ppm, regulate pH to 6.0 with ammoniacal liquor.Under 85 ℃ of temperature, 365V changes into 9min again;
The 8th step: under 60 ℃ of temperature, handle 3min in 5% the phosphoric acid;
The 9th step: under the step 7 reaction condition, 365V changes into 9min again;
The tenth step: heat treatment 2min in 500 ℃ of temperature;
The 11 step: under the step 7 reaction condition, 365V changes into 5min again;
The 12 step: under 50 ℃ of temperature, in the 1wt% ammonium phosphate solution, handle 2min.
Through the above-mentioned specific volume of electrode foil that changes into processing is 1.270ufcm
-2, leakage current 80mA/5cm
-2, the withstand voltage 375V of epithelium, bending 146 times, resistance to water experiment: paillon foil rises to 15 seconds withstand voltage times of advent of epithelium.
Embodiment 2:
By weight percentage:
The first step: this etched foil is boiled 9min in pure water;
Second the step: under 85 ℃ of temperature, in boric acid 10% and 0.1% the salicylic acid solution with 20mA.cm
-2The close current density row first order of advancing of electric current change into, voltage arrives constant voltage 9min behind the 110V;
The 3rd step: in 5% phosphoric acid and 0.5% ammonium dihydrogen phosphate (PDA) solution, handle 4min under 50 ℃ of temperature;
The 4th step: constant voltage 9min after boosting to 219V under the step 2 reaction condition;
The 5th step: constant voltage 35min after the step 2 reaction condition boosts to 365V;
The 6th step: heat treatment 2min in 500 ℃ of temperature;
The 7th step: in the boric acid of 5wt%, add the ammonium citrate of 250ppm and the phosphoric acid of 750ppm, regulate pH to 6.0 with ammoniacal liquor.Under 85 ℃ of temperature, 365V changes into 9min again;
The 8th step: under 60 ℃ of temperature, handle 3min in 5% the phosphoric acid;
The 9th step: under the step 7 reaction condition, 365V changes into 9min again;
The tenth step: heat treatment 2min in 500 ℃ of temperature;
The 11 step: under the step 7 reaction condition, 365V changes into 5min again;
The 12 step: under 50 ℃ of temperature, in the 1wt% ammonium phosphate solution, handle 2min.
Through the above-mentioned specific volume of electrode foil that changes into processing is 1.258uf.cm
-2, leakage current 60mA/5cm
-2, the withstand voltage 375V of epithelium, bending 152 times, resistance to water experiment: paillon foil rises to 9 seconds withstand voltage times of advent of epithelium.
Comparative example:
Make aluminum electrolysis capacitor anode foil with original technology, by weight percentage:
The first step: this etched foil is boiled 9min in pure water;
Second step: under 85 ℃ of temperature, be 20mAcm with the current density in boric acid 10% and 0.1% the salicylic acid solution
-2Boost to constant voltage 9min behind the 110V;
The 3rd step: constant voltage 9min after boosting to 219V under the step 2 reaction condition;
The 4th step: constant voltage 35min after the step 2 reaction condition boosts to 365V;
The 5th step: heat treatment 2min in 500 ℃ of temperature;
The 6th step: in the boric acid of 5wt%, add the ammonium citrate of 250ppm and the phosphoric acid of 750ppm, regulate pH to 6.0 with ammoniacal liquor.Under 85 ℃ of temperature, 365V changes into 9min again:
The 7th step: under 60 ℃ of temperature, handle 3min in 5% the phosphoric acid;
The 8th step: under the step 6 reaction condition, 365V changes into 9min again;
The 9th step: heat treatment 2min in 500 ℃ of temperature;
The tenth step: under the step 6 reaction condition, 365V changes into 5min again;
The 11 step: under 50 ℃ of temperature, in the 1wt% ammonium phosphate solution, handle 2min.
The specific volume of electrode foil that changes into processing with original technology is 1.228ufcm
-2, leakage current 105mA/5cm
-2, the withstand voltage 375V of epithelium, bending 118 times, resistance to water experiment: paillon foil rises to 36 seconds withstand voltage times of advent of epithelium.
By the contrast experiment as can be seen, carry out phosphatization after one-level changes under certain condition and handle, can produce the aluminium electrolytic capacitor mesohigh anode foils that capacitance is big, leakage current is little, water resistance is better, mechanical strength is high.
Claims (3)
1, a kind of aluminum electrolysis capacitor anode foil manufacturing method is characterized in that: may further comprise the steps: boiling pure water, one-level change into, phosphatization is handled, change into and reprocessing again.
2, aluminum electrolysis capacitor anode foil manufacturing method according to claim 1, it is characterized in that: after one-level changes into, increased the phosphatization treatment step, phosphatization is handled with one or more arbitrary proportions in phosphoric acid, phosphate or the organophosphor and is mixed, content is weight percentage 1%～20%, processing time 1min～10min, 20 ℃～70 ℃ of treatment temperatures.
3, aluminum electrolysis capacitor anode foil manufacturing method according to claim 1 and 2 is characterized in that: used phosphate was ammonium dihydrogen phosphate during phosphatization was handled.
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| CNA2008100298015A CN101425389A (en) | 2008-07-29 | 2008-07-29 | Aluminum electrolysis capacitor anode foil manufacturing method |
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| CNA2008100298015A CN101425389A (en) | 2008-07-29 | 2008-07-29 | Aluminum electrolysis capacitor anode foil manufacturing method |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN102021627A (en) * | 2010-11-10 | 2011-04-20 | 广西贺州市桂东电子科技有限责任公司 | Depolarization method in foiling process of electronic aluminum foil |
| CN102426923A (en) * | 2011-08-18 | 2012-04-25 | 青海金阳光电子材料股份有限公司 | Manufacturing method of electrode foil used in high pressure on plateau |
| US8784637B2 (en) | 2009-06-18 | 2014-07-22 | Panasonic Corporation | Method for manufacturing anode foil of aluminium electrolytic capacitor |
| CN105742067A (en) * | 2015-12-08 | 2016-07-06 | 恒扬（韶关）工业有限公司 | Aluminum foil production method capable of improving capacitance extraction rate of solid-state capacitor and decreasing leakage current of solid-state capacitor |
| CN108505095A (en) * | 2018-04-04 | 2018-09-07 | 南通海星电子股份有限公司 | A kind of formation processing method of high intensity medium-high pressure chemical foil |
| JP2021027120A (en) * | 2019-08-02 | 2021-02-22 | ニチコン株式会社 | Method for manufacturing electrode foil for aluminum electrolytic capacitor |
-
2008
- 2008-07-29 CN CNA2008100298015A patent/CN101425389A/en active Pending
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US8784637B2 (en) | 2009-06-18 | 2014-07-22 | Panasonic Corporation | Method for manufacturing anode foil of aluminium electrolytic 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 |
| CN102021627A (en) * | 2010-11-10 | 2011-04-20 | 广西贺州市桂东电子科技有限责任公司 | Depolarization method in foiling process of electronic aluminum foil |
| CN102426923A (en) * | 2011-08-18 | 2012-04-25 | 青海金阳光电子材料股份有限公司 | Manufacturing method of electrode foil used in high pressure on plateau |
| CN105742067A (en) * | 2015-12-08 | 2016-07-06 | 恒扬（韶关）工业有限公司 | Aluminum foil production method capable of improving capacitance extraction rate of solid-state capacitor and decreasing leakage current of solid-state capacitor |
| CN108505095A (en) * | 2018-04-04 | 2018-09-07 | 南通海星电子股份有限公司 | A kind of formation processing method of high intensity medium-high pressure chemical foil |
| JP2021027120A (en) * | 2019-08-02 | 2021-02-22 | ニチコン株式会社 | Method for manufacturing electrode foil for aluminum electrolytic capacitor |
| JP7227870B2 (en) | 2019-08-02 | 2023-02-22 | ニチコン株式会社 | Manufacturing method of electrode foil for aluminum electrolytic capacitor |
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Open date: 20090506 |