CN101030487A - Production of electrolytic capacitor anode aluminum foil - Google Patents
Production of electrolytic capacitor anode aluminum foil Download PDFInfo
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- CN101030487A CN101030487A CN 200610124352 CN200610124352A CN101030487A CN 101030487 A CN101030487 A CN 101030487A CN 200610124352 CN200610124352 CN 200610124352 CN 200610124352 A CN200610124352 A CN 200610124352A CN 101030487 A CN101030487 A CN 101030487A
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Abstract
The invention is concerned with the manufacture method for the anodic foil of the electrolytic capacitor, which is the manufacture method by using motor, it is: cleans the corrosive foil with pure water - oxalic acid forming - cleans with hot water - conducts forming in four stages - heat treatment - re-forming - treats with the phosphoric acid - re-forming - heat treatment - re-forming - drying. The advantages of the invention are low wastage, better flexibility, shorter voltage boosting, and better hydration proof.
Description
Technical field
The invention belongs to the manufacture method of electrolytic capacitor anode aluminum foil.
Background technology
The preparation method of the anode foils of conventional aluminium electrolytic capacitor generally comprises boiling pure water, changes into, heat treatment, depolarising, phosphoric acid handles, changes into processing.Changing into processing generally is to boil a period of time earlier in high temperature (greater than 95 ℃) pure water, allow etched foil generate one deck hydrated film earlier, inorganic acid (as boric acid, phosphoric acid) or organic acid (as adipic acid) at high temperature (greater than 85 ℃) carry out anodic oxidation, so that can allow the hydrated film on surface of etched foil produce the anode of the good crystalline aluminum oxide of one deck compact structure, insulation property as capacitor.The specific volume of the anode oxide film that obtains like this is higher, deviation is apparent in view, loss is also bigger, loss changes between 0.025～0.05% under the different specific volumes, pressure rising time is long simultaneously, water resistance is more difficult to get control, and these are not enough to make the anode foils of producing thus be difficult to satisfy the needs of alternating current motor with capacitor.Alternating current motor since when starting electric current bigger, if loss is big, heating is relatively more severe, can cause capacitor to damage; If the water-fast performance of closing of anode foils is bad in addition, under the temperature condition with higher, the generation hydrogen that can react with the water in the electrolyte of the aluminium in the anode makes capacitor play drum, so that the danger of blasting, and causes unnecessary loss.
Summary of the invention
The manufacture method that the purpose of this invention is to provide a kind of electrolytic capacitor anode aluminum foil.
The manufacture method of anode aluminum foil of electrolytic capacitor of the present invention, its technical solution is: the special corrosion of learning from else's experience, purity is that 99.99% etched foil cleans, in oxalic acid solution, change into, solution concentration is 20～80g/L, changing into temperature is 10-30 ℃, and forming current density is 10～40mA.cm
-2, the time of changing into is 20～60 minutes, then the pure water with heat cleans paillon foil, so that remove the foreign ions such as oxalate in the etched foil cavity; Carry out level Four respectively and change in boric acid 10～60g/L and a certain amount of borax soln, changing into temperature is 40～80 ℃, and forming current density is 10～30mA.cm
-2, when arriving setting voltage constant 6～30 minutes, (200～590Vf) required also differently the voltage of the anode foils of different size, and the voltage distribution of this level Four is 30%, 60%, 90%, 100%.After take out cleaning, in temperature is under 450～520 ℃, heat treatment 1～3 minute, in above-mentioned electrolyte, mend and form 3～10 minutes, in being the phosphoric acid solution of 2～8% (volume ratios), concentration handled 4～10 minutes then, 45～85 ℃ of the temperature of solution, then in above-mentioned electrolyte, form 5～10 minutes again, be under 450～520 ℃ and then in temperature, heat treatment 1～3 minute is carried out last benefit equally and is formed 5～10 minutes, at last 100 ℃ of oven dry in above-mentioned electrolyte, it is low that the anode foils of Sheng Chaning has loss like this, bending is good, pressure rising time is short, the water-fast good characteristics of performance of closing are suitable for the anode of the electrolytic capacitor of special purpose.
The present invention compared with prior art has following advantage and effect:
1. adopt earlier oxalic acid low temperature to change into, carry out boiling pure water when being different from conventional anode foils and changing into earlier;
2. ensuing changing into adopts low temperature to change into, and temperature must be greater than 85 ℃ when being different from conventional anode foils and changing into;
3. the temperature of phosphoric acid treatment fluid and concentration are higher, and the electrical property of oxide-film is had positive effect.
4. the product anode foils has that loss is low, bending good, pressure rising time is short, the water-fast good characteristics of performance of closing.
Concrete execution mode:
Below in conjunction with embodiment technical scheme of the present invention is described in further detail, but embodiments of the present invention are not limited thereto.
Embodiment 1
Etched foil is 20mA.cm with the current density in the 20g/L oxalic acid solution at room temperature
-2Change into, the time is 30min, and solution temperature is controlled at about 30 ℃; Taking-up is cleaned with hot water, in the aqueous solution of the boric acid of 20g/L and 10g/L borax, at 45 ℃, current density 20mA.cm
-2, voltage is to carry out the first order under the 100V condition to change into, constant voltage time is 8 minutes; Carry out the second level with identical condition and change in same electrolyte, voltage rises to 200V, constant voltage 8 minutes; Carry out the third level with identical condition and change in same electrolyte, voltage rises to 280V, constant voltage 12 minutes; Carry out the fourth stage with identical condition and change in same electrolyte, voltage rises to 335V, constant voltage 24 minutes; Then paillon foil was heat-treated under 460 ℃ 1.5 minutes, in above-mentioned electrolyte with 335V constant voltage 8 minutes, then carry out 55 ℃, the processing of 5% phosphoric acid, time is 4 minutes, again in above-mentioned electrolyte with 335V constant voltage 8 minutes, back paillon foil was heat-treated under 460 ℃ 1.5 minutes, in the last above-mentioned electrolyte with 335V constant voltage 8 minutes, take out oven dry at last, measure the relevant parameter (current density that changes in the above-mentioned BAS is all the same) that changes into paper tinsel, see Table 1.
Table 1 335Vf changes into the relevant parameter of paper tinsel when changing into
| Pressure rising time (s) | Leakage current (uA) | Loss (%) | Tr60(s) | Bending (returning) |
| 76 | 29 | 1.40 | 1 | 186 |
Embodiment 2
Etched foil is 25mA.cm with the current density in the 50g/L oxalic acid solution at room temperature
-2Change into, the time is 24min, and solution temperature is controlled at about 25 ℃; Taking-up is cleaned with hot water, in the aqueous solution of the boric acid of 40g/L and 10g/L borax, at 55 ℃, current density 20mA.cm
-2, voltage is to carry out the first order under the 140V condition to change into, constant voltage time is 8 minutes; Change into identical condition in same electrolyte, voltage rises to 280V, constant voltage 8 minutes; Carry out the third level and change in the aqueous solution of the boric acid of 40g/L and 5g/L borax, voltage rises to 420V, constant voltage 12 minutes; Carry out the fourth stage and change in the aqueous solution of the boric acid of 40g/L and 3g/L borax, voltage rises to 470V, constant voltage 24 minutes; Then paillon foil was heat-treated under 500 ℃ 2.0 minutes, in above-mentioned fourth stage electrolyte with 470V constant voltage 8 minutes, then carry out 75 ℃, the processing of 4% phosphoric acid, time is 8 minutes, again in above-mentioned fourth stage electrolyte with 470V constant voltage 8 minutes, back paillon foil was heat-treated under 500 ℃ 2.0 minutes, in the last above-mentioned fourth stage electrolyte with 470V constant voltage 8 minutes, take out oven dry at last, measure the relevant parameter (current density that changes in the above-mentioned BAS is all the same) that changes into paper tinsel, see Table 2.
Table 2 470Vf changes into the relevant parameter of paper tinsel when changing into
| Pressure rising time (s) | Leakage current (uA) | Loss (%) | Tr60(s) | Bending (returning) |
| 100 | 36 | 1.20 | 3 | 198 |
Embodiment 3
Etched foil is 10mA.cm with the current density in the 60g/L oxalic acid solution at room temperature
-2Change into, the time is 60min, and solution temperature is controlled at about 25 ℃; Taking-up is cleaned with hot water, carries out the first order and change in the aqueous solution of the boric acid of 50g/L and 10g/L borax, at 65 ℃, current density 20mA.cm
-2, voltage is to carry out under the 150V condition, constant voltage time is 8 minutes; Carry out the second level and change in the aqueous solution of the boric acid of 50g/L and 6g/L borax, voltage rises to 300V, constant voltage 8 minutes; Carry out the third level and change in the aqueous solution of the boric acid of 50g/L and 2.5g/L borax, voltage rises to 470V, constant voltage 14 minutes; Carry out the fourth stage and change in the aqueous solution of the boric acid of 50g/L and 1.0g/L borax, voltage rises to 520V, constant voltage 28 minutes; Then paillon foil was heat-treated under 460 ℃ 1.5 minutes, in above-mentioned fourth stage electrolyte with 520V constant voltage 8 minutes, then carry out 85 ℃, the processing of 4% phosphoric acid, time is 6 minutes, again in above-mentioned fourth stage electrolyte with 520V constant voltage 8 minutes, back paillon foil was heat-treated under 500 ℃ 1.5 minutes, in the last above-mentioned fourth stage electrolyte with 520V constant voltage 8 minutes, take out oven dry at last, measure the relevant parameter (current density that changes in the above-mentioned BAS is all the same) that changes into paper tinsel, see Table 3.
Table 3 520Vf changes into the relevant parameter of paper tinsel when changing into
| Pressure rising time (s) | Leakage current (uA) | Loss (%) | Tr60(s) | Bending (returning) |
| 110 | 39 | 1.25 | 3 | 200 |
Embodiment 4
Etched foil is 15mA.cm with the current density in the 80g/L oxalic acid solution at room temperature
-2Change into, the time is 28min, and solution temperature is controlled at about 30 ℃; Taking-up is cleaned with hot water, carries out the first order and change in the aqueous solution of the boric acid of 60g/L and 10g/L borax, at 80 ℃, current density 20mA.cm
-2, voltage is to carry out under the 230V condition, constant voltage time is 10 minutes; Carry out the second level and change in the aqueous solution of the boric acid of 50g/L and 3.5g/L borax, voltage rises to 450V, constant voltage 10 minutes; Change into the third level in the aqueous solution of the boric acid of 50g/L and 1.0g/L borax, voltage rises to 530V, constant voltage 15 minutes; Change into the fourth stage in the aqueous solution of the boric acid of 50g/L and 0.5g/L borax, voltage rises to 570V, constant voltage 30 minutes; Then paillon foil was heat-treated under 490 ℃ 2.5 minutes, in above-mentioned fourth stage electrolyte with 570V constant voltage 10 minutes, then carry out 65 ℃, the processing of 6% phosphoric acid, time is 8 minutes, again in above-mentioned fourth stage electrolyte with 570V constant voltage 8 minutes, back paillon foil was heat-treated under 500 ℃ 2.5 minutes, in the last above-mentioned fourth stage electrolyte with 570V constant voltage 8 minutes, take out oven dry at last, measure the relevant parameter (current density that changes in the above-mentioned BAS is all the same) that changes into paper tinsel, see Table 4.
Table 4 570Vf changes into the relevant parameter of paper tinsel when changing into
| Pressure rising time (s) | Leakage current (uA) | Loss (%) | Tr60(s) | Bending (returning) |
| 116 | 90 | 1.20 | 4 | 175 |
Claims (6)
1. the manufacture method of an electrolytic capacitor anode aluminum foil, it is characterized in that: etched foil is cleaned, in oxalic acid aqueous solution, change into, after carry out hot water and clean, then in the aqueous solution of boric acid and borax, under different voltage sections, carry out level Four and change into, wait to reach to reduce phlegm and internal heat behind the predetermined voltage and handle and the phosphoric acid processing, change into again, take out oven dry at last.
2. the manufacture method of electrolytic capacitor anode aluminum foil according to claim 1, it is characterized in that: the condition that oxalic acid changes into is: solution concentration is 20～80g/L, and changing into liquid temp is 10-30 ℃, and forming current density is 10～40mA.cm
-2, the time of changing into is 20～60 minutes.
3. according to the manufacture method of the electrolytic capacitor anode aluminum foil described in the claim 1, it is characterized in that: when boric acid and borax change into: solution consist of boric acid 10～60g/L, the concentration of borax is different according to different formation voltages, be 1～10g/L, changing into liquid temp is 40～80 ℃, and forming current density is 10～30mA.cm
-2, the time of changing into is 6～30 minutes.
4. according to the manufacture method of the electrolytic capacitor anode aluminum foil described in the claim 1, it is characterized in that: heat treatment temperature is 450～520 ℃, and the time is 1～3 minute.
5. according to the manufacture method of the electrolytic capacitor anode aluminum foil described in the claim 1, it is characterized in that: 35～85 ℃ of the temperature that phosphoric acid is handled, the time is 4～10 minutes, concentration is 2～8% (volume ratios).
6. according to the manufacture method of the electrolytic capacitor anode aluminum foil described in the claim 1, it is characterized in that: the formation voltage scope that is suitable for is 200～590Vf.
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| CN100587871C (en) * | 2008-02-22 | 2010-02-03 | 乳源瑶族自治县东阳光化成箔有限公司 | Production method of low pressure formed foil |
| CN101235529B (en) * | 2007-11-05 | 2010-04-07 | 乳源瑶族自治县东阳光化成箔有限公司 | Method for manufacturing low-pressure chemical synthesis foil for aluminum electrolysis capacitor and middle treatment groove |
| CN101425388B (en) * | 2008-07-29 | 2011-03-09 | 东莞市东阳光电容器有限公司 | Production method for anode foil used for high-voltage electrolysis capacitor |
| WO2012088700A1 (en) * | 2010-12-30 | 2012-07-05 | 新疆众和股份有限公司 | Manufacturing method for anode foil of aluminum electrolytic capacitor |
| CN102610390A (en) * | 2011-01-20 | 2012-07-25 | 严民 | Method for forming ultrahigh-voltage anode foil for aluminum electrolytic capacitors |
| CN102683047A (en) * | 2012-05-14 | 2012-09-19 | 肇庆绿宝石电子有限公司 | Preparation method of solid electrolyte aluminum electrolytic capacitor |
| CN102891012A (en) * | 2012-09-14 | 2013-01-23 | 朱健雄 | Method for manufacturing amorphous oxidation film aluminum foil |
| CN103227052A (en) * | 2013-01-09 | 2013-07-31 | 朱健雄 | Method for manufacturing medium-high voltage aluminum electrolytic capacitor |
| CN103280328A (en) * | 2013-05-16 | 2013-09-04 | 陶荣燕 | Manufacturing method for anode foil of electrolytic capacitor |
| CN103366964A (en) * | 2013-06-04 | 2013-10-23 | 广西苍梧华锋电子铝箔有限公司 | Low-voltage formation aluminum foil manufacturing method suitable for high-frequency low-impedance electrolytic condenser aqueous electrolyte |
| CN103779098A (en) * | 2014-01-06 | 2014-05-07 | 广西贺州市桂东电子科技有限责任公司 | Formation method of energy storage material applied to alternating current motor start capacitor |
| CN103774197A (en) * | 2014-01-06 | 2014-05-07 | 广西贺州市桂东电子科技有限责任公司 | Medium and high-pressure etched foil post-treatment method |
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| CN101235529B (en) * | 2007-11-05 | 2010-04-07 | 乳源瑶族自治县东阳光化成箔有限公司 | Method for manufacturing low-pressure chemical synthesis foil for aluminum electrolysis capacitor and middle treatment groove |
| CN100587871C (en) * | 2008-02-22 | 2010-02-03 | 乳源瑶族自治县东阳光化成箔有限公司 | Production method of low pressure formed foil |
| CN101425388B (en) * | 2008-07-29 | 2011-03-09 | 东莞市东阳光电容器有限公司 | Production method for anode foil used for high-voltage electrolysis capacitor |
| CN103354941A (en) * | 2010-12-30 | 2013-10-16 | 新疆众和股份有限公司 | Manufacturing method for anode foil of aluminum electrolytic capacitor |
| WO2012088700A1 (en) * | 2010-12-30 | 2012-07-05 | 新疆众和股份有限公司 | Manufacturing method for anode foil of aluminum electrolytic capacitor |
| CN103354941B (en) * | 2010-12-30 | 2016-09-28 | 新疆众和股份有限公司 | The preparation method of anode foil for aluminum electrolytic capacitor |
| CN102610390A (en) * | 2011-01-20 | 2012-07-25 | 严民 | Method for forming ultrahigh-voltage anode foil for aluminum electrolytic capacitors |
| CN102610390B (en) * | 2011-01-20 | 2014-02-19 | 严民 | Method for forming ultrahigh-voltage anode foil for aluminum electrolytic capacitors |
| CN102683047A (en) * | 2012-05-14 | 2012-09-19 | 肇庆绿宝石电子有限公司 | Preparation method of solid electrolyte aluminum electrolytic capacitor |
| CN102891012A (en) * | 2012-09-14 | 2013-01-23 | 朱健雄 | Method for manufacturing amorphous oxidation film aluminum foil |
| CN103227052A (en) * | 2013-01-09 | 2013-07-31 | 朱健雄 | Method for manufacturing medium-high voltage aluminum electrolytic capacitor |
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| CN103280328A (en) * | 2013-05-16 | 2013-09-04 | 陶荣燕 | Manufacturing method for anode foil of electrolytic capacitor |
| CN103280328B (en) * | 2013-05-16 | 2016-08-03 | 陶荣燕 | Electrolytic capacitor anode aluminum foil manufacture method |
| CN103366964A (en) * | 2013-06-04 | 2013-10-23 | 广西苍梧华锋电子铝箔有限公司 | Low-voltage formation aluminum foil manufacturing method suitable for high-frequency low-impedance electrolytic condenser aqueous electrolyte |
| CN103366964B (en) * | 2013-06-04 | 2015-09-30 | 广西苍梧华锋电子铝箔有限公司 | Be applicable to the manufacture method of the low pressure formed aluminum foil of low impedance at high frequency electrolytic capacitor aqueous electrolyte |
| CN103774197A (en) * | 2014-01-06 | 2014-05-07 | 广西贺州市桂东电子科技有限责任公司 | Medium and high-pressure etched foil post-treatment method |
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| CN103779098B (en) * | 2014-01-06 | 2017-02-08 | 广西贺州市桂东电子科技有限责任公司 | Formation method of energy storage material applied to alternating current motor start capacitor |
| CN104087997A (en) * | 2014-06-16 | 2014-10-08 | 北京工业大学 | Method for preparing regular small-aperture anodized aluminum template through mixed acid variable pressure two-stage oxidation |
| CN108183031A (en) * | 2018-01-03 | 2018-06-19 | 南通海星电子股份有限公司 | Mitigate the chemical synthesizing method of low-pressure chemical synthesis foil rippled edge |
| CN108183031B (en) * | 2018-01-03 | 2019-08-06 | 南通海星电子股份有限公司 | Mitigate the chemical synthesizing method of low-pressure chemical synthesis foil rippled edge |
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