CN104103428A - Manufacturing method for high-voltage high-dielectric formed foil for aluminium electrolytic capacitor - Google Patents
Manufacturing method for high-voltage high-dielectric formed foil for aluminium electrolytic capacitor Download PDFInfo
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- CN104103428A CN104103428A CN201410129903.XA CN201410129903A CN104103428A CN 104103428 A CN104103428 A CN 104103428A CN 201410129903 A CN201410129903 A CN 201410129903A CN 104103428 A CN104103428 A CN 104103428A
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Abstract
The invention relates to the technical field of an formed foil and especially relates to a manufacturing method for a high-voltage high-dielectric formed foil for an aluminium electrolytic capacitor. The method is characterized in that electroplating a high-voltage corrosion foil to form a uniform plated layer, then, carrying out formation, and carrying out high-temperature heat treatment to form a composite oxidation film; carrying out formation again; and finally, carrying out cleaning and drying to obtain the high-voltage high-dielectric formed foil. According to the method in the invention, the electroplating method is utilized to form the high-dielectric oxide plated layer on the surface of the aluminum foil; and the high-dielectric composite oxidation film is formed after the anodic oxidation and the heat treatment and the like, the dielectric constant of the composite film being 130 and the above, thereby greatly improving the electrostatic capacity of the foil; the consistency of the foil is good; and the plated layer is good in bonding. The manufacture method provided in the invention is low in manufacture cost and high in efficiency, and helps easy industrial production.
Description
Technical field
The present invention relates to Waste Acid From Hua Cheng Foil technical field, be specifically related to the manufacture method of a kind of aluminium electrolytic capacitor high pressure high-dielectric formed foil.
Background technology
Electrolytic capacitor is widely used in many industries, and along with electronic industry develops rapidly, sharply rising to the demand of aluminium electrolytic capacitor nearly decades.And electrode foil has obtained development at full speed as the crucial raw material of aluminium electrolytic capacitor manufacture, the requirement of higher technology and quality is also proposed for electrode foil manufacturing industry.The high speed development of information industry requires the further reduced volume of aluminium electrolytic capacitor, increases static capacity, and this depends primarily on the specific volume size of aluminum electric pole foil.
The capacity of aluminium electrolytic capacitor: C=ε
0ε
rs/d can find out from formula, improve anode foils specific volume, and the technological approaches of solution has: 1, expand anode foils surface area S, mainly depend on anodization electrochemical corrosion reaming process before; 2, improve electrolytical relative dielectric constant ε
r; 3, the thickness d that reduces dielectric layer, is determined by the character of material self.Conventional aluminium anode oxide film Al
2o
3ε
rfor 8-10, and the ε of the oxide of valve metal Ta, Ti, Nb, Zr, Hf etc.
rcompare Al
2o
3height, the ε of ferroelectric material barium titanate
rcan reach 500-6000, the ε of strontium titanates
rup to 200000, this type of valve metal oxides or ferroelectric material are compound in anode oxide film especially, form the oxide-film that high dielectric is adulterated mutually, can significantly improve the specific volume of aluminum electric pole foil, the volume of aluminium electrolytic capacitor is obviously dwindled.
Current high-k composite membrane preparation research mainly concentrates on the alloy such as evaporation, smelting method, and due to physical method ubiquity equipment complexity, the shortcoming that production cost is relatively high, is difficult to industrialization.Recently also there is the sol-gel process of employing to prepare valve metal complex oxide film, but because the aluminum electrolysis capacitor anode foil of sol-gel process processing need be through flooding-be dried several cycles repeatedly, need be through long-time dry to remove desolventizing, just can obtain good effect, process cycle is oversize, and the problem such as wettability and adhesive force of aluminium foil surface also exists simultaneously, be therefore difficult to ensure the even thickness of composite membrane, performance is consistent, stable.
Summary of the invention
The object of the invention is to customer service the deficiencies in the prior art, and provide a kind of technique simple, with low cost, efficiency is high, and is easy to the manufacture method of the aluminium electrolytic capacitor high pressure high-dielectric formed foil of large-scale production.High pressure high-dielectric formed foil static capacity prepared by this method is large, promotes 30-50% than common Waste Acid From Hua Cheng Foil, and paillon foil high conformity, and deviation is little.
Technical scheme of the present invention provides the manufacture method of a kind of aluminium electrolytic capacitor high pressure high-dielectric formed foil: first the logical direct current electrolysis in plating bath of high pressure etched foil is formed to homogeneous coating, then put into the perfectly straight stream electrification of electrolyte and become, high-temperature heat treatment forms complex oxide film; Again put into the perfectly straight stream of electrolyte electrification and become, then use the aqueous solution soaking processing of ammonium phosphate salt, final drying and get final product.
The manufacture method that technique scheme of the present invention provides, comprises following steps:
1) high pressure etched foil is put into plating bath, negative pole is connected with paillon foil, and logical direct current electrolysis, then cleans with pure water;
2) step 1) gained paillon foil is put into electrolyte, positive pole is connected with paillon foil, and perfectly straight stream electrification becomes, and then cleans and high-temperature heat treatment with pure water;
3) by step 2) gained paillon foil puts into electrolyte, is anodally connected with paillon foil, and perfectly straight stream electrification becomes, and being then placed in mass fraction is the aqueous solution immersion treatment of 1-2% ammonium phosphate salt, finally cleans rear being dried with pure water.
In some embodiments, plating bath described in step 1) is that mass fraction is the aqueous solution of 0.01-0.1% titanium tetrachloride and 0.001-0.1% fatty alcohol sulfate salt or the acetone soln of 3-10% butyl titanate and 0.001-0.1% alkylaryl phenolic ether sulfuric acid.
In some embodiments, step 1) plating condition is: groove temperature 10-40 DEG C, current density is 0.1-1mA/cm
2, conduction time 20-40 minute.
In some embodiments, step 2) with step 3) described in electrolyte be that mass fraction is 5-10% boric acid and the 0.001-1% organic acid aqueous solution or 5-10% boric acid aqueous solution.
In some embodiments, organic acid is selected from citric acid, tartaric acid, adipic acid or azelaic acid.
In some embodiments, step 2) condition of changing into is: groove temperature 70-90 DEG C, voltage 400-650V, electric current 4A, current density 0.1-10mA/cm
2, conduction time 20-40 minute.
In some embodiments, step 2) in high-temperature heat treatment temperature be 500-550 DEG C, time 4-6 minute.
In some embodiments, step 3) changes into condition and is: groove temperature 70-90 DEG C, voltage 400-650V, electric current 4A, current density 0.1-10mA/cm
2, conduction time 5-10 minute.
In some embodiments, described ammonium phosphate salt is selected from ammonium phosphate, ammonium dihydrogen phosphate or diammonium hydrogen phosphate.In some embodiments, the treatment trough temperature of the aqueous solution of step 3) ammonium phosphate salt is 50-60 DEG C, and drying condition temperature is 100-150 DEG C.
Definition of the present invention " aqueous solution of ammonium phosphate salt " comprises ammonium phosphate solution, ammonium dibasic phosphate aqueous solution, ammonium dihydrogen phosphate aqueous solution or their combination, and the mixed solution of ammoniacal liquor and phosphoric acid.
Definition of the present invention " high temperature " refers to the temperature that is not less than 500 DEG C.
The definition "or" that the present invention uses represents alternative, if suitable, they can be combined, and that is to say, term "or" comprises each listed independent alternative and their combination.For example, " organic acid is selected from citric acid, tartaric acid, adipic acid or azelaic acid " represents that described organic acid can be the one among citric acid, tartaric acid, adipic acid, azelaic acid, can be also its more than one combination.
Unless clearly state in contrast, otherwise all scopes that the present invention quotes comprised end value.For example, " 20-40 minute conduction time " represents that the scope of T conduction time is 20min≤T≤40min.
Manufacture method provided by the invention comprises preparation plating bath, logical direct current plating, drying and processing, perfectly straight stream electrification and becomes to be processed into Waste Acid From Hua Cheng Foil, heating and generate the steps such as composite high-dielectric oxide-film, logical direct current change into again.By above-mentioned steps, can make adhesive force, the high conformity of the composite membrane making, the dielectric constant of the more common aluminium oxide of dielectric constant improves 3-5 doubly, and static capacity improves 30-50%, and this manufacturing approach craft is simple simultaneously, cost is low, efficiency is high.
Embodiment
The following stated be the preferred embodiment of the present invention, what the present invention protected is not limited to following preferred implementation.It should be pointed out that on the basis of conceiving in these innovation and creation for a person skilled in the art, some distortion and the improvement made, all belong to protection scope of the present invention.
Embodiment 1
High pressure etched foil is put into the aqueous solution of 0.1% titanium tetrachloride and 0.05% fatty alcohol sulfate salt, negative pole is connected with paillon foil, and 20 DEG C of groove temperature adopt galvanostatic method to electroplate, and setting current density is 1mA/cm
2, 30 minutes conduction time; Then take out etched foil, use pure water clean surface; Paillon foil after cleaning is put into 5% boric acid aqueous solution, and positive pole is connected with paillon foil, 80 DEG C of groove temperature, voltage 580V, electric current 4A, current density 1mA/cm
2, 30 minutes conduction time; Then take out paillon foil, clean with pure water, insert temperature and be in the Muffle furnace of 500 DEG C, constant temperature took out after 5 minutes, naturally cooling; Cooling rear paillon foil is put into 5% boric acid aqueous solution, and positive pole is connected with paillon foil, 80 DEG C of groove temperature, voltage 580V, electric current 4A, current density 1mA/cm
2, 10 minutes conduction time; Then take out paillon foil, being placed in mass fraction is 50 DEG C of immersion treatment of 2% ammonium dihydrogen phosphate aqueous solution, finally cleans latter 100 DEG C with pure water and is dried.
Embodiment 2
High pressure etched foil is put into the aqueous solution of 0.05% titanium tetrachloride and 0.005% fatty alcohol sulfate salt, negative pole is connected with paillon foil, and 40 DEG C of groove temperature adopt galvanostatic method to electroplate, and setting current density is 0.5mA/cm
2, 40 minutes conduction time; Then take out etched foil, use pure water clean surface; Paillon foil after cleaning is put into 10% boric acid and 0.1% lemon aqueous acid, and positive pole is connected with paillon foil, groove temperature 70 C, voltage 650V, electric current 4A, current density 5mA/cm
2, 20 minutes conduction time; Then take out paillon foil, clean with pure water, insert temperature and be in the Muffle furnace of 550 DEG C, constant temperature took out after 4 minutes, naturally cooling; Cooling rear paillon foil is put into 10% boric acid and 0.1% lemon aqueous acid, and positive pole is connected with paillon foil, groove temperature 70 C, voltage 650V, electric current 4A, current density 5mA/cm
2, 5 minutes conduction time; Then take out paillon foil, being placed in mass fraction is 60 DEG C of immersion treatment of 2% ammonium dihydrogen phosphate aqueous solution, finally cleans latter 150 DEG C with pure water and is dried.
Embodiment 3
High pressure etched foil is put into the aqueous solution of 0.01% titanium tetrachloride and 0.001% fatty alcohol sulfate salt, negative pole is connected with paillon foil, and 10 DEG C of groove temperature adopt galvanostatic method to electroplate, and setting current density is 1mA/cm
2, 40 minutes conduction time; Then take out etched foil, use pure water clean surface; Paillon foil after cleaning is put into 5% boric acid and the 1% tartaric aqueous solution, and positive pole is connected with paillon foil, 90 DEG C of groove temperature, voltage 500V, electric current 4A, current density 10mA/cm
2, 20 minutes conduction time; Then take out paillon foil, clean with pure water, insert temperature and be in the Muffle furnace of 500 DEG C, constant temperature took out after 6 minutes, naturally cooling; Cooling rear paillon foil is put into 5% boric acid and the 1% tartaric aqueous solution, and positive pole is connected with paillon foil, 90 DEG C of groove temperature, voltage 500V, electric current 4A, current density 10mA/cm
2, 5 minutes conduction time; Then take out paillon foil, being placed in mass fraction is 60 DEG C of immersion treatment of 1% ammonium dibasic phosphate aqueous solution, finally cleans latter 150 DEG C with pure water and is dried.
Embodiment 4
The acetone soln of high pressure etched foil being put into 5% butyl titanate and 0.05% alkylaryl phenolic ether sulfuric acid, negative pole is connected with paillon foil, and 30 DEG C of groove temperature adopt galvanostatic method to electroplate, and setting current density is 1mA/cm
2, 30 minutes conduction time; Then take out etched foil, use pure water clean surface; Paillon foil after cleaning is put into 5% boric acid aqueous solution, and positive pole is connected with paillon foil, 80 DEG C of groove temperature, voltage 580V, electric current 4A, current density 1mA/cm
2, 30 minutes conduction time; Then take out paillon foil, clean with pure water, insert temperature and be in the Muffle furnace of 580 DEG C, constant temperature took out after 6 minutes, naturally cooling; Cooling rear paillon foil is put into 5% boric acid aqueous solution, and positive pole is connected with paillon foil, 80 DEG C of groove temperature, voltage 580V, electric current 4A, current density 1mA/cm
2, 10 minutes conduction time; Then take out paillon foil, being placed in mass fraction is 60 DEG C of immersion treatment of 5% ammonium dihydrogen phosphate aqueous solution, finally cleans latter 120 DEG C with pure water and is dried to dry.
Embodiment 5
The acetone soln of high pressure etched foil being put into 3% butyl titanate and 0.1% alkylaryl phenolic ether sulfuric acid, negative pole is connected with paillon foil, and 20 DEG C of groove temperature adopt galvanostatic method to electroplate, and setting current density is 0.1mA/cm
2, 40 minutes conduction time; Then take out etched foil, use pure water clean surface; The aqueous solution of paillon foil after cleaning being put into 5% boric acid and 0.01% azelaic acid, positive pole is connected with paillon foil, 90 DEG C of groove temperature, voltage 400V, electric current 4A, current density 0.5mA/cm
2, 40 minutes conduction time; Then take out paillon foil, clean with pure water, insert temperature and be in the Muffle furnace of 500 DEG C, constant temperature took out after 5 minutes, naturally cooling; Cooling rear paillon foil is put into the aqueous solution of 5% boric acid and 0.01% azelaic acid, positive pole is connected with paillon foil, 90 DEG C of groove temperature, voltage 400V, electric current 4A, current density 0.5mA/cm
2, 10 minutes conduction time; Then take out paillon foil, being placed in mass fraction is 60 DEG C of immersion treatment of 1% ammonium phosphate solution, finally cleans latter 110 DEG C with pure water and is dried to dry.
Embodiment 6
The acetone soln of high pressure etched foil being put into 10% butyl titanate and 0.001% alkylaryl phenolic ether sulfuric acid, negative pole is connected with paillon foil, and 20 DEG C of groove temperature adopt galvanostatic method to electroplate, and setting current density is 1mA/cm
2, 20 minutes conduction time; Then take out etched foil, use pure water clean surface; The aqueous solution of paillon foil after cleaning being put into 10% boric acid and 0.001% adipic acid, positive pole is connected with paillon foil, 80 DEG C of groove temperature, voltage 450V, electric current 4A, current density 0.1mA/cm
2, 40 minutes conduction time; Then take out paillon foil, clean with pure water, insert temperature and be in the Muffle furnace of 500 DEG C, constant temperature took out after 6 minutes, naturally cooling; Cooling rear paillon foil is put into the aqueous solution of 10% boric acid and 0.001% adipic acid, positive pole is connected with paillon foil, 80 DEG C of groove temperature, voltage 400V, electric current 4A, current density 0.1mA/cm
2, 10 minutes conduction time; Then take out paillon foil, being placed in mass fraction is 60 DEG C of immersion treatment of 2% ammonium dihydrogen phosphate aqueous solution, finally cleans latter 100 DEG C with pure water and is dried.
Comparative example
High pressure etched foil is put into 5% boric acid aqueous solution, and positive pole is connected with paillon foil, 80 DEG C of groove temperature, voltage 580V, electric current 4A, current density 1mA/cm
2, 30 minutes conduction time; Then take out paillon foil, clean with pure water, insert temperature and be in the Muffle furnace of 500 DEG C, constant temperature took out after 5 minutes, naturally cooling; Cooling rear paillon foil is put into 5% boric acid aqueous solution, and positive pole is connected with paillon foil, 80 DEG C of groove temperature, voltage 580V, electric current 4A, current density 1mA/cm
2, 10 minutes conduction time; Then take out paillon foil, being placed in mass fraction is 50 DEG C of immersion treatment of 2% ammonium dihydrogen phosphate aqueous solution, finally cleans latter 110 DEG C with pure water and is dried.
Respectively the Waste Acid From Hua Cheng Foil of above-mentioned preparation is detected, detection method is undertaken by standard, and test data the results are shown in Table 1.
The experimental test data of table 1 high dielectric high pressure Waste Acid From Hua Cheng Foil and common high pressure Waste Acid From Hua Cheng Foil
| ? | Arrive voltage | Static capacity | Loss value | Bending intensity | Water resistance | Deviation |
| Embodiment 1 | 602 | 0.895μF/cm 2 | 2.7 | 168 | 28 | 3% |
| Embodiment 2 | 652 | 0.786μF/cm 2 | 2.5 | 162 | 21 | 3% |
| Embodiment 3 | 521 | 1.125μF/cm 2 | 2.9 | 178 | 24 | 1.5% |
| Embodiment 4 | 603 | 0.942μF/cm 2 | 2.8 | 176 | 26 | 2% |
| Embodiment 5 | 418 | 1.678μF/cm 2 | 3.8 | 182 | 29 | 1% |
| Embodiment 6 | 470 | 1.437μF/cm 2 | 3.4 | 186 | 27 | 1.2% |
| Comparative example | 605 | 0.619μF/cm 2 | 2.6 | 172 | 29 | 5% |
As can be seen from Table 1, under 600V voltage, high-dielectric formed foil improves 44-52% than the static capacity of common Waste Acid From Hua Cheng Foil, and high conformity, and deviation is little.In 400-650V voltage range, can obtain high performance high-dielectric formed foil.
Claims (11)
1. the manufacture method of an aluminium electrolytic capacitor use high pressure high-dielectric formed foil, it is characterized in that, the logical direct current electrolysis in plating bath of high pressure etched foil is formed to homogeneous coating, then put into the perfectly straight stream electrification of electrolyte and become, high-temperature heat treatment forms complex oxide film; Again put into the perfectly straight stream of electrolyte electrification and become, then use the aqueous solution soaking processing of ammonium phosphate salt, final drying and get final product.
2. manufacture method according to claim 1, is characterized in that comprising following steps:
1) high pressure etched foil is put into plating bath, negative pole is connected with paillon foil, and logical direct current electrolysis, then cleans with pure water;
2) step 1) gained paillon foil is put into electrolyte, positive pole is connected with paillon foil, and perfectly straight stream electrification becomes, and then cleans and high-temperature heat treatment with pure water;
3) by step 2) gained paillon foil puts into electrolyte, is anodally connected with paillon foil, and perfectly straight stream electrification becomes, and being then placed in mass fraction is the aqueous solution immersion treatment of 1-2% ammonium phosphate salt, finally cleans rear being dried with pure water.
3. manufacture method according to claim 2, it is characterized in that, plating bath described in step 1) is that mass fraction is the aqueous solution of 0.01-0.1% titanium tetrachloride and 0.001-0.1% fatty alcohol sulfate salt or the acetone soln of 3-10% butyl titanate and 0.001-0.1% alkylaryl phenolic ether sulfuric acid.
4. manufacture method according to claim 2, is characterized in that, step 1) plating condition is: groove temperature 10-40 DEG C, current density is 0.1-1mA/cm
2, conduction time 20-40 minute.
5. manufacture method according to claim 2, is characterized in that step 2) with step 3) described in electrolyte be that mass fraction is 5-10% boric acid and 0.001-1% organic acid mixed aqueous solution or 5-10% boric acid aqueous solution.
6. manufacture method according to claim 5, is characterized in that, described organic acid is selected from citric acid, tartaric acid, adipic acid or azelaic acid.
7. manufacture method according to claim 2, is characterized in that step 2) condition of changing into is: groove temperature 70-90 DEG C, voltage 400-650V, electric current 4A, current density 0.1-10mA/cm
2, conduction time 20-40 minute.
8. manufacture method according to claim 2, is characterized in that step 2) in high-temperature heat treatment temperature be 500-550 DEG C, time 4-6 minute.
9. manufacture method according to claim 2, is characterized in that, step 3) changes into condition and is: groove temperature 70-90 DEG C, voltage 400-650V, electric current 4A, current density 0.1-10mA/cm
2, conduction time 5-10 minute.
10. manufacture method according to claim 2, is characterized in that, described ammonium phosphate salt is selected from ammonium phosphate, diammonium hydrogen phosphate or ammonium dihydrogen phosphate.
11. manufacture methods according to claim 2, is characterized in that, the aqueous solution treatment trough temperature of step 3) ammonium phosphate salt is 50-60 DEG C, and drying condition temperature is 100-150 DEG C.
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| CN201410129903.XA CN104103428B (en) | 2013-04-01 | 2014-04-01 | A kind of manufacture method of aluminium electrolutic capacitor high pressure high-dielectric formed foil |
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Cited By (4)
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| CN107354498A (en) * | 2017-07-18 | 2017-11-17 | 丰宾电子（深圳）有限公司 | A kind of manufacture method of the electrode foil for aluminum electrolytic capacitors of high pressure high power capacity |
| CN107967996A (en) * | 2017-11-15 | 2018-04-27 | 广西贺州市桂东电子科技有限责任公司 | A kind of chemical synthesizing method of mash welder capacitor anode foils |
| CN108505051A (en) * | 2018-03-28 | 2018-09-07 | 电子科技大学 | A kind of preparation method of smooth barrier type TFT anodic oxidation aluminum insulation layers |
| CN111074260A (en) * | 2019-12-30 | 2020-04-28 | 南通南平电子科技有限公司 | Efficient and intelligent formation process of capacitor guide pin |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107354498A (en) * | 2017-07-18 | 2017-11-17 | 丰宾电子（深圳）有限公司 | A kind of manufacture method of the electrode foil for aluminum electrolytic capacitors of high pressure high power capacity |
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| CN107967996A (en) * | 2017-11-15 | 2018-04-27 | 广西贺州市桂东电子科技有限责任公司 | A kind of chemical synthesizing method of mash welder capacitor anode foils |
| CN108505051A (en) * | 2018-03-28 | 2018-09-07 | 电子科技大学 | A kind of preparation method of smooth barrier type TFT anodic oxidation aluminum insulation layers |
| CN111074260A (en) * | 2019-12-30 | 2020-04-28 | 南通南平电子科技有限公司 | Efficient and intelligent formation process of capacitor guide pin |
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Address after: No. 368 East Sunshine Science Park 523871 Guangdong city of Dongguan province Changan Zhen Sha Zhen'an Road Applicant after: DONGGUAN DONGYANG GUANGKE R & D CO., LTD. Address before: No. 368 East Sunshine Science Park 523871 Guangdong city of Dongguan province Changan Zhen Sha Zhen'an Road Applicant before: Dongyang, Dongguan City Chang'an light Aluminum research and development company limited |
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