CN101246779B - Production method of medium and high pressure formed foil - Google Patents
Production method of medium and high pressure formed foil Download PDFInfo
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- CN101246779B CN101246779B CN2008100657018A CN200810065701A CN101246779B CN 101246779 B CN101246779 B CN 101246779B CN 2008100657018 A CN2008100657018 A CN 2008100657018A CN 200810065701 A CN200810065701 A CN 200810065701A CN 101246779 B CN101246779 B CN 101246779B
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Abstract
The invention relates to a preparing method of a middle-high voltage formed foil, comprising the steps that: a middle-high voltage etched foil is put in pure water with a temperature no less than 96 DEG C to hydrate; the hydrated foil is electrified three to four levels to form; the formed foil is heated; the heated foil is put into the processing liquid including phosphorus-containing inorganic acid and/or phosphorus-containing organic acid to middle processing; the middle processed foil is put into the forming liquid to first reforming, with the same forming liquid as that of the second step; the first reformed foil is reheated; the reheated foil is second reformed; and the high-middle voltage formed foil is got. The invention has the advantages that: the passivation is highly effective, the passivant can be freely selected, the control scope of the parameter of the passivation is large, the processing process is more energy-saving and time-saving, as well as more suitable for current workshop scale production.
Description
Technical field
The present invention relates to a kind of preparation method of capacitor aluminium foil, more particularly, the present invention relates to the manufacture method of a kind of electrolytic capacitor with the mesohigh anode foils.
Background technology
Electrolytic capacitor is widely used in many relevant industries such as electronics.Now, scientific and technological progress and industrial expansion propose higher requirement to electrolytic capacitor in power frequency, Low ESR, long-life etc.In order to reach the higher electric property of electrolytic capacitor, in capacitor, often need to adopt the electrolyte of high moisture content, but, at high temperature, aluminum foil oxidation film is meeting of anode foils oxide-film and moisture generation aquation especially, thereby generate aluminium hydroxide on the anode foils surface, cause the decline of anode foils proof voltage, leakage current to increase, even can in capacitor, produce hydrogen, press liter in causing, shell drum shell and even quick-fried shell occur, have influence on electric property, the working life of electrolytic capacitor and even whole electric system, in addition safe in utilization.
For addressing the above problem, industry has extensively taked the passivation measure to prevent aluminum foil oxidation film and moisture generation aquation at present.Generally speaking, different with inhibition, the degree of passivation of water reaction to aluminium according to anion, general material can be divided into four classes promptly: unrestraint effect class, medium inhibitory action class, strong inhibitory action class and extremely strong inhibitory action class.And wherein, the aluminum orthophoshpate of generation is water insoluble, and the aluminum orthophoshpate structure on aluminum foil oxidation film surface is identical with the low quartz crystal formation, is stable positive tetrahedron crystalline texture, so phosphate radical belongs to the passivator of extremely strong inhibitory action class; The aluminum phosphate film has suppressed the effect of hydrated aluminum, having improved change into paper tinsel water-fast on apparent closes performance (its test mechanism shows as and surveys under the poach condition of back and directly under the poach condition, the time that extra electric field is set up voltage on fine and close aluminum phosphate film two sides is that pressure rising time is shorter), the pot-life that changes into paper tinsel and the working life of capacitor have been prolonged, in order to make the working life that improves capacitor, the mesohigh anode foils of high request adopts level Four to change into usually, and the general mesohigh anode foils that requires can adopt three grades to change into.
For this reason, industry normally adds a certain amount of Phos acids passivator such as phosphoric acid in the particular procedure tank liquor of chemical synthesis technology process at present, phosphorous acid, ortho phosphorous acid and its esters, or add a certain amount of organic phosphine acids passivator such as amino trimethylene methyl tri methylene phosphonic acid (ATMP), even carboxylic acid waits and carries out Passivation Treatment: promptly changing into after paper tinsel arrives maximum and become voltage (being commonly called as the seal making alive), etched foil inserted in the tank liquor that contains passivator soak certain hour, in the Passivation Treatment process, phosphoric acid or other acid groups have dissolved a part of pellumina, and the acid group on the passivator generates crystallization phosphating coat or alkyl reticular membrane on the pellumina surface.These film forming matters can make alumite that the aquation sensitivity is reduced, thereby the passivation of playing has improved the anti-hydrability that changes into paper tinsel and capacitor product thereof.
But existing Passivation Treatment has very important defective when enhancing product performance.At first, though it is straight hole shape hole that high pressure changes into the hole of paper tinsel, but the oxide-film that its surface generates still has certain thickness, passivator acid group or be difficult to fully diffuse into hole inside or when Passivation Treatment in conjunction with insecure, thus cause Passivation Treatment to be difficult to cover completely or destroyed easily comprehensively; And because Passivation Treatment efficient is lower, effect often improves concentration and temperature in order to reach preferably, and the static capacity of so easy loss part can not get both static capacity and anti-hydrability.
For addressing the above problem, it is that 200610063522.1 Chinese patent application discloses a kind of treatment process and method of inspection that suppresses aluminum foil for electrolytic condenser oxide-film and water reaction that application number is arranged, it is on existing aluminum foil for electrolytic condenser production technology (corrosion-cleaning one changes into) basis, increase the Passivation Treatment on aluminum foil oxidation film surface, its technology is: aluminium foil is after corrosion and clean technology, aluminium foil is flooded in containing the aqueous solution of phosphonium ion, clean and heat treatment through pure water again.But, the heat treatment of this technology is that 200 ℃-500 ℃ following processing times are 1h～3h in temperature, and the practical experience prompting: this heat treated burning sheet processing time is oversize, one comes the easy embrittlement of paillon foil, disconnected paper tinsel, or the paillon foil melting phenomenon takes place easily, unfavorable paillon foil oxide-film overall performance promotes, and the 2nd, heat treatment 1～3h power consumption, consuming time all too many.Obviously, this technical disadvantages is obvious, especially is difficult to realize large-scale production under existing workshop appliance, condition.
Also having application number is the manufacture method that 200610039699.8 Chinese patent application discloses a kind of electrode foil for aluminum electrolytic capacitors, press during it is got in the pure water of corrosive aluminum foil more than 95 degree reach and carry out hydration, after the hydration, soak in 40-80 0.1～5% ℃ the phosphoric acid solution, then carrying out secondary in the aqueous solution of 60～90 ℃ of the boric acid of the ammonium adipate of 0.5-3% and 3-10% changes into, after changing into for the first time, constant voltage 20-30 minute, and the high-temperature process by 350-500 ℃, after changing into for the second time, constant voltage 10～15 minutes.Between the Passivation Treatment that this technology is soaked phosphoric acid solution is arranged in hydration-treated and changes into, it is said that the electrode foil after the Passivation Treatment can improve specific volume 4-10%.But, the practical experience prompting: the water-repellent film performance of handling the paillon foil that obtains like this is not good, particularly along with formation voltage increases, serious curling can appear in paillon foil, and change into all variation of rear oxidation film electrical property and resistance to water, in a word, this technology does not possess practicality to the paillon foil that formation voltage surpasses 400V, is difficult to implement scale production under existing industry workshop appliance, condition yet.
Application number is 03139816.2 Chinese patent aluminum electrolysis capacitor anode foil manufacturing method in addition, comprise boiling pure water, change into, depolarising and change into processing again, change into electrolyte and comprise boronic acid containing or this type of inorganic acid of phosphoric acid or this type of organic acid of adipic acid, or the wherein at least a aqueous solution of their salt, in changing into electrolyte, the hypophosphorous acid, phosphorous acid, ortho phosphorous acid or its esters that add content and be 50ppm-5000ppm be as active material, and the citric acid, tartaric acid or its esters that add content and be 100ppm-10000ppm are as complexing agent.It is said: this method can resist the dissolving of paillon foil, helps reducing the decay of capacitance, thereby can make that capacitance is big, leakage current is less, resistance to water anode foil for aluminum electrolytic capacitor preferably.
Summary of the invention
Above-mentioned shortcoming at prior art; the objective of the invention is to provide a kind of mesohigh to change into the manufacture method of paper tinsel; this invention technical scheme has following advantage: Passivation Treatment efficient is higher; and passivator is selected, and the degree of freedom is big, the parameter control range elasticity of Passivation Treatment is big; processing procedure is more energy-conservation, save time, and is adapted to the workshop large-scale production of existing industry more.
For this reason, technical solution of the present invention is the manufacture method that a kind of mesohigh changes into paper tinsel, and it comprises the steps: A) mesohigh is corroded the pure water that paillon foil places temperature to be greater than or equal to 96 ℃ carry out hydration-treated; B) paillon foil after the hydration-treated being carried out three changes into to powering up of level Four; C) will heat-treat through the described paillon foil that changes into; D) will place treatment fluid to carry out processing through heat treated paillon foil, treatment fluid comprises that the containing parameter scope carries out elasticity control, therefore, is adapted to the large-scale production in existing industry workshop more.
Because the inventive method is improved and above-mentioned microcosmic mechanism advantage, even the inventive method changes into for the aluminium foil of the highest withstand voltage aluminium dielectric capacitor, also can accomplish only to adopt the tertiary voltage distribution and needn't adopt the level Four voltage distribution, thereby saved the cost of energy consumption and production operation, the conventional art of comparing, the Passivation Treatment process of the inventive method can also be saved once and changes into except heat treatment time is shortened, thus also save time more, energy-conservation, efficient.
The manufacture method that mesohigh of the present invention changes into paper tinsel also further comprises following concrete improvement:
For obtaining better resultant effect, in the described steps A, described hydration-treated temperature more than 98 ℃, 6～15 minutes processing times.
Among the described step B, the described liquid that changes into is for containing the aqueous solution of 2～10 (wt%) boric acid and ammonium borate or boric acid and Boratex.
The described temperature that changes into liquid is 75～90 ℃, changes into to reach behind the ceiling voltage constant 10～30 minutes.
For guaranteeing passivation effect and excellent electrical and simplify the operation, described the 1st, 2 change into again change into the liquid proportioning, change into liquid temp, formation voltage is same as that afterbody changes among the described step B.
Described heat treatment, heat treated temperature all is controlled to be 400～520 ℃ once more, and the processing time is 1～4 minute.
Because the inventive method is improved and the advantage of microcosmic mechanism guarantees, the scope of choosing for deactivation matter is expanded promptly, in described step D, described inorganic phosphor-contained acid be phosphoric acid, phosphate, phosphorous acid, phosphite, hypophosphorous acid, hypophosphites one of them, described phosphorous organic acid be phytic acid, amino trimethyl phosphonic acids (ATMP), hydroxy ethylene diphosphonic acid (HEDP) one of them.
Because the inventive method is improved and the assurance of the advantage of microcosmic mechanism, also be expanded promptly for the control range of passivation operation, in described step D, the concentration of treatment fluid is 0.1～10g/L, temperature is 30～85 ℃, 2～15 minutes processing times.
For increasing the long-term storage performance of finished product, described manufacture method also comprises carries out reprocessing and oven dry with the 2nd paillon foil that changes into again.The ammonium dihydrogen phosphate of 2-6wt%, temperature 40-55 ℃, processing time 2-7 minute are adopted in described reprocessing; Described bake out temperature is 100～150 ℃ of scopes, and drying time is 2～7 minutes.
The present invention will be further described below in conjunction with specific embodiment.
Comparative example:
Adopt as etched foil same among the embodiment, poach is 12 minutes in the pure water more than 98 ℃, carries out the first order under 85 ℃ and change in the mixed solution of 5.0wt% boric acid, 1.0wt% ammonium borate (or sodium) aqueous solution, and constant voltage was 8 minutes when voltage arrived 200V; Then carry out the second level under 85 ℃ in the mixed solution of 5wt% boric acid, 0.5wt% ammonium borate (or sodium) aqueous solution and change into, constant voltage was 10 minutes when voltage arrived 400V; Then carry out the third level under 85 ℃ in the mixed solution of 5wt% boric acid, 0.15wt% ammonium borate (or sodium) aqueous solution and change into, constant voltage was 15 minutes when voltage arrived 520V; Then carry out the fourth stage under 85 ℃ in the mixed solution of 5wt% boric acid, 0.08wt% ammonium borate (or sodium) aqueous solution and change into, constant voltage was 30 minutes when voltage arrived 580V, then heat-treated, and temperature is 520 ℃, and the time is 2.5 minutes; Change at the above-mentioned fourth stage and to carry out the 1st in the liquid and change into again; Then carry out the phosphoric acid Passivation Treatment, solution concentration is that 6% (volume ratio), 65 ℃ of temperature, time are 6 minutes, cleans up the back and changes at the above-mentioned fourth stage and carry out the 2nd in the liquid and change into; Heat-treat, temperature is 500 ℃ again, and the time is 2.5 minutes; Change at the above-mentioned fourth stage and to carry out last changing in the liquid; Relevant electrical quantity is measured in oven dry at last, and measurement result sees Table 1.
Embodiment
Embodiment one:
Adopt the mesohigh etched foil, poach is 12 minutes in the pure water more than 98 ℃, and constant voltage is 10 minutes when then carrying out first order level formation voltage arrival 250V under 85 ℃ in the mixed solution of 5wt% boric acid, 0.3wt% ammonium borate (or sodium) aqueous solution; Then carry out the second level under 85 ℃ in 5wt% boric acid, 0.15wt% ammonium borate (or sodium) aqueous solution and change into, constant voltage was 15 minutes when voltage arrived 480V; Then carry out the third level under 85 ℃ in 5wt% boric acid, 0.08wt% ammonium borate (or sodium) mixed solution and change into, constant voltage was 30 minutes when voltage arrived 580V; Then heat-treat, temperature is 480 ℃, and the time is 2.5 minutes; Middle processing is carried out in the back in temperature is 45 ℃, 5g/L phosphoric acid solution, the time is 4.5 minutes; The back changes in the liquid the above-mentioned third level and changes into; Then carry out the heat treatment second time, temperature is 480 ℃, and the time is 2.5 minutes; Change into the above-mentioned third level and to carry out the 2nd in the liquid and change into, reprocessing adopts 4wt% ammonium dihydrogen phosphate, temperature to handle for 45 ℃, and the time is 4 minutes; Relevant electrical quantity is measured in oven dry at last.
Embodiment two:
Adopt the mesohigh etched foil, poach is 10 minutes in the pure water more than 98 ℃, then carries out first order level under 85 ℃ in the mixed solution of 6wt% boric acid, 0.2wt% ammonium borate (or sodium) aqueous solution and changes into, and constant voltage was 10 minutes when voltage arrived 250V; Then carry out the second level under 90 ℃ in 5wt% boric acid, 0.15wt% ammonium borate (or sodium) aqueous solution and change into, constant voltage was 15 minutes when voltage arrived 480V; Then carry out the third level under 90 ℃ in 5wt% boric acid, 0.08wt% ammonium borate (or sodium) mixed solution and change into, constant voltage was 30 minutes when voltage arrived 580V; Then heat-treat, temperature is 500 ℃, and the time is 2 minutes; Back temperature in the 2g/L phytic acid aqueous solution is 60 ℃, and the middle processing time is 6 minutes; The back changes in the liquid the above-mentioned third level and changes into; Then carry out the heat treatment second time, temperature is 500 ℃, and the time is 2 minutes; Change into the above-mentioned third level and to carry out the 2nd in the liquid and change into again; Relevant electrical quantity is measured in oven dry at last.
Embodiment three:
Adopt the mesohigh etched foil, poach is 12 minutes in the pure water more than 98 ℃, then carries out first order level under 85 ℃ in the mixed solution of 6wt% boric acid, 0.3wt% ammonium borate (or sodium) aqueous solution and changes into, and constant voltage was 10 minutes when voltage arrived 250V; Then carry out the second level under 85 ℃ in 5wt% boric acid, 0.15wt% ammonium borate (or sodium) aqueous solution and change into, constant voltage was 15 minutes when voltage arrived 480V; Then carry out the third level under 85 ℃ in 5wt% boric acid, 0.08wt% ammonium borate (or sodium) mixed solution and change into, constant voltage was 30 minutes when voltage arrived 580V; Then heat-treat, temperature is 500 ℃, and the time is 2.5 minutes; Back temperature in 1g/L ammonium hypophosphite solution is 70 ℃, and the middle processing time is 8 minutes; The back changes in the liquid the above-mentioned third level and changes into; Then carry out the heat treatment second time, temperature is 500 ℃, and the time is 2.5 minutes; Change into the above-mentioned third level and to carry out the 2nd in the liquid and change into, reprocessing adopts 4% phosphate, temperature to handle for 45 ℃, and the time is 6 minutes; Relevant electrical quantity is measured in oven dry at last.
Embodiment four:
Adopt the mesohigh etched foil, poach is 14 minutes in the pure water more than 98 ℃, then carries out first order level under 85 ℃ in the mixed solution of 6wt% boric acid, 0.3wt% ammonium borate (or sodium) aqueous solution and changes into, and constant voltage was 10 minutes when voltage arrived 250V; Then carry out the second level under 85 ℃ in 5wt% boric acid, 0.15wt% ammonium borate (or sodium) aqueous solution and change into, constant voltage was 15 minutes when voltage arrived 480V; Then carry out the third level under 85 ℃ in 5wt% boric acid, 0.08wt% ammonium borate (or sodium) mixed solution and change into, constant voltage was 30 minutes when voltage arrived 580V; Then heat-treat, temperature is 500 ℃, and the time is 2.5 minutes; Back temperature in the ATMP of 3g/L solution is 55 ℃, and the middle processing time is 4 minutes; The back changes in the liquid the above-mentioned third level and changes into; Then carry out the heat treatment second time, temperature is 500 ℃, and the time is 2.5 minutes; Change into the above-mentioned third level and to carry out the 2nd in the liquid and change into, reprocessing adopts 3wt% ammonium dihydrogen phosphate, temperature to handle for 50 ℃, and the time is 6 minutes; Relevant electrical quantity is measured in oven dry at last.
Respectively the paper tinsel that changes into of embodiment one to four, comparative example is tested, test event comprises static capacity, pressure rising time, resistance to water (survey back poach pressure rising time), and method of testing is tested by SJ/T 11140 standards, and test result is listed in the table 1.
Table 1
| Project | Pressure rising time (s) | Static capacity | Tr60(s) | 85 ℃ of life tests of capacitor |
| Comparative example | 158 | 100.0％ | 25 | Only reach 3000h |
| Embodiment one | 146 | 101.0％ | 12 | Reach 7000h |
| Embodiment two | 147 | 100.7％ | 15 | Reach 7000h |
| Embodiment three | 153 | 101.5％ | 11 | Reach 7000h |
| Embodiment four | 154 | 101.2％ | 13 | Reach 7000h |
As seen from the above table, the present invention makes change into paper tinsel water-fastly close the respective performances that performance and static capacity etc. all are better than traditional handicraft.
Claims (10)
1. a mesohigh changes into the manufacture method of paper tinsel, and it comprises the steps: A) mesohigh is corroded the pure water that paillon foil places temperature to be greater than or equal to 96 ℃ carry out hydration-treated; B) paillon foil after the hydration-treated being carried out three changes into to powering up of level Four; C) will heat-treat through the described paillon foil that changes into; D) will place treatment fluid to carry out processing through heat treated paillon foil, treatment fluid comprises inorganic phosphor-contained acid and/or phosphorous organic acid; E) paillon foil of handling in will passing through places and changes into liquid and carry out the 1st and change into, and the constituent that changes into liquid is identical with step B's; F) will carry out heat treatment once more through the 1st paillon foil that changes into again; G) will carry out the 2nd through heat treated paillon foil once more changes into again; H) obtain the finished product that described mesohigh changes into paper tinsel.
2. mesohigh changes into the manufacture method of paper tinsel according to claim 1, it is characterized in that: in the described steps A, described hydration-treated temperature more than 98 ℃, 6～15 minutes processing times.
3. mesohigh changes into the manufacture method of paper tinsel according to claim 1, it is characterized in that: among the described step B, the described liquid that changes into is for containing the aqueous solution of 2～10 (wt%) boric acid and ammonium borate or boric acid and Boratex.
4. change into the manufacture method of paper tinsel as mesohigh as described in the claim 3, it is characterized in that: the described temperature that changes into liquid is 75～90 ℃, changes into to reach behind the ceiling voltage constant 10～30 minutes.
5. mesohigh changes into the manufacture method of paper tinsel according to claim 1, it is characterized in that: described the 1st, 2 change into again change into the liquid proportioning, change into liquid temp, formation voltage is same as that afterbody changes among the described step B.
6. mesohigh changes into the manufacture method of paper tinsel according to claim 1, it is characterized in that: described heat treatment, heat treated temperature all is controlled to be 400～520 ℃ once more, and the processing time is 1～4 minute.
7. mesohigh changes into the manufacture method of paper tinsel according to claim 1, it is characterized in that: among the described step D, described inorganic phosphor-contained acid be phosphoric acid, phosphate, phosphorous acid, phosphite, hypophosphorous acid, hypophosphites one of them, described phosphorous organic acid be phytic acid, amino trimethyl phosphonic acids (ATMP), hydroxy ethylene diphosphonic acid (HEDP) one of them.
8. mesohigh changes into the manufacture method of paper tinsel according to claim 1, and it is characterized in that: among the described step D, the concentration of treatment fluid is 0.1～10g/L, and temperature is 30～85 ℃, 2～15 minutes processing times.
9. mesohigh changes into the manufacture method of paper tinsel according to claim 1, and it is characterized in that: described manufacture method also comprises carries out reprocessing and oven dry with the 2nd paillon foil that changes into again.
10. change into the manufacture method of paper tinsel as mesohigh as described in the claim 9, it is characterized in that: the ammonium dihydrogen phosphate of 2-6wt%, temperature 40-55 ℃, processing time 2-7 minute are adopted in described reprocessing; Described bake out temperature is 100～150 ℃ of scopes, and drying time is 2～7 minutes.
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| CN2008100657018A CN101246779B (en) | 2008-02-22 | 2008-02-22 | Production method of medium and high pressure formed foil |
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| CN101246779B true CN101246779B (en) | 2010-08-18 |
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| CN102891012A (en) * | 2012-09-14 | 2013-01-23 | 朱健雄 | Method for manufacturing amorphous oxidation film aluminum foil |
| CN106252081B (en) * | 2016-08-11 | 2019-01-29 | 四川立业电子有限公司 | A kind of anodizing composite dielectric film and preparation method thereof |
| JP6933931B2 (en) * | 2017-07-28 | 2021-09-08 | 日本軽金属株式会社 | Electrodes for Aluminum Electrolytic Capacitors and Their Manufacturing Methods |
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| CN109859949B (en) * | 2018-01-26 | 2021-03-26 | 东莞东阳光科研发有限公司 | Method for reducing leakage current of medium-high voltage formed foil |
| CN108511195A (en) * | 2018-03-19 | 2018-09-07 | 南通海星电子股份有限公司 | A kind of post-processing approach improving middle-high voltage electrode foil coating mass |
| JP7172129B2 (en) * | 2018-05-17 | 2022-11-16 | 日本軽金属株式会社 | Manufacturing method of electrode for aluminum electrolytic capacitor |
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| CN111146005B (en) * | 2019-12-25 | 2021-04-20 | 西安交通大学 | Sintered low-voltage anode foil of aluminum electrolytic capacitor and preparation method thereof |
| CN110993347B (en) * | 2019-12-25 | 2021-02-12 | 西安交通大学 | High-voltage anode foil of sintered aluminum electrolytic capacitor and preparation method thereof |
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| CN113764191B (en) * | 2021-09-14 | 2022-08-30 | 南通海星电子股份有限公司 | An inhibitor for Al (OH) 3 Method for manufacturing low-voltage electrode foil formed by crystallization |
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