CN101281823A - High specific volume anode aluminum foil and preparation method thereof - Google Patents
High specific volume anode aluminum foil and preparation method thereof Download PDFInfo
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- CN101281823A CN101281823A CNA2008100284934A CN200810028493A CN101281823A CN 101281823 A CN101281823 A CN 101281823A CN A2008100284934 A CNA2008100284934 A CN A2008100284934A CN 200810028493 A CN200810028493 A CN 200810028493A CN 101281823 A CN101281823 A CN 101281823A
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Abstract
The present invention provides a high specific-volume cathode aluminum foil and a method for producing the cathode aluminum foil; the method can increase the specific volume of aluminum electrolytic capacitor; the high specific-volume cathode aluminum foil is a silver-coated cathode aluminum foil with a high dielectric constant. The present invention utilizes the seepage effect of the conducting silver particles doped in aluminum oxide pores to the dielectric layer; the material is dipped in silver-containing solution to deposit silver on the corroded aluminum foil or formed aluminum foil; the silver coated aluminum foil is dried, then the surface is treated or not treated, and the silver-coated aluminum foil is treated through thermal decomposition to form composite Ag-Al oxide film on the surface; finally, the aluminum foil is treated by anodic oxidation, to obtain the high specific-volume cathode aluminum foil. Low-voltage or medium-voltage aluminum electrolytic capacitors fabricated with the high specific-volume aluminize foil have a specific volume improved by 30-200 percent when compared with similar low-voltage or medium-voltage aluminum electrolytic capacitors fabricated with untreated formed foil; in addition, the voltage endurance feature of the anodized dielectric film is greatly improved. The technique can be used with existing electro-chemical corroded surface expansion production lines or formation production lines.
Description
Technical field
The present invention relates to electrolytic capacitor manufacturing technology field, be specifically related to high specific volume anode aluminum foil that is used for by aluminium electrolytic capacitor and preparation method thereof.
Background technology
Specific volume is meant the capacitance that the material of unit volume has.Compare with traditional capacitor, aluminium electrolytic capacitor has the advantage that specific volume is big, price is low, uses in a large number in complete electronic set.But at present big capacity aluminium electrolytic capacitor can't adopt semiconductor technology to realize, in Circuits System, can only be as discrete assembly, and its volume has seriously restricted the progress of miniaturization of complete electronic set system.The core component of aluminium electrolytic capacitor is an aluminium anode foil, its volume dwindle the raising that depends on aluminum electric pole foil specific volume level.
The aluminum electrolysis capacitor anode foil specific volume can be expressed as:
Reduce dielectric layer thickness d in theory, increase anode foils surface area S and can improve specific volume, but the two improvement technology is made slow progress owing near perfect condition.Another effective way is to improve relative dielectric constant ε
r, existing at present a lot of researchers have carried out in aluminium anode foil superficial growth or load high-k complex oxide film Study on Technology, to improve the specific volume of aluminium anode foil.European patent EP 350108 discloses a kind of technology of Dimethyl Ammonium titanate thermal decomposition that adopts at aluminium etched foil superficial growth high-k oxide-film.Japanese kokai publication sho 60-115215 communique discloses the technology that another kind of isopropyl titanate thermal decomposition obtains high-k titanium oxide/aluminum composite membrane.Above technology all need realize that the commercial Application difficulty is big under the non-water environment of strictness.The flat 5-315197 of Te Kaiping 4-42519 and Te Kai Japan special permission communique openly adopts at metal alkoxides such as etched foil surface impregnation titanium, barium, thermal decomposition growth high-k complex oxide film.But because used solution system organic component content height, and need dipping repeatedly, and can't or change into production line with corrosion and realize interlock, production efficiency is low.
In recent years, by the compound system that conducting particles is distributed in the dielectric base body to be constituted, reach and significantly improve the dielectric film STUDY ON THE DIELECTRIC CONSTANTS and cause people's attention gradually.By filled conductive particulate (as carbon black, metal etc.) in dielectric base body, utilize " seep effect " that variation produced of dielectric property with conducting particles content, can significantly change the conductivity of composite material and significantly improve dielectric constant.When compound system reached the seepage flow threshold values, electrically conductive particles can be induced dielectric material polarization greatly under electric field action, make the material of unit volume have bigger capacitance, caused dielectric constant to improve rapidly and reached maximum.High-k means the performance with good store electrical energy, but better application is in miniature large value capacitor.About studies show that of the dielectric property of acetylene black/barium titanate composite material, near the seepage flow threshold values, when acetylene black content was in 0.8～2.0wt% scope, the dielectric constant of acetylene black/barium titanate composite diphase material reached more than 35000, improved about 12 times than pure barium titanate.Halder etc. have studied trace silver and have mixed to the influence of barium phthalate base ceramic capacity density and dielectric constant.Found that when Ag content reached 0.2wt%, its dielectric constant was near 3600.
Summary of the invention
The objective of the invention is to overcome high specific volume aluminium electrolytic capacitor above shortcomings in the prior art, a kind of high specific volume anode aluminum foil and preparation method thereof be provided, described high specific volume anode aluminum foil be have a high-k cover the silver anode aluminium foil.Utilization of the present invention is doped in conductive silver particulate in the aluminium oxide duct to the seepage effect of dielectric layer, not only can improve the dielectric constant of anode oxide film, and the anode foils specific volume is significantly improved, and the voltage endurance of anode foils also improves simultaneously.This technology can expand the face production line with present electrochemical corrosion or change into line realization interlock.
The present invention is implemented in the surface deposition silver of corrosive aluminum foil or formed aluminum foil by the impregnation process Ag-containing solution, after the drying, through or without surface treatment, elevated temperature heat is decomposed to form the Ag-Al complex oxide film, carry out anodized at last, the calorize that obtains high specific volume becomes paper tinsel.The low medium-high voltage aluminum electrolytic capacitor of utilizing the calorize of the high specific volume that the present invention prepares to become paper tinsel to make changes into paper tinsel relatively with undressed, and its specific volume improves 30%-200%.Purpose of the present invention is achieved through the following technical solutions.
The preparation method of high specific volume anode aluminum foil provided by the invention comprises the steps:
(1) cover silver: corrosive aluminum foil or formed aluminum foil are immersed in the Ag-containing solution, and silver concentration is 0.0001～0.05mol/L in the Ag-containing solution, and solution temperature is 0～60 ℃, and soak time is 0.1～10min, and 80～120 ℃ of dryings get the surperficial silver-colored aluminium foil that covers then;
(2) solid silver: silver-colored aluminium foil heat treatment 0.5～30min under 360～600 ℃ of high temperature is covered on the surface that obtains in the step (1), get Ag-Al complex oxide film aluminium foil;
(3) change into: have the aluminium foil of Ag-Al complex oxide film in electrolyte solution, to carry out anodic oxidation surface coverage in the step (2) and change into processing and promptly get described high specific volume anode aluminum foil.
Among the above-mentioned preparation method, also silver-colored aluminium foil is covered on described surface before the heat treatment in the step (2) and in containing the solution of surface modifier, flood 0.1～10min, dry.
Among the above-mentioned preparation method, that the described corrosive aluminum foil of step (1) comprises is low, in or the high pressure corrosive aluminum foil, that described formed aluminum foil comprises is low, in or the high pressure formed aluminum foil;
Among the above-mentioned preparation method, the withstand voltage scope of described corrosive aluminum foil or formed aluminum foil is at 6～720V.
Among the above-mentioned preparation method, described Ag-containing solution comprises inorganic silver saline solution or organic silver salts solution, and described inorganic silver salt is more than one materials in silver soluble complex or the inorganic silver salt; Described organic silver salts is the solubility acylate.
Among the above-mentioned preparation method, described surface modifier is more than one materials in stearic acid, oleic acid, tetraethoxysilane, butyl titanate, softex kw and TBAB mixture, glucose, the polyethylene glycol.
Among the above-mentioned preparation method, described silver soluble complex is silver-colored amine complex, thiosulfuric acid closes silver or dicyan closes silver.
Among the above-mentioned preparation method, described inorganic silver salt is a silver nitrate.
The high specific volume anode aluminum foil that makes by said method.
The present invention has the following advantages and effect:
(1) a kind of novel Ag-Al high-k complex oxide film anode foils of preparation, utilization contains the aluminium electrolytic capacitor of the anode foils preparation of this complex oxide film, its specific volume has improved 30～200% than the electrolytic capacitor that the anode foils with conventional pellumina prepares, and voltage endurance also improves.
(2) technology of the present invention is simple, and is with short production cycle, can or change into the line compatibility with present industrial electrochemistry expansion face corrosion production line, improved product quality and class.
Embodiment
Embodiment 1:
With 335V mesohigh aluminium etched foil at 0.0001mol/LAgNO
3Flood in the solution, the temperature of control solution is 30 ℃, and dip time is 10min.Sample takes out the back and uses washed with de-ionized water, and 100 ℃ of oven dry place 550 ℃ of following constant temperature heat treatment 10min of Muffle furnace immediately, generates the Ag-Al complex oxide film.
Adopt the etched foil after above-mentioned processing step is handled, under the 335V direct voltage, change into corresponding electrolyte solution, get the paper tinsel that changes into of loaded Ag-Al complex oxide film, measure then and change into the paper tinsel specific volume, it becomes the paper tinsel specific volume to improve 35% with respect to the calorize without the present technique Processing of Preparation.
Embodiment 2:
Become paper tinsel to flood in the 0.005mol/L silver ammino solution 590V mesohigh calorize, the temperature of control solution is 0 ℃, and dip time is 0.5min.Sample takes out the back and use washed with de-ionized water, and 90 ℃ of oven dry are dipped in the acetone soln of 50% oleic acid immediately, take out airing and are placed on 400 ℃ of following constant temperature heat treatment 30min in the Muffle furnace, generation Ag-Al complex oxide film.
Adopt the etched foil after above-mentioned processing step is handled, under the 590V direct voltage, change into corresponding electrolyte solution, get the paper tinsel that changes into of loaded Ag-Al complex oxide film, measure then and change into the paper tinsel specific volume, it becomes the paper tinsel specific volume to improve 80% with respect to the calorize without the present technique Processing of Preparation.
Embodiment 3
The low jewelling etched foil of 6V is flooded in 0.003mol/L silver acetate solution, and the temperature of control solution is 50 ℃, and dip time is 0.2min.Take out the sample washed with de-ionized water, 80 ℃ of oven dry then in 5% tetraethoxysilane ethanolic solution lixiviate, are taken out sample and are dried the back at 500 ℃ of following constant temperature heat treatment 10min, generate the Ag-Si-Al complex oxide film.
Adopt the etched foil after above-mentioned processing step is handled, under the 6V direct voltage, change into corresponding electrolyte solution, get the paper tinsel that changes into of loaded Ag-Si-Al complex oxide film, measure then and change into the paper tinsel specific volume, it becomes the paper tinsel specific volume to improve 200% with respect to the calorize without the present technique Processing of Preparation.
Embodiment 4:
Become paper tinsel to put into the mixed solution that concentration that silver-colored ammonium ion and two thiosulfuric acids close silver ion is 0.01mol/L the 375V calorize and flood 5min, solution temperature remains on about 0 ℃.Then sample is dipped in 80 ℃, 2wt% glucose solution, takes out behind the reaction 3min, use the hot water injection, 110 ℃ of dryings.Then at 360 ℃ of constant temperature heat treatment 25min.
The calorize that adopts above-mentioned processing step to handle becomes paper tinsel, changes into corresponding electrolyte solution under the 375V direct voltage, measures then and changes into the paper tinsel specific volume, and it becomes the paper tinsel specific volume to improve 120% with respect to the calorize without the present technique Processing of Preparation.
Embodiment 5:
Become paper tinsel to close in the silver-colored solution at the 0.025mol/L thiosulfuric acid 250V calorize and flood, the temperature of solution is controlled at about 60 ℃, and dip time is 1min.80 ℃ of dryings are placed in 50% stearic acid and oleic acid (mol ratio=1: the 2) ethanolic solution soaks 1min, dries the back at 600 ℃ of following constant temperature heat treatment 0.5min, generates the Al-Ag complex oxide film.
After the above-mentioned steps processing, become paper tinsel under the 250V direct voltage, to change into calorize with corresponding electrolyte solution, test its specific volume then, become paper tinsel to compare with the calorize of handling without present technique, specific volume improves 25%.
Embodiment 6:
720V aluminium etched foil at 60 ℃, is immersed 0.005mol/L liquor argenti nitratis ophthalmicus 1min.Take out sample 80 ℃ of dryings.At room temperature immerse in the following solution then: this solution mixes back room temperature lower magnetic force stirring 3min by CTAB (1.385g), TBAB (0.3073g), ammoniacal liquor (10mL), deionized water (60mL) and is made into.Soak time is 5min.The taking-up sample dries and is placed in 550 ℃ of Muffle furnaces, calcining 8min.
Calorize through above-mentioned PROCESS FOR TREATMENT becomes paper tinsel to change into corresponding electrolyte solution under the 720V direct voltage, tests its specific volume then, becomes paper tinsel to compare with conventional calorize without this technical finesse, and specific volume improves and reaches 30%.
Embodiment 7
Jewelling etched foil among the 120V closed in the silver-colored solution at the 0.05mol/L dicyan flood, the temperature of control solution is 20 ℃, and dip time is 6min.Sample takes out the back and uses washed with de-ionized water, and 85 ℃ of oven dry are dipped in the ethanolic solution of 60% polyethylene glycol (degree of polymerization 500), dip time 10min immediately.Take out airing and be placed on 500 ℃ of following constant temperature heat treatment 10min in the Muffle furnace, generate the Ag-Al complex oxide film.
Adopt the etched foil after above-mentioned processing step is handled, under the 120V direct voltage, change into corresponding electrolyte solution, get the paper tinsel that changes into of loaded Ag-Al complex oxide film, measure then and change into the paper tinsel specific volume, it becomes the paper tinsel specific volume to improve 80% with respect to the calorize without the present technique Processing of Preparation.
Embodiment 8
65V is hanged down the jewelling etched foil at 0.001mol/LAgNO
3Flood in the solution, the temperature of control solution is 20 ℃, and dip time is 2min.Sample takes out the back and uses washed with de-ionized water, and 120 ℃ of oven dry place 580 ℃ of following constant temperature heat treatment 8min of Muffle furnace immediately, generates the Ag-Al complex oxide film.
Adopt the etched foil after above-mentioned processing step is handled, under the 65V direct voltage, change into corresponding electrolyte solution, get the paper tinsel that changes into of loaded Ag-Al complex oxide film, measure then and change into the paper tinsel specific volume, it becomes the paper tinsel specific volume to improve 120% with respect to the calorize without the present technique Processing of Preparation.
Embodiment 9
Low pressure 12V aluminium etched foil is flooded in 0.01mol/L silver acetate solution, and the temperature of control solution is 20 ℃, and dip time is 0.2min.Sample takes out the back and uses washed with de-ionized water, and 3min in the ethanolic solution that contains 30% polyethylene glycol (degree of polymerization 200) and 5% glucose is immersed in 80 ℃ of oven dry, dries to be placed on 560 ℃ of following constant temperature heat treatment 9min in the Muffle furnace, generates the Ag-Al complex oxide film.
Adopt the etched foil after above-mentioned processing step is handled, under the 12V direct voltage, change into corresponding electrolyte solution, get the paper tinsel that changes into of loaded Ag-Al complex oxide film, measure then and change into the paper tinsel specific volume, it becomes the paper tinsel specific volume to improve 30% with respect to the calorize without the present technique Processing of Preparation.
Embodiment 10
Become paper tinsel to flood in the silver nitrate of 0.05mol/L and silver acetate mixed solution at concentration of silver ions low pressure 45V calorize, the temperature of control solution is 0 ℃, and dip time is 0.1min.Sample takes out the back and uses washed with de-ionized water, and 10min in the acetone soln that contains 30% polyethylene glycol (degree of polymerization 100) and 5% oleic acid is immersed in 80 ℃ of oven dry, dries to be placed on 580 ℃ of following constant temperature heat treatment 3min in the Muffle furnace, generates the Ag-Al complex oxide film.
Adopt the etched foil after above-mentioned processing step is handled, under the 45V direct voltage, change into corresponding electrolyte solution, get the paper tinsel that changes into of loaded Ag-Al complex oxide film, measure then and change into the paper tinsel specific volume, it becomes the paper tinsel specific volume to improve 100% with respect to the calorize without the present technique Processing of Preparation.
Embodiment 11
Adopt 290V aluminium etched foil to flood in 0.01mol/L silver acetate solution, the temperature of control solution is 20 ℃, and dip time is 3min.Sample takes out the back washed with de-ionized water, 80 ℃ of oven dry, immersion contains 5min in the ethanolic solution of 10% polyethylene glycol (degree of polymerization 100), 5% butyl titanate and 5% oleic acid, dries to be placed on 600 ℃ of following constant temperature heat treatment 2min of Muffle furnace, generates the Ag-Ti-Al complex oxide film.
Adopt the etched foil after above-mentioned processing step is handled, under the 290V direct voltage, change into corresponding electrolyte solution, get the paper tinsel that changes into of loaded Ag-Ti-Al complex oxide film, measure then and change into the paper tinsel specific volume, it becomes the paper tinsel specific volume to improve 90% with respect to the calorize without the present technique Processing of Preparation.
Embodiment 12
250V mesohigh aluminium etched foil is flooded in 0.009mol/L silver acetate solution, and the temperature of control solution is 35 ℃, and dip time is 8min.Sample takes out the back and uses washed with de-ionized water, and 80 ℃ of oven dry place 360 ℃ of following constant temperature heat treatment 30min of Muffle furnace immediately, generates the Ag-Al complex oxide film.
Adopt the etched foil after above-mentioned processing step is handled, under the 250V direct voltage, change into corresponding electrolyte solution, get the paper tinsel that changes into of loaded Ag-Al complex oxide film, measure then and change into the paper tinsel specific volume, it becomes the paper tinsel specific volume to improve 55% with respect to the calorize without the present technique Processing of Preparation.
Embodiment 13
480V mesohigh aluminium etched foil is flooded in the 0.09mol/L liquor argenti nitratis ophthalmicus, and the temperature of control solution is 55 ℃, and dip time is 1min.Sample takes out the back and uses washed with de-ionized water, and 80 ℃ of oven dry place 600 ℃ of following constant temperature heat treatment 0.5min of Muffle furnace immediately, generates the Ag-Al complex oxide film.
Adopt the etched foil after above-mentioned processing step is handled, under the 480V direct voltage, change into corresponding electrolyte solution, get the paper tinsel that changes into of loaded Ag-Al complex oxide film, measure then and change into the paper tinsel specific volume, it becomes the paper tinsel specific volume to improve 25% with respect to the calorize without the present technique Processing of Preparation.
Claims (9)
1, the preparation method of high specific volume anode aluminum foil is characterized in that comprising the steps:
(1) corrosive aluminum foil or formed aluminum foil are immersed in the Ag-containing solution, silver concentration is 0.0001～0.05mol/L in the Ag-containing solution, and solution temperature is 0～60 ℃, and soak time is 0.1～10min, and 80～120 ℃ of dryings get the surperficial silver-colored aluminium foil that covers then;
(2) silver-colored aluminium foil heat treatment 0.5～30min under 360～600 ℃ of high temperature is covered on the surface that obtains in the step (1), get Ag-Al complex oxide film aluminium foil;
(3) surface coverage in the step (2) being had the aluminium foil of Ag-Al complex oxide film carry out anodic oxidation in electrolyte solution changes into processing and promptly gets described high specific volume anode aluminum foil.
2,, it is characterized in that also silver-colored aluminium foil being covered on described surface before the heat treatment in the step (2) floods 0.1～10min in containing the solution of surface modifier, dry according to the described preparation method of claim 1.
3, preparation method according to claim 1 and 2, it is characterized in that the described corrosive aluminum foil of step (1) comprise low, in or the high pressure corrosive aluminum foil, that described formed aluminum foil comprises is low, in or the high pressure formed aluminum foil.
4, preparation method according to claim 3, the withstand voltage scope that it is characterized in that described corrosive aluminum foil or formed aluminum foil is at 6～720V.
5, preparation method according to claim 4 is characterized in that described Ag-containing solution comprises inorganic silver saline solution or organic silver salts solution, and described inorganic silver salt is more than one materials in silver soluble complex or the inorganic silver salt; Described organic silver salts is the solubility acylate.
6, preparation method according to claim 4 is characterized in that described surface modifier is more than one materials in softex kw and TBAB mixture, stearic acid, oleic acid, tetraethoxysilane, butyl titanate, glucose, the polyethylene glycol.
7, preparation method according to claim 5 is characterized in that described silver soluble complex is silver-colored amine complex, thiosulfuric acid closes silver or dicyan closes silver.
8, preparation method according to claim 5 is characterized in that described inorganic silver salt is a silver nitrate.
9, a kind of high specific volume anode aluminum foil that makes as the described preparation method of one of claim 1～8.
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| CN2008100284934A CN101281823B (en) | 2008-06-03 | 2008-06-03 | High specific volume anode aluminum foil and preparation method thereof |
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| CN2008100284934A CN101281823B (en) | 2008-06-03 | 2008-06-03 | High specific volume anode aluminum foil and preparation method thereof |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101457381B (en) * | 2008-12-24 | 2010-11-17 | 电子科技大学 | Method for preparing high overpressure resistant aluminum electric pole foil |
| CN102568858A (en) * | 2012-01-13 | 2012-07-11 | 西安交通大学 | Production method of high dielectric constant composite alumina film |
| CN103871747A (en) * | 2014-03-06 | 2014-06-18 | 扬州宏远电子有限公司 | Method for improving specific volume of anode foil for aluminum electrolytic condenser |
| CN111926374A (en) * | 2020-07-29 | 2020-11-13 | 东莞东阳光科研发有限公司 | Corrosion method of corrosion foil for aluminum electrolytic capacitor |
| CN117954230A (en) * | 2024-03-27 | 2024-04-30 | 南通江海电容器股份有限公司 | Preparation method and application of medium-high pressure composite formed foil |
-
2008
- 2008-06-03 CN CN2008100284934A patent/CN101281823B/en not_active Expired - Fee Related
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101457381B (en) * | 2008-12-24 | 2010-11-17 | 电子科技大学 | Method for preparing high overpressure resistant aluminum electric pole foil |
| CN102568858A (en) * | 2012-01-13 | 2012-07-11 | 西安交通大学 | Production method of high dielectric constant composite alumina film |
| CN102568858B (en) * | 2012-01-13 | 2013-11-06 | 西安交通大学 | Production method of high dielectric constant composite alumina film |
| CN103871747A (en) * | 2014-03-06 | 2014-06-18 | 扬州宏远电子有限公司 | Method for improving specific volume of anode foil for aluminum electrolytic condenser |
| CN103871747B (en) * | 2014-03-06 | 2017-01-25 | 扬州宏远电子有限公司 | Method for improving specific volume of anode foil for aluminum electrolytic condenser |
| CN111926374A (en) * | 2020-07-29 | 2020-11-13 | 东莞东阳光科研发有限公司 | Corrosion method of corrosion foil for aluminum electrolytic capacitor |
| CN117954230A (en) * | 2024-03-27 | 2024-04-30 | 南通江海电容器股份有限公司 | Preparation method and application of medium-high pressure composite formed foil |
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Assignee: FOILTEC INDUSTRIAL Co.,Ltd. Assignor: South China Normal University Contract record no.: 2012440000328 Denomination of invention: High specific volume anode aluminum foil and preparation method thereof Granted publication date: 20100929 License type: Exclusive License Open date: 20081008 Record date: 20120614 |
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