CN103871747A - Method for improving specific volume of anode foil for aluminum electrolytic condenser - Google Patents
Method for improving specific volume of anode foil for aluminum electrolytic condenser Download PDFInfo
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- CN103871747A CN103871747A CN201410080534.XA CN201410080534A CN103871747A CN 103871747 A CN103871747 A CN 103871747A CN 201410080534 A CN201410080534 A CN 201410080534A CN 103871747 A CN103871747 A CN 103871747A
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Abstract
The invention discloses a method for improving the specific volume of an anode foil for an aluminum electrolytic condenser, belonging to the technical field of electronic material process. The method comprises the following steps of preparing a TiC14 water solution with a certain concentration, mixing uniformly, dropping a certain amount of tetraethoxysilane into the solution, and repeating the steps of dipping the formed aluminum electrode foil in the solution, aqueous cleaning for twice, and drying for many times, and lastly, performing high-temperature processing to obtain the aluminum electrode boil of which the voltage withstand value and the specific volume value are both improved. The processed object of the method is the formed foil, and the process is simple and convenient for use in production.
Description
Technical field
The present invention relates to a kind of method that improves anode foil for aluminum electrolytic capacitor specific volume, belong to electronic material technology field.
Background technology
For core component-anode aluminum electric pole foil of aluminium electrolytic capacitor, researcher's sight mainly focuses on and how to improve on its specific volume, how the present situation and the oxidated layer thickness substantially invariable fact under certain formation voltage that have reached bottleneck for raising aluminium etched foil sufacing, become study hotspot by the alumina deielectric-coating of modified electrode paper tinsel with the object that reaches raising aluminium anode foil specific volume already.And compared with improving the dielectric constant of alumina dielectric layer, reach by increasing the proof voltage intensity of dielectric layer unit thickness the method that improves aluminium anode foil specific volume, for this research direction provides a kind of brand-new technical thought and approach.
The oxide-film of anode aluminium foil is except having high dielectric constant, and its proof voltage is also an important parameter weighing coating mass and reliability.The content distribution of the densification of oxide-film, integrated degree, the interior impurity of oxide-film and defect, and the dielectric property of oxide self all exert an influence to the withstand voltage of oxide-film.Therefore the proof voltage intensity wanting by increasing dielectric layer unit thickness reaches the object that improves aluminium anode foil specific volume, will be to introducing the good or little material of formation constant of dielectric property in film.SiO
2formation constant less, dielectric property are good, TiO
2dielectric constant higher, therefore the silicon dioxide of high dielectric property is incorporated in the composite membrane of high-k, not only improves the dielectric property of composite membrane, increase pellumina proof voltage intensity, and realize the increase of anode foils specific volume, but report is in this respect less at present.
Summary of the invention
The object of this invention is to provide a kind of method that improves anode foil for aluminum electrolytic capacitor specific volume.
For realizing object of the present invention, a kind of method that improves anode foil for aluminum electrolytic capacitor specific volume, adopts following technical proposals:
A. get certain volume TiCl
4dropwise be added drop-wise to temperature and in intermediate water, stir within the scope of 0～10 DEG C, be mixed with TiCl
4the aqueous solution;
B. in above-mentioned solution, drip tetraethoxysilane (TEOS), be mixed with certain density TEOS maceration extract, in this process, keep solution temperature within the scope of 0～10 DEG C;
C. get the aluminum electric pole foil after changing into, be immersed in completely in above-mentioned dipping solution, dipping, takes out, and after deionized water rinsing, in baking oven, toasts;
D. repeat above-mentioned impregnation steps c;
E. the aluminium foil having flooded is placed in to Muffle furnace calcining and takes out, be cooled to room temperature, obtain the aluminum electric pole foil that withstand voltage improves.
Described TiCl
4concentration of aqueous solution is 0.001～0.1mol/L.
Described TEOS impregnation concentration is 0.0001～0.01mol/L.
Aluminum electric pole foil dip time after described changing into is 30s～30min.
Described baking temperature is 65～115 DEG C.
Described baking time is 30s～20min.
Described repeated impregnations number of times 3～10 times.
The aluminium foil calcining heat that described dipping is good is 300～600 DEG C.
The aluminium foil calcination time that described dipping is good is 30s～30min.
The beneficial effect that the present invention obtains: make Waste Acid From Hua Cheng Foil repeatedly flood the TiCl that contains tetraethoxysilane
4the aqueous solution, after heat treatment reaches withstand voltage and bulking value all increases, and saves material for the production of aluminium electrolytic capacitor, dwindle small product size, and technique is succinct, is convenient to production application.
Embodiment
Below in conjunction with specific embodiment, the present invention is further elaborated, but the present invention is not limited to following examples.Described method is conventional method if no special instructions.
Embodiment 1:
A. get certain volume TiCl
4dropwise be added drop-wise to temperature and within the scope of 0～10 DEG C, in intermediate water, be mixed with the solution that concentration is 0.02mol/L, stir;
B. in above-mentioned solution, drip tetraethoxysilane (TEOS), make the concentration of TEOS at 0.004mol/L, in this process, keep solution temperature within the scope of 0～10 DEG C;
C. get the aluminum electric pole foil after changing into, be immersed in completely in above-mentioned dipping solution, dipping 90s, take out, deionized water rinsing, after in 100 DEG C of baking ovens, dry 3min;
D. repeating step c, 3 times;
E. the aluminium foil having flooded is placed in to Muffle furnace, in 550 DEG C, calcines 5min, take out, be cooled to room temperature, obtain the aluminum electric pole foil that withstand voltage and bulking value all increase.
Embodiment 2:
A. get certain volume TiCl
4dropwise be added drop-wise to temperature and within the scope of 0～10 DEG C, in intermediate water, be mixed with the solution that concentration is 0.008mol/L, stir;
B. in above-mentioned solution, drip tetraethoxysilane (TEOS), make the concentration of TEOS at 0.001mol/L, in this process, keep solution temperature within the scope of 0～10 DEG C;
C. get the aluminum electric pole foil after changing into, be immersed in completely in above-mentioned dipping solution, dipping 5min, take out, deionized water rinsing, after in 90 DEG C of baking ovens, dry 5min;
D. repeating step c, 5 times;
E. the aluminium foil having flooded is placed in to Muffle furnace, in 500 DEG C, calcines 8min, take out, be cooled to room temperature, obtain the aluminum electric pole foil that withstand voltage and bulking value all increase.
Embodiment 3:
A. get certain volume TiCl
4dropwise be added drop-wise to temperature and within the scope of 0～10 DEG C, in intermediate water, be mixed with the solution that concentration is 0.004mol/L, stir;
B. in above-mentioned solution, drip tetraethoxysilane (TEOS), make the concentration of TEOS at 0.001mol/L, in this process, keep solution temperature within the scope of 0～10 DEG C;
C. get the aluminum electric pole foil after changing into, be immersed in completely in above-mentioned dipping solution, dipping 8min, take out, deionized water rinsing, after in 80 DEG C of baking ovens, dry 8min;
D. repeating step c, 6 times;
E. the aluminium foil having flooded is placed in to Muffle furnace, in 450 DEG C, calcines 10min, take out, be cooled to room temperature, obtain the aluminum electric pole foil that withstand voltage and bulking value all increase.
Embodiment 4:
A. get certain volume TiCl
4dropwise be added drop-wise to temperature and within the scope of 0～10 DEG C, in intermediate water, be mixed with the solution that concentration is 0.002mol/L, stir;
B. in above-mentioned solution, drip tetraethoxysilane (TEOS), make the concentration of TEOS at 0.0005mol/L, in this process, keep solution temperature within the scope of 0～10 DEG C;
C. get the aluminum electric pole foil after changing into, be immersed in completely in above-mentioned dipping solution, dipping 15min, take out, deionized water rinsing, after in 80 DEG C of baking ovens, dry 10min;
D. repeating step c, 7 times;
E. the aluminium foil having flooded is placed in to Muffle furnace, in 300 DEG C, calcines 15min, take out, be cooled to room temperature, obtain the electrode foil that withstand voltage and bulking value all increase.
Table 1 aluminium Waste Acid From Hua Cheng Foil processes front and back withstand voltage and bulking value changes
| Numbering | Withstand voltage/V | Bulking value/μ f/cm 2 |
| Embodiment 1 | 25.5 | 75.3 |
| Embodiment 2 | 28.8 | 74.6 |
| Embodiment 3 | 29.4 | 73.9 |
| Embodiment 4 | 27.9 | 74.1 |
| Untreated Waste Acid From Hua Cheng Foil | 23.7 | 73.5 |
Claims (9)
1. improve a method for anode foil for aluminum electrolytic capacitor specific volume, it is characterized in that comprising the following steps:
A. get certain volume TiCl
4dropwise be added drop-wise to temperature and in intermediate water, stir within the scope of 0 ~ 10 C, be mixed with TiCl
4the aqueous solution;
B. in above-mentioned solution, drip tetraethoxysilane, be mixed with certain density tetraethoxysilane maceration extract, in this process, keep solution temperature within the scope of 0 ~ 10 C;
C. get the aluminum electric pole foil after changing into, be immersed in completely in above-mentioned dipping solution, dipping, take out, deionized water rinsing, after in baking oven, toast;
D. repeat above-mentioned impregnation steps c;
E. the aluminium foil having flooded is placed in to Muffle furnace calcining and takes out, be cooled to room temperature, obtain the aluminum electric pole foil that withstand voltage improves.
2. a kind of method that improves anode foil for aluminum electrolytic capacitor specific volume as claimed in claim 1, is characterized in that: TiCl
4concentration of aqueous solution is 0.001 ~ 0.1mol/L.
3. a kind of method that improves anode foil for aluminum electrolytic capacitor specific volume as claimed in claim 1, is characterized in that: tetraethoxysilane impregnation concentration is 0.0001 ~ 0.01 mol/L.
4. a kind of method that improves anode foil for aluminum electrolytic capacitor specific volume as claimed in claim 1, is characterized in that: the aluminum electric pole foil dip time after changing into is 30s ~ 30min.
5. a kind of method that improves anode foil for aluminum electrolytic capacitor specific volume as claimed in claim 1, is characterized in that: baking temperature is 65 ~ 115 C.
6. a kind of method that improves anode foil for aluminum electrolytic capacitor specific volume as claimed in claim 1, is characterized in that: baking time is 30s ~ 20min.
7. a kind of method that improves anode foil for aluminum electrolytic capacitor specific volume as claimed in claim 1, is characterized in that: repeated impregnations number of times 3 ~ 10 times.
8. a kind of method that improves anode foil for aluminum electrolytic capacitor specific volume as claimed in claim 1, is characterized in that: the aluminium foil calcining heat of having flooded is 300 ~ 600 C.
9. a kind of method that improves anode foil for aluminum electrolytic capacitor specific volume as claimed in claim 1, is characterized in that: the aluminium foil calcination time having flooded is 30s ~ 30min.
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| CN201410080534.XA CN103871747B (en) | 2014-03-06 | 2014-03-06 | Method for improving specific volume of anode foil for aluminum electrolytic condenser |
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| CN103871747B CN103871747B (en) | 2017-01-25 |
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Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH08213288A (en) * | 1995-02-03 | 1996-08-20 | Mitsubishi Shindoh Co Ltd | Anodic foil for electrolytic capacitor and manufacture thereof |
| JP2003224036A (en) * | 2002-01-31 | 2003-08-08 | Japan Carlit Co Ltd:The | Aluminum anode foil for electrolytic capacitor and its manufacturing method |
| US20060076243A1 (en) * | 2004-10-12 | 2006-04-13 | Tatsuji Aoyama | Electrode foil for electrolytic capacitor and method for manufacturing the same |
| CN1766168A (en) * | 2005-10-10 | 2006-05-03 | 西安交通大学 | Titanium oxide/aluminum oxide high dielectric constant composite anode film preparation method |
| CN101191224A (en) * | 2006-11-24 | 2008-06-04 | 横店集团东磁有限公司 | Method for manufacturing anode foil for aluminum electrolytic capacitor |
| CN101281823A (en) * | 2008-06-03 | 2008-10-08 | 华南师范大学 | High specific volume anode aluminum foil and preparation method thereof |
| CN102568858A (en) * | 2012-01-13 | 2012-07-11 | 西安交通大学 | Production method of high dielectric constant composite alumina film |
-
2014
- 2014-03-06 CN CN201410080534.XA patent/CN103871747B/en active Active
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH08213288A (en) * | 1995-02-03 | 1996-08-20 | Mitsubishi Shindoh Co Ltd | Anodic foil for electrolytic capacitor and manufacture thereof |
| JP2003224036A (en) * | 2002-01-31 | 2003-08-08 | Japan Carlit Co Ltd:The | Aluminum anode foil for electrolytic capacitor and its manufacturing method |
| US20060076243A1 (en) * | 2004-10-12 | 2006-04-13 | Tatsuji Aoyama | Electrode foil for electrolytic capacitor and method for manufacturing the same |
| CN1766168A (en) * | 2005-10-10 | 2006-05-03 | 西安交通大学 | Titanium oxide/aluminum oxide high dielectric constant composite anode film preparation method |
| CN101191224A (en) * | 2006-11-24 | 2008-06-04 | 横店集团东磁有限公司 | Method for manufacturing anode foil for aluminum electrolytic capacitor |
| CN101281823A (en) * | 2008-06-03 | 2008-10-08 | 华南师范大学 | High specific volume anode aluminum foil and preparation method thereof |
| CN102568858A (en) * | 2012-01-13 | 2012-07-11 | 西安交通大学 | Production method of high dielectric constant composite alumina film |
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