CN103871747B - 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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- CN103871747B CN103871747B CN201410080534.XA CN201410080534A CN103871747B CN 103871747 B CN103871747 B CN 103871747B CN 201410080534 A CN201410080534 A CN 201410080534A CN 103871747 B CN103871747 B CN 103871747B
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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 improving anode foil for aluminum electrolytic capacitor specific volume, belong to electronic material Technology
Field.
Background technology
For the core component anode aluminum electric pole foil of aluminium electrolutic capacitor, the sight of researcher is focused primarily on and how to carry
On its specific volume high, the present situation of bottleneck and oxidated layer thickness are reached under certain formation voltage for improving aluminum etched foil sufacing
The fact that substantially constant, how the purpose improving aluminium anode foil specific volume is reached already by the alumina deielectric-coating of modified electrode paper tinsel
Become study hotspot.And compared with the dielectric constant improving alumina dielectric layer, by increasing the proof voltage of dielectric layer unit thickness
Intensity, to reach the method improving aluminium anode foil specific volume, provides a kind of brand-new technical thought and approach for this research direction.
Except having high dielectric constant, its proof voltage is also to weigh coating mass and can to the oxide-film of anode aluminium foil
An important parameter by property.The densification of oxide-film, integrated degree, in oxide-film impurity and defect content distribution, and oxygen
The pressure generation impact all on oxide-film for the dielectric properties of compound itself.Therefore want by increasing the resistance to of dielectric layer unit thickness
It is necessary to introduce into film, dielectric properties are good or formation constantc1 is little to reach the purpose improving aluminium anode foil specific volume for voltage strength
Material.sio2Formation constantc1 less, dielectric properties are good, tio2Dielectric constant higher, therefore by the dioxy of high dielectric property
SiClx is incorporated in the composite membrane of high-k, not only improves the dielectric properties of composite membrane, increases pellumina proof voltage strong
Degree, and realize the increase of anode foils specific volume, but report in this respect is less at present.
Content of the invention
It is an object of the invention to provide a kind of method improving anode foil for aluminum electrolytic capacitor specific volume.
For realizing the purpose of the present invention, a kind of method of raising anode foil for aluminum electrolytic capacitor specific volume, using following skills
Art scheme:
A. take certain volume ticl4Dropwise it is added drop-wise in temperature secondary water in the range of 0~10 DEG C, stirs, prepare
Become ticl4Aqueous solution;
B. to Deca tetraethyl orthosilicate (teos) in above-mentioned solution, it is configured to certain density teos impregnation liquid, this process
Middle holding solution temperature is in the range of 0~10 DEG C;
C. take the aluminum electric pole foil after chemical conversion, be totally immersed in above-mentioned dipping solution, dipping, takes out, deionized water rinsing
Afterwards, toast in an oven;
D. above-mentioned impregnation steps c are repeated;
E. the aluminium foil having impregnated is placed in calcining in Muffle furnace to take out, is cooled to room temperature, that is, obtain pressure voltage raising
Aluminum electric pole foil.
Described ticl4Concentration 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 chemical conversion 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 described aluminium foil calcining heat having impregnated is 300~600 DEG C.
The described aluminium foil calcination time having impregnated is 30s~30min.
The beneficial effect that the present invention obtains: make Waste Acid From Hua Cheng Foil repeatedly impregnate the ticl containing tetraethyl orthosilicate4Aqueous solution, through warm
Reach pressure voltage after process and bulking value all increase, be that material is saved in the production of aluminium electrolutic capacitor, reduce small product size,
And concise in technology, it is easy to production application.
Specific embodiment
With reference to specific embodiment, the present invention is further elaborated, but the present invention is not limited to following examples.Institute
Method of stating is conventional method if no special instructions.
Embodiment 1:
A. take certain volume ticl4Dropwise it is added drop-wise to and be configured to concentration in temperature secondary water in the range of 0~10 DEG C and be
The solution of 0.02mol/l, stirs;
B. to Deca tetraethyl orthosilicate (teos) in above-mentioned solution, the concentration making teos in 0.004mol/l, should during
Keep solution temperature in the range of 0~10 DEG C;
C. take the aluminum electric pole foil after chemical conversion, be totally immersed in above-mentioned dipping solution, impregnate 90s, take out, deionized water rushes
Wash, after in 100 DEG C of baking ovens dry 3min;
D. repeat step c, 3 times;
E. the aluminium foil having impregnated is placed in Muffle furnace, in 550 DEG C, calcines 5min, take out, be cooled to room temperature, obtain final product
The aluminum electric pole foil all increasing to pressure voltage and bulking value.
Embodiment 2:
A. take certain volume ticl4Dropwise it is added drop-wise to and be configured to concentration in temperature secondary water in the range of 0~10 DEG C and be
The solution of 0.008mol/l, stirs;
B. to Deca tetraethyl orthosilicate (teos) in above-mentioned solution, the concentration making teos in 0.001mol/l, should during
Keep solution temperature in the range of 0~10 DEG C;
C. take the aluminum electric pole foil after chemical conversion, be totally immersed in above-mentioned dipping solution, impregnate 5min, take out, deionized water
Rinse, after in 90 DEG C of baking ovens dry 5min;
D. repeat step c, 5 times;
E. the aluminium foil having impregnated is placed in Muffle furnace, in 500 DEG C, calcines 8min, take out, be cooled to room temperature, obtain final product
The aluminum electric pole foil all increasing to pressure voltage and bulking value.
Embodiment 3:
A. take certain volume ticl4Dropwise it is added drop-wise to and be configured to concentration in temperature secondary water in the range of 0~10 DEG C and be
The solution of 0.004mol/l, stirs;
B. to Deca tetraethyl orthosilicate (teos) in above-mentioned solution, the concentration making teos in 0.001mol/l, should during
Keep solution temperature in the range of 0~10 DEG C;
C. take the aluminum electric pole foil after chemical conversion, be totally immersed in above-mentioned dipping solution, impregnate 8min, take out, deionized water
Rinse, after in 80 DEG C of baking ovens dry 8min;
D. repeat step c, 6 times;
E. the aluminium foil having impregnated is placed in Muffle furnace, in 450 DEG C, calcines 10min, take out, be cooled to room temperature, that is,
Obtain the aluminum electric pole foil that pressure voltage and bulking value all increase.
Embodiment 4:
A. take certain volume ticl4Dropwise it is added drop-wise to and be configured to concentration in temperature secondary water in the range of 0~10 DEG C and be
The solution of 0.002mol/l, stirs;
B. to Deca tetraethyl orthosilicate (teos) in above-mentioned solution, the concentration making teos in 0.0005mol/l, should during
Keep solution temperature in the range of 0~10 DEG C;
C. take the aluminum electric pole foil after chemical conversion, be totally immersed in above-mentioned dipping solution, impregnate 15min, take out, deionized water
Rinse, after in 80 DEG C of baking ovens dry 10min;
D. repeat step c, 7 times;
E. the aluminium foil having impregnated is placed in Muffle furnace, in 300 DEG C, calcines 15min, take out, be cooled to room temperature, that is,
Obtain the electrode foil that pressure voltage and bulking value all increase.
Pressure voltage and specific volume value changes after table 1 aluminum Waste Acid From Hua Cheng Foil before processing
Numbering | Pressure voltage/v | Bulking value/μ f/cm2 |
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. a kind of method improving anode foil for aluminum electrolytic capacitor specific volume is it is characterised in that comprise the following steps:
A. take certain volume ticl4Dropwise it is added drop-wise in temperature secondary water in the range of 0~10 DEG C, stir, be configured to
ticl4Aqueous solution;
B. to Deca tetraethyl orthosilicate in above-mentioned solution, it is configured to certain density tetraethyl orthosilicate impregnation liquid, protect during being somebody's turn to do
Hold solution temperature in the range of 0~10 DEG C;
C. take the aluminum electric pole foil after chemical conversion, be totally immersed in above-mentioned dipping solution, dipping, take out, deionized water rinsing, after
Toast in baking oven;
D. above-mentioned impregnation steps c are repeated;
E. the aluminium foil having impregnated is placed in calcining in Muffle furnace to take out, is cooled to room temperature, that is, obtain the aluminum electricity of pressure voltage raising
Pole paper tinsel.
2. as claimed in claim 1 a kind of improve anode foil for aluminum electrolytic capacitor specific volume method it is characterised in that: ticl4
Concentration of aqueous solution is 0.001~0.1mol/l.
3. as claimed in claim 1 a kind of method improving anode foil for aluminum electrolytic capacitor specific volume it is characterised in that: positive silicon
In acetoacetic ester impregnation liquid, the concentration of tetraethyl orthosilicate is 0.0001~0.01mol/l.
4. as claimed in claim 1 a kind of improve anode foil for aluminum electrolytic capacitor specific volume method it is characterised in that: chemical conversion
Aluminum electric pole foil dip time afterwards is 30s~30min.
5. as claimed in claim 1 a kind of improve anode foil for aluminum electrolytic capacitor specific volume method it is characterised in that: baking
Temperature is 65~115 DEG C.
6. as claimed in claim 1 a kind of improve anode foil for aluminum electrolytic capacitor specific volume method it is characterised in that: baking
Time is 30s~20min.
7. as claimed in claim 1 a kind of improve anode foil for aluminum electrolytic capacitor specific volume method it is characterised in that: repeat
Dipping number of times 3~10 times.
8. as claimed in claim 1 a kind of improve anode foil for aluminum electrolytic capacitor specific volume method it is characterised in that: dipping
Good aluminium foil calcining heat is 300~600 DEG C.
9. as claimed in claim 1 a kind of improve anode foil for aluminum electrolytic capacitor specific volume method it is characterised in that: dipping
Good aluminium foil calcination time is 30s~30min.
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Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
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 | Manufacturing method of 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 |
Family Cites Families (3)
Publication number | Priority date | Publication date | Assignee | Title |
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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 |
JP4572649B2 (en) * | 2004-10-12 | 2010-11-04 | パナソニック株式会社 | Method for producing electrode foil for electrolytic capacitor |
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Patent Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
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 | Manufacturing method of 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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