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 PDF

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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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specific volume
foil
aluminum electrolytic
electrolytic capacitor
anode foil
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CN103871747A (en
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宋卫国
黄佩佩
张椿年
马坤松
曹安民
吴昊
乔正山
张淮浩
王赪胤
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Yangzhou Hongyuan Electronics Co., Ltd.
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YANGZHOU HONGYUAN ELECTRONICS CO Ltd
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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

The method improving anode foil for aluminum electrolytic capacitor specific volume
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.
CN201410080534.XA 2014-03-06 2014-03-06 Method for improving specific volume of anode foil for aluminum electrolytic condenser Active CN103871747B (en)

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Citations (4)

* Cited by examiner, † Cited by third party
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)

* Cited by examiner, † Cited by third party
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
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

Patent Citations (4)

* Cited by examiner, † Cited by third party
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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