CN100365167C - Titanium oxide/aluminum oxide high dielectric constant composite anode film preparation method - Google Patents
Titanium oxide/aluminum oxide high dielectric constant composite anode film preparation method Download PDFInfo
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- CN100365167C CN100365167C CNB2005100961315A CN200510096131A CN100365167C CN 100365167 C CN100365167 C CN 100365167C CN B2005100961315 A CNB2005100961315 A CN B2005100961315A CN 200510096131 A CN200510096131 A CN 200510096131A CN 100365167 C CN100365167 C CN 100365167C
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Abstract
The present invention relates to a making method for high dielectric constant combined anodized films of titanium dioxide/alumina. The method adopts a sol and gel method to make a precursor of titanium, the precursor is coated on the surface of corroded aluminum foil through a soaking and pulling method, and a layer of titanium oxide film with a high dielectric constant is formed after heat treatment. Then, anodic oxidation is carried out to the corroded aluminum foil coated with the titanium oxide film to form a layer of combined anodic oxide film with a high dielectric constant. Because the dielectric constant of the titanium oxide is much larger than that of the aluminum oxide, the dielectric constant of the made combined film is larger than 10, and the specific capacity of an aluminum electrolytic capacitor is greatly increased. The present invention has the advantages of simple process and convenient operation.
Description
Technical field
The invention belongs to the electronic material preparing technical field, particularly the preparation method of titanium oxide/aluminum oxide oxide high dielectric constant composite anode film.
Background technology
Along with the high speed development of electronic industry, the integrated degree of electronic product is more and more higher, and electronic system product is miniaturization more, portability.This just requires various electronic components to develop towards the mini-direction.Aluminium electrolutic capacitor has the big advantage of specific volume and uses in a large number in electronic product, but at present also can't be integrated, and its volume has restricted the miniaturization of electronic system product.The volume of aluminium electrolutic capacitor is limited by the specific volume of anode foils, and the specific volume that improves anode foils can dwindle its volume.The specific capacitance of anode foils is directly proportional with specific inductivity, the specific surface area of anode oxide film in theory, is inversely proportional to thickness.In order to improve specific capacitance, can improve specific inductivity and specific surface area, reduce thickness, but technical being difficult to improved the etched foil specific surface area again, and thickness is decided by operating voltage.Thereby the raising specific inductivity is a kind of desirable method.
Usually the method for the anode oxide film of preparation aluminium electrolutic capacitor is: etched foil is immersed in applies certain voltage in the boric acid or the aqueous solution such as its ammonium salt, hexanodioic acid or its ammonium salt and carry out anodic oxidation and form Al
2O
3Deielectric-coating.The specific inductivity of this deielectric-coating is not high, usually between 8～10.
Summary of the invention
The object of the present invention is to provide a kind of preparation method that can improve the titanium oxide/aluminum oxide oxide high dielectric constant composite anode film of the electrical capacity of electrolytic condenser.
For achieving the above object, the preparation method that the present invention adopts is: at first the huge legendary turtle that tetrabutyl titanate, isopropyl titanate or tetraethyl titanate and pure lactic acid, acetic acid, methyl ethyl diketone or ethylene glycol monomethyl ether solution were carried out under 40-80 ℃ 6-24 hour by 1: 1～5 volume ratio is closed reaction, and then adding the water adjusting, to make the concentration of titanium be the organic slat solution that 0.01～5mol/l makes titanium; Then corrosive aluminum foil was immersed in the organic slat solution of titanium 0.5～3 minute, and took out the air thermal treatment 5～60 minutes of directly putting into 450～600 ℃ after drying, on corrosive aluminum foil, form thin film of titanium oxide; It is in 1～15% the feeble-acid-ammonium salt solution that the corrosive aluminum foil that will form thin film of titanium oxide is at last inserted mass concentration, anodic oxidation is 5～120 minutes under the voltage of 10～300V, then 450～550 ℃ of thermal treatments after 1～10 minute, insert once more in the above-mentioned feeble-acid-ammonium salt solution, anodic oxidation got final product in 1～10 minute under identical voltage.
The said feeble-acid-ammonium salt solution of the present invention is ammonium adipate, ammonium borate or ammonium dihydrogen phosphate.
Because the specific inductivity of titanium oxide is higher than aluminum oxide far away, so the present invention forms the oxide film that one deck forms high-k earlier on the corrosive aluminum foil surface, and then anodic oxidation, thereby form the composite dielectric film of high-k, can prepare specific inductivity according to preparation method of the present invention and surpass 10 compound medium layer, thereby prepare the anode foils of the aluminium electrolutic capacitor of high specific capacitance amount.
Embodiment 1: at first the huge legendary turtle that tetrabutyl titanate and pure lactic acid solution were carried out under 80 ℃ 6 hours by 1: 1 volume ratio is closed reaction, and then adds water and regulate that to make the concentration of titanium be the organic slat solution that 0.01mol/l makes titanium; Then corrosive aluminum foil was immersed in the organic slat solution of titanium 3 minutes, and took out the air thermal treatment 60 minutes of directly putting into 450 ℃ after drying, on corrosive aluminum foil, form thin film of titanium oxide; It is in 15% the ammonium adipate solution that the corrosive aluminum foil that will form thin film of titanium oxide is at last inserted mass concentration, anodic oxidation is 5 minutes under the voltage of 10V, then 450 ℃ of thermal treatments after 10 minutes, insert once more in the above-mentioned ammonium adipate solution, anodic oxidation got final product in 1 minute under identical voltage.
Embodiment 2: at first the huge legendary turtle that isopropyl titanate and pure acetum were carried out under 50 ℃ 12 hours by 1: 4 volume ratio is closed reaction, and then adds water and regulate that to make the concentration of titanium be the organic slat solution that 0.1mol/l makes titanium; Then corrosive aluminum foil was immersed in the organic slat solution of titanium 2 minutes, and took out the air thermal treatment 5 minutes of directly putting into 600 ℃ after drying, on corrosive aluminum foil, form thin film of titanium oxide; It is in 8% the ammonium borate solution that the corrosive aluminum foil that will form thin film of titanium oxide is at last inserted mass concentration, anodic oxidation is 120 minutes under the voltage of 300V,, insert once more in the above-mentioned ammonium borate solution after 1 minute 550 ℃ of thermal treatments then, anodic oxidation got final product in 10 minutes under identical voltage.
Embodiment 3: at first the huge legendary turtle that tetraethyl titanate and methyl ethyl diketone solution were carried out under 70 ℃ 20 hours by 1: 2 volume ratio is closed reaction, and then adds water and regulate that to make the concentration of titanium be the organic slat solution that 3mol/l makes titanium; Then corrosive aluminum foil was immersed in the organic slat solution of titanium 1 minute, and took out the air thermal treatment 30 minutes of directly putting into 500 ℃ after drying, on corrosive aluminum foil, form thin film of titanium oxide; It is in 1% the ammonium dihydrogen phosphate that the corrosive aluminum foil that will form thin film of titanium oxide is at last inserted mass concentration, anodic oxidation is 70 minutes under the voltage of 100V, then 500 ℃ of thermal treatments after 5 minutes, insert once more in the above-mentioned ammonium dihydrogen phosphate, anodic oxidation got final product in 5 minutes under identical voltage.
Embodiment 4: at first the huge legendary turtle that tetrabutyl titanate and pure ethylene glycol monomethyl ether solution were carried out under 40 ℃ 24 hours by 1: 3 volume ratio is closed reaction, and then adds water and regulate that to make the concentration of titanium be the organic slat solution that 1mol/l makes titanium; Then corrosive aluminum foil was immersed in the organic slat solution of titanium 2.5 minutes, and took out the air thermal treatment 20 minutes of directly putting into 560 ℃ after drying, on corrosive aluminum foil, form thin film of titanium oxide; It is in 7% the ammonium adipate solution that the corrosive aluminum foil that will form thin film of titanium oxide is at last inserted mass concentration, anodic oxidation is 100 minutes under the voltage of 200V, then 520 ℃ of thermal treatments after 3 minutes, insert once more in the above-mentioned ammonium adipate solution, anodic oxidation got final product in 8 minutes under identical voltage.
Embodiment 5: at first the huge legendary turtle that isopropyl titanate and pure lactic acid solution were carried out under 60 ℃ 18 hours by 1: 5 volume ratio is closed reaction, and then adds water and regulate that to make the concentration of titanium be the organic slat solution that 5mol/l makes titanium; Then corrosive aluminum foil was immersed in the organic slat solution of titanium 0.5 minute, and took out the air thermal treatment 45 minutes of directly putting into 480 ℃ after drying, on corrosive aluminum foil, form thin film of titanium oxide; It is in 5% the ammonium borate solution that the corrosive aluminum foil that will form thin film of titanium oxide is at last inserted mass concentration, anodic oxidation is 50 minutes under the voltage of 80V,, insert once more in the above-mentioned ammonium borate solution after 8 minutes 480 ℃ of thermal treatments then, anodic oxidation got final product in 5 minutes under identical voltage.
Embodiment 6: at first the huge legendary turtle that tetraethyl titanate and pure methyl ethyl diketone solution were carried out under 73 ℃ 10 hours by 1: 2.5 volume ratio is closed reaction, and then adds water and regulate that to make the concentration of titanium be the organic slat solution that 2.5mol/l makes titanium; Then corrosive aluminum foil was immersed in the organic slat solution of titanium 1.5 minutes, and took out the air thermal treatment 38 minutes of directly putting into 530 ℃ after drying, on corrosive aluminum foil, form thin film of titanium oxide; It is in 10% the ammonium dihydrogen phosphate that the corrosive aluminum foil that will form thin film of titanium oxide is at last inserted mass concentration, anodic oxidation is 80 minutes under the voltage of 150V, then 465 ℃ of thermal treatments after 6 minutes, insert once more in the above-mentioned ammonium dihydrogen phosphate, anodic oxidation got final product in 6 minutes under identical voltage.
Because the specific inductivity of titanium oxide is higher than aluminum oxide far away, so the present invention forms one deck thin film of titanium oxide earlier and forms composite anode oxide film by anodic oxidation on the corrosive aluminum foil surface again on corrosive aluminum foil, prepare specific inductivity and surpass 10 compound medium layer, thereby prepare the anode foils of the aluminium electrolutic capacitor of high specific capacitance amount.
Claims (8)
1. the preparation method of titanium oxide/aluminum oxide oxide high dielectric constant composite anode film is characterized in that:
1) huge legendary turtle that at first tetrabutyl titanate, isopropyl titanate or tetraethyl titanate and pure lactic acid, acetic acid, methyl ethyl diketone or ethylene glycol monomethyl ether solution was carried out under 40-80 ℃ 6-24 hour by 1: 1～5 volume ratio is closed reaction, and then adds water and regulate that to make the concentration of titanium be the organic slat solution that 0.01～5mol/l makes titanium;
2) then corrosive aluminum foil is immersed in the organic slat solution of titanium 0.5～3 minute, take out the air thermal treatment 5～60 minutes of directly putting into 450～600 ℃ after drying, on corrosive aluminum foil, form thin film of titanium oxide;
3) to insert mass concentration be in 1～15% the feeble-acid-ammonium salt solution to the corrosive aluminum foil that will form thin film of titanium oxide at last, anodic oxidation is 5～120 minutes under the voltage of 10～300V, then 450～550 ℃ of thermal treatments after 1～10 minute, insert once more in the above-mentioned feeble-acid-ammonium salt solution, anodic oxidation got final product in 1～10 minute under identical voltage.
2. the preparation method of titanium oxide according to claim 1/aluminum oxide oxide high dielectric constant composite anode film is characterized in that: said feeble-acid-ammonium salt solution is ammonium adipate, ammonium borate or ammonium dihydrogen phosphate.
3. the preparation method of titanium oxide according to claim 1/aluminum oxide oxide high dielectric constant composite anode film, it is characterized in that: at first the huge legendary turtle that tetrabutyl titanate and pure lactic acid solution were carried out under 80 ℃ 6 hours by 1: 1 volume ratio is closed reaction, and then adds water and regulate that to make the concentration of titanium be the organic slat solution that 0.01mol/l makes titanium; Then corrosive aluminum foil was immersed in the organic slat solution of titanium 3 minutes, and took out the air thermal treatment 60 minutes of directly putting into 450 ℃ after drying, on corrosive aluminum foil, form thin film of titanium oxide; It is in 15% the ammonium adipate solution that the corrosive aluminum foil that will form thin film of titanium oxide is at last inserted mass concentration, anodic oxidation is 5 minutes under the voltage of 10V, then 450 ℃ of thermal treatments after 10 minutes, insert once more in the above-mentioned ammonium adipate solution, anodic oxidation got final product in 1 minute under identical voltage.
4. the preparation method of titanium oxide according to claim 1/aluminum oxide oxide high dielectric constant composite anode film, it is characterized in that: at first the huge legendary turtle that isopropyl titanate and pure acetum were carried out under 50 ℃ 12 hours by 1: 4 volume ratio is closed reaction, and then adds water and regulate that to make the concentration of titanium be the organic slat solution that 0.1mol/l makes titanium; Then corrosive aluminum foil was immersed in the organic slat solution of titanium 2 minutes, and took out the air thermal treatment 5 minutes of directly putting into 600 ℃ after drying, on corrosive aluminum foil, form thin film of titanium oxide; It is in 8% the ammonium borate solution that the corrosive aluminum foil that will form thin film of titanium oxide is at last inserted mass concentration, anodic oxidation is 120 minutes under the voltage of 300V,, insert once more in the above-mentioned ammonium borate solution after 1 minute 550 ℃ of thermal treatments then, anodic oxidation got final product in 10 minutes under identical voltage.
5. the preparation method of titanium oxide according to claim 1/aluminum oxide oxide high dielectric constant composite anode film, it is characterized in that: at first the huge legendary turtle that tetraethyl titanate and methyl ethyl diketone solution were carried out under 70 ℃ 20 hours by 1: 2 volume ratio is closed reaction, and then adds water and regulate that to make the concentration of titanium be the organic slat solution that 3mol/l makes titanium; Then corrosive aluminum foil was immersed in the organic slat solution of titanium 1 minute, and took out the air thermal treatment 30 minutes of directly putting into 500 ℃ after drying, on corrosive aluminum foil, form thin film of titanium oxide; It is in 1% the ammonium dihydrogen phosphate that the corrosive aluminum foil that will form thin film of titanium oxide is at last inserted mass concentration, anodic oxidation is 70 minutes under the voltage of 100V, then 500 ℃ of thermal treatments after 5 minutes, insert once more in the above-mentioned ammonium dihydrogen phosphate, anodic oxidation got final product in 5 minutes under identical voltage.
6. the preparation method of titanium oxide according to claim 1/aluminum oxide oxide high dielectric constant composite anode film, it is characterized in that: at first the huge legendary turtle that tetrabutyl titanate and pure ethylene glycol monomethyl ether solution were carried out under 40 ℃ 24 hours by 1: 3 volume ratio is closed reaction, and then adds water and regulate that to make the concentration of titanium be the organic slat solution that 1mol/l makes titanium; Then corrosive aluminum foil was immersed in the organic slat solution of titanium 2.5 minutes, and took out the air thermal treatment 20 minutes of directly putting into 560 ℃ after drying, on corrosive aluminum foil, form thin film of titanium oxide; It is in 7% the ammonium adipate solution that the corrosive aluminum foil that will form thin film of titanium oxide is at last inserted mass concentration, anodic oxidation is 100 minutes under the voltage of 200V, then 520 ℃ of thermal treatments after 3 minutes, insert once more in the above-mentioned ammonium adipate solution, anodic oxidation got final product in 8 minutes under identical voltage.
7. the preparation method of titanium oxide according to claim 1/aluminum oxide oxide high dielectric constant composite anode film, it is characterized in that: at first the huge legendary turtle that isopropyl titanate and pure lactic acid solution were carried out under 60 ℃ 18 hours by 1: 5 volume ratio is closed reaction, and then adds water and regulate that to make the concentration of titanium be the organic slat solution that 5mol/l makes titanium; Then corrosive aluminum foil was immersed in the organic slat solution of titanium 0.5 minute, and took out the air thermal treatment 45 minutes of directly putting into 480 ℃ after drying, on corrosive aluminum foil, form thin film of titanium oxide; It is in 5% the ammonium borate solution that the corrosive aluminum foil that will form thin film of titanium oxide is at last inserted mass concentration, anodic oxidation is 50 minutes under the voltage of 80V,, insert once more in the above-mentioned ammonium borate solution after 8 minutes 480 ℃ of thermal treatments then, anodic oxidation got final product in 5 minutes under identical voltage.
8. the preparation method of titanium oxide according to claim 1/aluminum oxide oxide high dielectric constant composite anode film, it is characterized in that: at first the huge legendary turtle that tetraethyl titanate and pure methyl ethyl diketone solution were carried out under 73 ℃ 10 hours by 1: 2.5 volume ratio is closed reaction, and then adds water and regulate that to make the concentration of titanium be the organic slat solution that 2.5mol/l makes titanium; Then corrosive aluminum foil was immersed in the organic slat solution of titanium 1.5 minutes, and took out the air thermal treatment 38 minutes of directly putting into 530 ℃ after drying, on corrosive aluminum foil, form thin film of titanium oxide; It is in 10% the ammonium dihydrogen phosphate that the corrosive aluminum foil that will form thin film of titanium oxide is at last inserted mass concentration, anodic oxidation is 80 minutes under the voltage of 150V, then 465 ℃ of thermal treatments after 6 minutes, insert once more in the above-mentioned ammonium dihydrogen phosphate, anodic oxidation got final product in 6 minutes under identical voltage.
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Families Citing this family (15)
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| CN101814378A (en) * | 2010-04-16 | 2010-08-25 | 厦门大学 | Method for preparing anodic composite film for aluminum electrolytic capacitor |
| CN102568858B (en) * | 2012-01-13 | 2013-11-06 | 西安交通大学 | Production method of high dielectric constant composite alumina film |
| 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 |
| CN105513802B (en) * | 2015-12-24 | 2018-02-06 | 南通海星电子股份有限公司 | A kind of manufacture method of the low-pressure chemical synthesis foil containing composite dielectric film |
| CN106065488B (en) * | 2016-05-19 | 2018-07-17 | 西安交通大学 | A method of preparing anode aluminium foil using positive negative pulse stuffing anodizing |
| CN107354498B (en) * | 2017-07-18 | 2019-04-30 | 丰宾电子（深圳）有限公司 | A kind of manufacturing method of the electrode foil for aluminum electrolytic capacitors of high pressure high capacity |
| CN107604416B (en) * | 2017-08-09 | 2019-05-03 | 聊城大学 | A kind of high dielectric composite anode oxide film preparation method of anode aluminium foil |
| CN107610935A (en) * | 2017-08-30 | 2018-01-19 | 丰宾电子（深圳）有限公司 | Electrode foil for aluminum electrolytic capacitors preparation method, electrode foil and aluminium electrolutic capacitor |
| CN110565140A (en) * | 2019-09-18 | 2019-12-13 | 南通海星电子股份有限公司 | Preparation method of high-dielectric-constant composite film aluminum foil |
| CN113161150A (en) * | 2021-04-22 | 2021-07-23 | 湖南艾华集团股份有限公司 | Preparation method of anode foil composite film of aluminum electrolytic capacitor |
| CN113462197B (en) * | 2021-06-30 | 2022-08-09 | 常熟世名化工科技有限公司 | Preparation method of titanium dioxide aqueous dispersion, product and application thereof |
| CN113718310A (en) * | 2021-08-09 | 2021-11-30 | 中南大学 | Preparation method of high-dielectric-constant composite anodic oxide film |
| CN114446667B (en) * | 2022-01-17 | 2023-09-08 | 南通海星电子股份有限公司 | Preparation method of high dielectric constant electrode foil |
| CN115172061B (en) * | 2022-08-02 | 2024-01-30 | 南通海星电子股份有限公司 | Preparation method of high-dielectric composite powder sintered foil |
| CN116092834B (en) * | 2023-03-31 | 2023-07-14 | 南通海星电子股份有限公司 | Preparation method of high-specific capacitance electrode foil |
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Assignee: Zhaoqing Huafeng Electronic Aluminum Foil Co., Ltd. Assignor: Xi'an Jiaotong University Contract record no.: 2011440000039 Denomination of invention: Titanium oxide/aluminum oxide high dielectric constant composite anode film preparation method Granted publication date: 20080130 License type: Common License Open date: 20060503 Record date: 20110120 |
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