CN102709059B - Formation method for anode foil of intermediate-voltage aluminum electrolytic capacitor - Google Patents
Formation method for anode foil of intermediate-voltage aluminum electrolytic capacitor Download PDFInfo
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- CN102709059B CN102709059B CN201210188205.8A CN201210188205A CN102709059B CN 102709059 B CN102709059 B CN 102709059B CN 201210188205 A CN201210188205 A CN 201210188205A CN 102709059 B CN102709059 B CN 102709059B
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Abstract
The invention discloses a formation method for an anode foil of an intermediate-voltage aluminum electrolytic capacitor, and belongs to the technical field of manufacture of anode foils of aluminum electrolytic capacitors. According to the formation method for the anode foil of the intermediate-voltage aluminum electrolytic capacitor, ammonium adipate is adopted as four-stage formation electrolyte. The technical scheme is that: the method comprises the following steps of: performing three-stage formation by adopting a solution of ammonium adipate as electrolyte, performing the formation of a fourth stage by using a boric acid and ammonium dihydrogen phosphate, performing high-temperature treatment, performing treatment by using a phosphate solution, and performing drying to obtain the anode foil of the intermediate-voltage aluminum electrolytic capacitor. The ammonium adipate is adopted as the formation electrolyte, so that the obtained anode foil of the capacitor is high in specific capacity and high in hydration resistance, boosting time is shortened, and a Tr60 value is decreased.
Description
Technical field
The chemical synthesizing method of a kind of middle jewelling electrolytic capacitor anode aluminum foil of the present invention belongs to the manufacturing technology field of aluminum electrolysis capacitor anode foil.
Background technology
Currently available technology is normally in the reprocessing of chemical synthesis technology process, and in reprocessing tank liquor, add a certain amount of phosphoric acid class passivator, as phosphoric acid carries out chemical processing, namely be reach after maximum becomes voltage at Waste Acid From Hua Cheng Foil, inserted in phosphoric acid and soaked certain hour, in chemical processing process, phosphoric acid has dissolved a part of pellumina, generates phosphating coat.Except adopting phosphoric acid as passivating solution, generally also adopt boric acid and citric acid etc., or the salt of these acid, as electrolyte.The domestic research about chemical synthesis technology has report more, but with the aluminum electrolysis capacitor anode foil that existing method is produced, technically still can not meet the demands.
Summary of the invention
The present invention, in order to overcome the deficiencies in the prior art, provides a kind of ammonium adipate that adopts to be the middle jewelling electrolytic capacitor anode aluminum foil chemical synthesizing method of level Four electrolyte.
In order to solve the problems of the technologies described above, the technical solution used in the present invention is: a kind of chemical synthesizing method of middle jewelling electrolytic capacitor anode aluminum foil, carries out according to following steps:
(1) first the aluminium foil after electrolytic corrosion process is placed in temperature 95 DEG C and above pure water, soaks 5-12 minute; Then put into the aqueous solution that concentration is the ammonium adipate of 0.01-0.6wt%, formation voltage is 75-85V, current density is 90-120mA/cm
2, change into temperature and be 86-90 DEG C, change into time 10-20 minute, obtain one-level formed aluminum foil;
(2) described one-level formed aluminum foil is put into the aqueous solution that concentration is the ammonium adipate of 0.01-0.04wt%, formation voltage is 155-170V, current density is 90-120mA/cm
2, change into temperature and be 86-90 DEG C, change into time 10-20 minute, obtain secondary formed aluminum foil;
(3) described secondary formed aluminum foil is put into the aqueous solution that concentration is 0.01-0.04wt% ammonium adipate, formation voltage is 200-230V, current density is 90-120mA/cm
2, change into temperature and be 86-90 DEG C, change into time 10-20 minute, obtain three grades of formed aluminum foils;
(4) cleaned by described three grades of formed aluminum foil pure water, then change into the aqueous solution of 2-10wt% boric acid and 0.01-0.4wt% ammonium dihydrogen phosphate, formation voltage is 250-380V, current density is 90-120mA/cm
2, change into that temperature is 86-90 DEG C, the time of changing into is 15-50 minute; Be heat treatment 1-5 minute in the baking oven of 350-600 DEG C in temperature after the cleaning of taking-up pure water; Putting into concentration is that 0.01-0.4wt% ammonium dihydrogen phosphate changes into, and formation voltage is 250-380V, current density is 90-120mA/cm
2, change into that temperature is 86-90 DEG C, the time of changing into is 10-20 minute; Put into temperature 40-80 DEG C after the cleaning of taking-up pure water, concentration is process 2-10 minute in 1-10wt% phosphoric acid solution; Putting into concentration is again that 0.01-0.4wt% ammonium dihydrogen phosphate changes into, and formation voltage is 250-380V, current density is 90-120mA/cm
2, change into that temperature is 86-90 DEG C, the time of changing into is 10-20 minute; Take out and be placed in the baking oven heat treatment 1-5 minute that temperature is 350-600 DEG C; Putting into concentration is that 0.01-0.1wt% ammonium dihydrogen phosphate changes into, and formation voltage is 250-380V, current density is 90-120mA/cm
2, change into that temperature is 86-90 DEG C, the time of changing into is 10-20 minute; Finally putting into temperature 20-60 DEG C of concentration is that 1-10wt% phosphoric acid solution processes 2-10 minute and cleans post-drying with pure water, namely obtains middle jewelling electrolytic capacitor anode aluminum foil.
The beneficial effect that the present invention compared with prior art has is: the present invention adopts ammonium adipate as electrolyte, obtains the anode foil of capacitor of Fabrication of High Specific Capacitance, and resistance to hydration performance is good, reduces pressure rising time, and Tr60 value reduces.
Embodiment
Below in conjunction with specific embodiment, the invention will be further described.
Embodiment 1
A chemical synthesizing method for middle jewelling electrolytic capacitor anode aluminum foil, carries out according to following steps:
(1) first the aluminium foil after electrolytic corrosion process is placed in temperature 95 DEG C and above pure water, soaks 5 minutes; Then put into the aqueous solution that concentration is the ammonium adipate of 0.6wt%, formation voltage is 75V, current density is 90mA/cm
2, change into temperature and be 90 DEG C, change into 20 minutes time, obtain one-level formed aluminum foil;
(2) described one-level formed aluminum foil is put into the aqueous solution that concentration is the ammonium adipate of 0.04wt%, formation voltage is 170V, current density is 90mA/cm
2, change into temperature and be 90 DEG C, change into 20 minutes time, obtain secondary formed aluminum foil;
(3) described secondary formed aluminum foil is put into the aqueous solution that concentration is 0.04wt% ammonium adipate, formation voltage is 230V, current density is 90mA/cm
2, change into temperature and be 90 DEG C, change into 20 minutes time, obtain three grades of formed aluminum foils;
(4) cleaned by described three grades of formed aluminum foil pure water, then change into the aqueous solution of 10wt% boric acid and 0.4wt% ammonium dihydrogen phosphate, formation voltage is 380V, current density is 90mA/cm
2, change into that temperature is 90 DEG C, the time of changing into is 50 minutes; Be heat treatment 5 minutes in the baking oven of 600 DEG C in temperature after the cleaning of taking-up pure water; Putting into concentration is that 0.4wt% ammonium dihydrogen phosphate changes into, and formation voltage is 380V, current density is 90mA/cm
2, change into that temperature is 90 DEG C, the time of changing into is 20 minutes; Put into temperature 80 DEG C after the cleaning of taking-up pure water, concentration is process 10 minutes in 10wt% phosphoric acid solution; Putting into concentration is again that 0.4wt% ammonium dihydrogen phosphate changes into, and formation voltage is 380V, current density is 90mA/cm
2, change into that temperature is 90 DEG C, the time of changing into is 20 minutes; Take out and be placed in the baking oven heat treatment 5 minutes that temperature is 600 DEG C; Putting into concentration is that 0.1wt% ammonium dihydrogen phosphate changes into, and formation voltage is 380V, current density is 90mA/cm
2, change into that temperature is 90 DEG C, the time of changing into is 20 minutes; Finally putting into temperature 60 C concentration is that the process of 10wt% phosphoric acid solution cleans post-drying with pure water in 10 minutes, namely obtains middle jewelling electrolytic capacitor anode aluminum foil.Obtained middle jewelling electrolytic capacitor anode aluminum foil pressure rising time is 92 seconds, and Tr60 is 10 seconds.
Embodiment 2
A chemical synthesizing method for middle jewelling electrolytic capacitor anode aluminum foil, carries out according to following steps:
(1) first the aluminium foil after electrolytic corrosion process is placed in temperature 95 DEG C and above pure water, soaks 12 minutes; Then put into the aqueous solution that concentration is the ammonium adipate of 0.01wt%, formation voltage is 85V, current density is 120mA/cm
2, change into temperature and be 86 DEG C, change into 10 minutes time, obtain one-level formed aluminum foil;
(2) described one-level formed aluminum foil is put into the aqueous solution that concentration is the ammonium adipate of 0.01wt%, formation voltage is 155V, current density is 120mA/cm
2, change into temperature and be 86 DEG C, change into 10 minutes time, obtain secondary formed aluminum foil;
(3) described secondary formed aluminum foil is put into the aqueous solution that concentration is 0.01wt% ammonium adipate, formation voltage is 200V, current density is 120mA/cm
2, change into temperature and be 86 DEG C, change into 10 minutes time, obtain three grades of formed aluminum foils;
(4) cleaned by described three grades of formed aluminum foil pure water, then change into the aqueous solution of 2wt% boric acid and 0.01wt% ammonium dihydrogen phosphate, formation voltage is 250V, current density is 120mA/cm
2, change into that temperature is 86 DEG C, the time of changing into is 15 minutes; Be heat treatment 1 minute in the baking oven of 350 DEG C in temperature after the cleaning of taking-up pure water; Putting into concentration is that 0.01wt% ammonium dihydrogen phosphate changes into, and formation voltage is 250V, current density is 120mA/cm
2, change into that temperature is 86 DEG C, the time of changing into is 10 minutes; Put into temperature 40 DEG C after the cleaning of taking-up pure water, concentration is process 2 minutes in 1wt% phosphoric acid solution; Putting into concentration is again that 0.01wt% ammonium dihydrogen phosphate changes into, and formation voltage is 250V, current density is 120mA/cm
2, change into that temperature is 86 DEG C, the time of changing into is 10 minutes; Take out and be placed in the baking oven heat treatment 1 minute that temperature is 350 DEG C; Putting into concentration is that 0.01wt% ammonium dihydrogen phosphate changes into, and formation voltage is 250V, current density is 120mA/cm
2, change into that temperature is 86 DEG C, the time of changing into is 10 minutes; Finally putting into temperature 20 DEG C of concentration is that the process of 1wt% phosphoric acid solution cleans post-drying with pure water in 2 minutes, namely obtains middle jewelling electrolytic capacitor anode aluminum foil.Obtained middle jewelling electrolytic capacitor anode aluminum foil pressure rising time is 85 seconds, and Tr60 is 9 seconds.
Embodiment 3
A chemical synthesizing method for middle jewelling electrolytic capacitor anode aluminum foil, carries out according to following steps:
(1) first the aluminium foil after electrolytic corrosion process is placed in temperature 95 DEG C and above pure water, soaks 10 minutes; Then put into the aqueous solution that concentration is the ammonium adipate of 0.2wt%, formation voltage is 80V, current density is 100mA/cm
2, change into temperature and be 88 DEG C, change into 16 minutes time, obtain one-level formed aluminum foil;
(2) described one-level formed aluminum foil is put into the aqueous solution that concentration is the ammonium adipate of 0.02wt%, formation voltage is 160V, current density is 100mA/cm
2, change into temperature and be 88 DEG C, change into 16 minutes time, obtain secondary formed aluminum foil;
(3) described secondary formed aluminum foil is put into the aqueous solution that concentration is 0.02wt% ammonium adipate, formation voltage is 220V, current density is 100mA/cm
2, change into temperature and be 88 DEG C, change into 16 minutes time, obtain three grades of formed aluminum foils;
(4) cleaned by described three grades of formed aluminum foil pure water, then change into the aqueous solution of 6wt% boric acid and 0.1wt% ammonium dihydrogen phosphate, formation voltage is 300V, current density is 100mA/cm
2, change into that temperature is 88 DEG C, the time of changing into is 30 minutes; Be heat treatment 3 minutes in the baking oven of 500 DEG C in temperature after the cleaning of taking-up pure water; Putting into concentration is that 0.15wt% ammonium dihydrogen phosphate changes into, and formation voltage is 300V, current density is 100mA/cm
2, change into that temperature is 88 DEG C, the time of changing into is 15 minutes; Put into temperature 60 C after the cleaning of taking-up pure water, concentration is process 7 minutes in 5wt% phosphoric acid solution; Putting into concentration is again that 0.2wt% ammonium dihydrogen phosphate changes into, and formation voltage is 300V, current density is 100mA/cm
2, change into that temperature is 88 DEG C, the time of changing into is 16 minutes; Take out and be placed in the baking oven heat treatment 4 minutes that temperature is 500 DEG C; Putting into concentration is that 0.05wt% ammonium dihydrogen phosphate changes into, and formation voltage is 300V, current density is 100mA/cm
2, change into that temperature is 88 DEG C, the time of changing into is 16 minutes; Finally putting into temperature 50 C concentration is that the process of 7wt% phosphoric acid solution cleans post-drying with pure water in 7 minutes, namely obtains middle jewelling electrolytic capacitor anode aluminum foil.Obtained middle jewelling electrolytic capacitor anode aluminum foil pressure rising time is 87 seconds, and Tr60 is 8 seconds.
The present invention can summarize with other the concrete form without prejudice to spirit of the present invention or principal character.Therefore, no matter from that, above-mentioned embodiment of the present invention all can only be thought explanation of the present invention and can not limit invention, claims indicate scope of the present invention, and scope of the present invention is not pointed out in above-mentioned explanation, therefore, any change in the implication suitable with claims of the present invention and scope, all should think to be included in the scope of claims.
Claims (1)
1. a chemical synthesizing method for jewelling electrolytic capacitor anode aluminum foil in, is characterized in that carrying out according to following steps:
(1) first the aluminium foil after electrolytic corrosion process is placed in temperature 95 DEG C and above pure water, soaks 5-12 minute; Then put into the aqueous solution that concentration is the ammonium adipate of 0.01-0.6wt%, formation voltage is 75-85V, current density is 90-120mA/cm
2, change into temperature and be 86-90 DEG C, change into time 10-20 minute, obtain one-level formed aluminum foil;
(2) described one-level formed aluminum foil is put into the aqueous solution that concentration is the ammonium adipate of 0.01-0.04wt%, formation voltage is 155-170V, current density is 90-120mA/cm
2, change into temperature and be 86-90 DEG C, change into time 10-20 minute, obtain secondary formed aluminum foil;
(3) described secondary formed aluminum foil is put into the aqueous solution that concentration is 0.01-0.04wt% ammonium adipate, formation voltage is 200-230V, current density is 90-120mA/cm
2, change into temperature and be 86-90 DEG C, change into time 10-20 minute, obtain three grades of formed aluminum foils;
(4) cleaned by described three grades of formed aluminum foil pure water, then change into the aqueous solution of 2-10wt% boric acid and 0.01-0.4wt% ammonium dihydrogen phosphate, formation voltage is 250-380V, current density is 90-120mA/cm
2, change into that temperature is 86-90 DEG C, the time of changing into is 15-50 minute; Be heat treatment 1-5 minute in the baking oven of 350-600 DEG C in temperature after the cleaning of taking-up pure water; Putting into concentration is that 0.01-0.4wt% ammonium dihydrogen phosphate changes into, and formation voltage is 250-380V, current density is 90-120mA/cm
2, change into that temperature is 86-90 DEG C, the time of changing into is 10-20 minute; Put into temperature 40-80 DEG C after the cleaning of taking-up pure water, concentration is process 2-10 minute in 1-10wt% phosphoric acid solution; Putting into concentration is again that 0.01-0.4wt% ammonium dihydrogen phosphate changes into, and formation voltage is 250-380V, current density is 90-120mA/cm
2, change into that temperature is 86-90 DEG C, the time of changing into is 10-20 minute; Take out and be placed in the baking oven heat treatment 1-5 minute that temperature is 350-600 DEG C; Putting into concentration is that 0.01-0.1wt% ammonium dihydrogen phosphate changes into, and formation voltage is 250-380V, current density is 90-120mA/cm
2, change into that temperature is 86-90 DEG C, the time of changing into is 10-20 minute; Finally putting into temperature 20-60 DEG C of concentration is that 1-10wt% phosphoric acid solution processes 2-10 minute and cleans post-drying with pure water, namely obtains middle jewelling electrolytic capacitor anode aluminum foil.
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| CN201210188205.8A CN102709059B (en) | 2012-06-09 | 2012-06-09 | Formation method for anode foil of intermediate-voltage aluminum electrolytic capacitor |
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| CN201210188205.8A CN102709059B (en) | 2012-06-09 | 2012-06-09 | Formation method for anode foil of intermediate-voltage aluminum electrolytic capacitor |
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| CN102709059B true CN102709059B (en) | 2015-06-03 |
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Families Citing this family (12)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103160902B (en) * | 2012-12-13 | 2015-12-23 | 宝兴县剑锋制箔电子有限公司 | Middle-high voltage electrode foil 5 sections changes into 2 grades of liquid feedback production methods |
| CN103227053B (en) * | 2013-05-15 | 2015-08-19 | 南通海星电子股份有限公司 | Reduce the formation processing method of medium-high pressure chemical foil leakage current |
| CN104711663B (en) * | 2013-12-15 | 2017-05-31 | 江苏荣生电子有限公司 | It is a kind of to use seven grades of middle-high voltage electrode foil manufacture methods of different hair engaging aperture conditions |
| CN104611747B (en) * | 2014-12-31 | 2017-06-06 | 日丰（清远）电子有限公司 | A kind of production method of solid-state capacitor aluminum foil special |
| CN104966615A (en) * | 2015-07-13 | 2015-10-07 | 南通南铭电子有限公司 | Manufacturing method for solid-state capacitor lead-out wire |
| CN107452518B (en) * | 2017-08-10 | 2019-02-12 | 佛山科学技术学院 | Reduce the chemical synthesizing method of medium-high pressure chemical foil leakage current |
| CN108376611A (en) * | 2017-12-29 | 2018-08-07 | 广西贺州市桂东电子科技有限责任公司 | A kind of production method of no foil ash medium-high pressure chemical foil |
| CN109628979A (en) * | 2018-12-20 | 2019-04-16 | 宝兴县华锋储能材料有限公司 | A kind of manufacturing method of extremely low pressure Fabrication of High Specific Capacitance Waste Acid From Hua Cheng Foil |
| CN110938853A (en) * | 2019-11-27 | 2020-03-31 | 新疆众和股份有限公司 | High specific volume electrode foil electrolyte, composition thereof and preparation method of electrode foil |
| CN111863453B (en) * | 2020-06-29 | 2021-09-03 | 凯普松电子科技(包头)有限公司 | Manufacturing method of formation aluminum foil for high-stability aluminum electrolytic capacitor |
| CN112103084B (en) * | 2020-08-17 | 2021-10-15 | 新疆众和股份有限公司 | Anode foil and preparation method thereof |
| CN113862750A (en) * | 2021-08-23 | 2021-12-31 | 南通南辉电子材料股份有限公司 | Manufacturing method of electrode foil for special capacitor of electric automobile |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101593630A (en) * | 2008-05-26 | 2009-12-02 | 南通海一电子有限公司 | Improve the manufacture method of water resisting property of low voltage electrode foil |
| CN101964257A (en) * | 2010-11-04 | 2011-02-02 | 南通华冠电子科技有限公司 | Ultrahigh-pressure anode aluminum foil formation method |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101593630A (en) * | 2008-05-26 | 2009-12-02 | 南通海一电子有限公司 | Improve the manufacture method of water resisting property of low voltage electrode foil |
| CN101964257A (en) * | 2010-11-04 | 2011-02-02 | 南通华冠电子科技有限公司 | Ultrahigh-pressure anode aluminum foil formation method |
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