CN101221855A - Method for manufacturing formed foil used for medium-high pressure aluminum electrolytic capacitor - Google Patents
Method for manufacturing formed foil used for medium-high pressure aluminum electrolytic capacitor Download PDFInfo
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Abstract
The invention relates to a manufacturing method for formed foil used in a middle and high pressure aluminum electrolytic capacitor; the invention includes six formations and adjusts two corresponding high temperature treatment processes and corresponding additional processes; compared with the pure boric acid formation process, the specific volume conversion rate and the bending conversion rate of the invention are greatly improved, thereby when the aluminum foil acquired in the invention is used to make the formed foil for the middle and high pressure aluminum electrolytic capacitor, the effect of improving the specific volume conversion rate and the bending conversion rate can be achieved.
Description
Technical field
The present invention relates to the manufacture method of capacitor electric pole foil, be particularly useful for the manufacture method of mesohigh capacitor electric pole foil.
Background technology
Medium-high voltage aluminum electrolytic capacitor generally adopts pure boric acid technology with the manufacture method that changes into paper tinsel, specific as follows: the excessive erosion of learning from else's experience, the purity dipping that is 99.99% aluminium foil in the pure water of (90～100) ℃ 10 minutes, taking-up places the aqueous solution of the boric acid of 3wt%, in temperature is that 85 ℃, current density are under the condition of 50mA/cm2, formation voltage 170V, changed into 10 minutes, and took out washing; Placing with one-level and change into liquid, is that 85 ℃, current density are under the condition of 50mA/cm2, formation voltage 300V in temperature, changes into 10 minutes, takes out washing; Placing the aqueous solution of the boric acid of 4wt%, is that 85 ℃, current density are under the condition of 50mA/cm2, formation voltage 455V in temperature, changes into 10 minutes, takes out washing; Placing the aqueous solution of the boric acid of 5wt%, is that 85 ℃, current density are under the condition of 50mA/cm2, formation voltage 530V in temperature, changes into 30 minutes, takes out washing, through 530 ℃ of heat treatments 3 minutes; Placing the aqueous solution of the boric acid of 5wt%, is that 85 ℃, current density are under the condition of 50mA/cm2, formation voltage 530V in temperature, changes into 10 minutes, takes out washing, handles 8～10 minutes down for 60 ℃ through the 5wt% phosphoric acid solution; Placing the aqueous solution of the boric acid of 5wt%, is that 85 ℃, current density are under the condition of 50mA/cm2, formation voltage 530V in temperature, changes into 10 minutes, takes out washing, through 530 ℃ of heat treatments 3 minutes; Placing the aqueous solution of the boric acid of 5wt%, is that 85 ℃, current density are under the condition of 50mA/cm2, formation voltage 530V in temperature, changes into 10 minutes, takes out washing, oven dry.This technology specific volume conversion ratio is lower, and the bending conversion ratio is general.
Summary of the invention
The invention solves the above-mentioned technical problem of existing in prior technology, provide a kind of make change into the good medium-high voltage aluminum electrolytic capacitor of paper tinsel specific volume conversion ratio height, bending conversion ratio with the nitration mixture manufacture method that changes into paper tinsel.
Above-mentioned technical purpose of the present invention solves by the following technical programs: a kind of medium-high voltage aluminum electrolytic capacitor manufacture method that changes into paper tinsel may further comprise the steps with this:
Dipping: the excessive erosion of learning from else's experience, purity is that aluminium foil more than 99.9% flooded in 90～100 ℃ water 5～15 minutes;
Once change into: taking out the aluminium foil soak behind the pool and place the boric acid that contains 0.1～3wt%, the adipic acid of 0.1～6wt% and the ammonium adipate aqueous solution of 0.1～1wt%, is that 75～90 ℃, current density are 45～55mA/cm in temperature
2, formation voltage 295～305V condition under, changed into 15～30 minutes;
Secondary changes into: the aluminium foil after will once changing into places the boric acid that contains 0.1～4wt%, the adipic acid of 0.1～4wt% and the ammonium adipate aqueous solution of 0.02～0.5wt%, is that 80～90 ℃, current density are 45～55mA/cm in temperature
2, formation voltage 455～465V condition under, changed into 5～15 minutes;
Change into for three times: the aluminium foil after secondary is changed into places the boric acid that contains 0.2～8wt%, the citric acid of 0.01～0.5wt% and the ammonium pentaborate aqueous solution of 0.04～0.2wt%, is that 80～90 ℃, current density are 45～55mA/cm in temperature
2, formation voltage 525～535V condition under, changed into 20～40 minutes;
High-temperature process: the aluminium foil after three times changed into was in 450～550 ℃ of high-temperature process 2～6 minutes;
Change into for four times: the aluminium foil after the high-temperature process is placed the boric acid that contains 0.2～8wt% and the ammonium pentaborate aqueous solution of 0.02～0.1wt%, is 45～55mA/cm in 80～90 ℃ of temperature, current density
2, formation voltage 525～535V condition under, changed into 5～15 minutes;
Acid treatment once more: the aluminium foil after three times changed into was handled 2～10 minutes down at 40～60 ℃ through 1～8wt% phosphoric acid solution;
Change into for five times: will be once more aluminium foil after the acid treatment place the boric acid that contains 0.2～8wt% and the ammonium pentaborate aqueous solution of 0.02～0.1wt%, be 45～55mA/cm in 80～90 ℃ of temperature, current density
2, formation voltage 525～535V condition under, changed into 5～15 minutes;
High-temperature process once more: the aluminium foil after five times changed into was through 495～505 ℃ of high-temperature process 2～6 minutes;
Change into for six times: will be once more aluminium foil after the high-temperature process place the boric acid that contains 0.2～8wt% and the ammonium pentaborate aqueous solution of 0.02～0.1wt%, be 45～55mA/cm in 80～90 ℃ of temperature, current density
2, formation voltage 525～535V condition under, changed into 5～15 minutes;
Reprocessing: the aluminium foil after six times changed into through the phosphorous ammonium salt solution of 2～8wt% 30～60 ℃ handle 2～10 minutes down after oven dry.
Phosphorous ammonium salt refers to ammonium hydrogen phosphate or ammonium hypophosphite etc. in the treatment fluid wherein.
As preferentially, change into for three times and high-temperature process between also have acid treatment step: the aluminium foil after three times are changed into was handled 2～10 minutes down at 40～60 ℃ through the phosphoric acid solution of 1～8wt%.
Each time changed into the adjusting that the electrolyte electricity leads adopt corresponding ammonium salt, as ammonium adipate or ammonium pentaborate, rather than ammoniacal liquor.
The present invention compares with above-mentioned pure boric acid chemical synthesis technology, and its specific volume conversion ratio and bending conversion ratio all are greatly improved, and be specifically as shown in table 1.
The performance comparison sheet of table 1 the present invention and boric acid chemical synthesis technology:
| The specific volume conversion ratio | The bending conversion ratio | |
| Pure boric acid technology | 102％ | 50％ |
| The present invention's (nitration mixture technology) | 113％ | 80％ |
Embodiment
Embodiment 1: the excessive erosion of learning from else's experience, the purity dipping that is 99.99% aluminium foil in the pure water of (90～100) ℃ 5 minutes, taking-up places the boric acid of 0.1wt%, the adipic acid of 0.1wt% and the ammonium adipate aqueous solution of 0.1wt%, is that 75 ℃, current density are 50mA/cm in temperature
2, formation voltage 300V condition under, changed into 15 minutes, take out washing; Placing the boric acid of 0.1wt%, the adipic acid of 0.1wt% and the ammonium adipate aqueous solution of 0.02wt%, is that 80 ℃, current density are 50mA/cm in temperature
2, formation voltage 460V condition under, changed into 5 minutes, take out washing; Placing the boric acid of 0.2wt%, the citric acid of 0.01wt% and the ammonium pentaborate aqueous solution of 0.04wt%, is that 80 ℃, current density are 50mA/cm in temperature
2, formation voltage 530V condition under, changed into 20 minutes, take out, handled 10 minutes 500 ℃ of high-temperature process 2 minutes down at 40 ℃ through the phosphoric acid solution of 1wt%; Placing the boric acid of 0.2wt% and the ammonium pentaborate aqueous solution of 0.02wt%, is that 85 ℃, current density are 50mA/cm in temperature
2, formation voltage 530V condition under, changed into 10 minutes, take out, handled 10 minutes down at 40 ℃ through the 1wt% phosphoric acid solution; Placing the boric acid of 0.2wt% and the ammonium pentaborate aqueous solution of 0.02wt% again, is that 85 ℃, current density are 50mA/cm in temperature
2, formation voltage 530V condition under, changed into 10 minutes, take out, through 500 ℃ of high-temperature process 2 minutes; Placing the boric acid of 0.2wt% and the ammonium pentaborate aqueous solution of 0.02wt% again, is that 85 ℃, current density are 50mA/cm in temperature
2, formation voltage 530V condition under, changed into 10 minutes, take out, handled 10 minutes oven dry down at 30 ℃ through the 2wt% ammonium dihydrogen phosphate.
Embodiment 2: the excessive erosion of learning from else's experience, the purity dipping that is 99.99% aluminium foil in the pure water of (90～100) ℃ 15 minutes, taking-up places the boric acid of 3wt%, the adipic acid of 6wt% and the ammonium adipate aqueous solution of 1wt%, is that 85 ℃, current density are 50mA/cm in temperature
2, formation voltage 300V condition under, changed into 25 minutes, take out washing; Placing the boric acid of 4wt%, the adipic acid of 4wt% and the ammonium adipate aqueous solution of 0.5wt%, is that 80 ℃, current density are 50mA/cm in temperature
2, formation voltage 460V condition under, changed into 5 minutes, take out washing; Placing the boric acid of 8wt%, the citric acid of 0.5wt% and the ammonium pentaborate aqueous solution of 0.2wt%, is that 80 ℃, current density are 50mA/cm in temperature
2, formation voltage 530V condition under, changed into 30 minutes, take out, handled 2 minutes 500 ℃ of high-temperature process 6 minutes down at 60 ℃ through the phosphoric acid solution of 8wt%; Placing the boric acid of 8wt% and the ammonium pentaborate aqueous solution of 0.1wt%, is that 85 ℃, current density are 50mA/cm in temperature
2, formation voltage 530V condition under, changed into 10 minutes, take out, handled 2 minutes down at 60 ℃ through the 8wt% phosphoric acid solution; Placing the boric acid of 8wt% and the ammonium pentaborate aqueous solution of 0.1wt% again, is that 85 ℃, current density are 50mA/cm in temperature
2, formation voltage 530V condition under, changed into 10 minutes, take out, through 500 ℃ of high-temperature process 6 minutes; Placing the boric acid of 8wt% and the ammonium pentaborate aqueous solution of 0.1wt% again, is that 85 ℃, current density are 50mA/cm in temperature
2, formation voltage 530V condition under, changed into 10 minutes, take out, handled 2 minutes oven dry down at 60 ℃ through the 8wt% ammonium dihydrogen phosphate.
Embodiment 3: the excessive erosion of learning from else's experience, the purity dipping that is 99.99% aluminium foil in the pure water of (90～100) ℃ 15 minutes, taking-up places the boric acid of 0.5wt%, the adipic acid of 0.5wt% and the ammonium adipate aqueous solution of 0.5wt%, is that 80 ℃, current density are 50mA/cm in temperature
2, formation voltage 300V condition under, changed into 20 minutes, take out washing; Placing the boric acid of 1wt%, the adipic acid of 0.8wt% and the ammonium adipate aqueous solution of 0.2wt%, is that 80 ℃, current density are 50mA/cm in temperature
2, formation voltage 460V condition under, changed into 8 minutes, take out washing; Placing the boric acid of 2wt%, the citric acid of 0.1wt% and the ammonium pentaborate aqueous solution of 0.1wt%, is that 80 ℃, current density are 50mA/cm in temperature
2, formation voltage 530V condition under, changed into 30 minutes, take out, handled 4 minutes 500 ℃ of high-temperature process 3 minutes down at 50 ℃ through the phosphoric acid solution of 4wt%; Placing the boric acid of 2wt% and the ammonium pentaborate aqueous solution of 0.05wt%, is that 85 ℃, current density are 50mA/cm in temperature
2, formation voltage 530V condition under, changed into 10 minutes, take out, handled 4 minutes down at 50 ℃ through the 4wt% phosphoric acid solution; Placing the boric acid of 2wt% and the ammonium pentaborate aqueous solution of 0.05wt% again, is that 85 ℃, current density are 50mA/cm in temperature
2, formation voltage 530V condition under, changed into 10 minutes, take out, through 500 ℃ of high-temperature process 3 minutes; Placing the boric acid of 2wt% and the ammonium pentaborate aqueous solution of 0.05wt% again, is that 85 ℃, current density are 50mA/cm in temperature
2, formation voltage 530V condition under, changed into 10 minutes, take out, handled 4 minutes oven dry down at 50 ℃ through the 5wt% ammonium dihydrogen phosphate.
Embodiment 4: the excessive erosion of learning from else's experience, the purity dipping that is 99.99% aluminium foil in the pure water of (90～100) ℃ 10 minutes, taking-up places the boric acid of 0.2wt%, the adipic acid of 0.2wt% and the ammonium adipate aqueous solution of 0.2wt%, is that 85 ℃, current density are 50mA/cm in temperature
2, formation voltage 300V condition under, changed into 15 minutes, take out washing; Placing the boric acid of 3wt%, the adipic acid of 3wt% and the ammonium adipate aqueous solution of 0.1wt%, is that 80 ℃, current density are 50mA/cm in temperature
2, formation voltage 460V condition under, changed into 8 minutes, take out washing; Placing the boric acid of 8wt%, the citric acid of 0.3wt% and the ammonium pentaborate aqueous solution of 0.15wt%, is that 85 ℃, current density are 50mA/cm in temperature
2, formation voltage 530V condition under, changed into 30 minutes, take out, handled 8 minutes 500 ℃ of high-temperature process 4 minutes down at 40 ℃ through the phosphoric acid solution of 2wt%; Placing the boric acid of 5wt% and the ammonium pentaborate aqueous solution of 0.1wt%, is that 85 ℃, current density are 50mA/cm in temperature
2, formation voltage 530V condition under, changed into 10 minutes, take out, handled 8 minutes down at 40 ℃ through the 2wt% phosphoric acid solution; Placing the boric acid of 5wt% and the ammonium pentaborate aqueous solution of 0.1wt% again, is that 85 ℃, current density are 50mA/cm in temperature
2, formation voltage 530V condition under, changed into 10 minutes, take out, through 500 ℃ of high-temperature process 3 minutes; Placing the boric acid of 5wt% and the ammonium pentaborate aqueous solution of 0.1wt% again, is that 85 ℃, current density are 50mA/cm in temperature
2, formation voltage 530V condition under, changed into 10 minutes, take out, handled 4 minutes oven dry down at 50 ℃ through 3wt% ortho phosphorous acid ammonium salt solution.
Claims (4)
1. a medium-high voltage aluminum electrolytic capacitor may further comprise the steps with this with the manufacture method that changes into paper tinsel:
Dipping: the excessive erosion of learning from else's experience, purity is that aluminium foil more than 99.9% flooded in 90～100 ℃ water 5～15 minutes;
Once change into: taking out the aluminium foil soak behind the pool and place the boric acid that contains 0.1～3wt%, the adipic acid of 0.1～6wt% and the ammonium adipate aqueous solution of 0.1～1wt%, is that 75～90 ℃, current density are 45～55mA/cm in temperature
2, formation voltage 295～305V condition under, changed into 15～30 minutes;
Secondary changes into: the aluminium foil after will once changing into places the boric acid that contains 0.1～4wt%, the adipic acid of 0.1～4wt% and the ammonium adipate aqueous solution of 0.02～0.5wt%, is that 80～90 ℃, current density are 45～55mA/cm in temperature
2, formation voltage 455～465V condition under, changed into 5～15 minutes;
Change into for three times: the aluminium foil after secondary is changed into places the boric acid that contains 0.2～8wt%, the citric acid of 0.01～0.5wt% and the ammonium pentaborate aqueous solution of 0.04～0.2wt%, is that 80～90 ℃, current density are 45～55mA/cm in temperature
2, formation voltage 525～535V condition under, changed into 20～40 minutes;
High-temperature process: with aluminium foil in 450～550 ℃ of high-temperature process 2～6 minutes;
Change into for four times: the aluminium foil after the high-temperature process is placed the boric acid that contains 0.2～8wt% and the ammonium pentaborate aqueous solution of 0.02～0.1wt%, is 45～55mA/cm in 80～90 ℃ of temperature, current density
2, formation voltage 525～535V condition under, changed into 5～15 minutes;
Acid treatment: the aluminium foil after three times changed into was handled 2～10 minutes down at 40～60 ℃ through 1～8wt% phosphoric acid solution;
Change into for five times: will be once more aluminium foil after the acid treatment place the boric acid that contains 0.2～8wt% and the ammonium pentaborate aqueous solution of 0.02～0.1wt%, be 45～55mA/cm in 80～90 ℃ of temperature, current density
2, formation voltage 525～535V condition under, changed into 5～1 5 minutes;
High-temperature process once more: the aluminium foil after five times changed into was through 495～505 ℃ of high-temperature process 2～6 minutes;
Change into for six times: will be once more aluminium foil after the high-temperature process place the boric acid that contains 0.2～8wt% and the ammonium pentaborate aqueous solution of 0.02～0.1wt%, be 45～55mA/cm in 80～90 ℃ of temperature, current density
2, formation voltage 525～535V condition under, changed into 5～15 minutes;
Reprocessing: the aluminium foil after six times changed into through the phosphorous ammonium salt solution of 2～8wt% 30～60 ℃ handle 2～10 minutes down after oven dry.
2. medium-high voltage aluminum electrolytic capacitor according to claim 1 is characterized in that with the manufacture method that changes into paper tinsel ammonium salt phosphorous in the treatment fluid refers to ammonium hydrogen phosphate or ammonium hypophosphite etc.
3. medium-high voltage aluminum electrolytic capacitor according to claim 1 is with the manufacture method that changes into paper tinsel, its feature: each time changed into the adjusting that the electrolyte electricity leads adopt corresponding ammonium salt.
4. medium-high voltage aluminum electrolytic capacitor according to claim 1 is characterized in that with the manufacture method that changes into paper tinsel: change into for three times and high temperature processing step between acid treatment step is arranged: the aluminium foil after being about to change into for three times was handled 2～10 minutes down at 40～60 ℃ through the phosphoric acid solution of 1～8wt%.
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| CN2007101943173A CN101221855B (en) | 2007-12-14 | 2007-12-14 | Method for manufacturing formed foil used for medium-high pressure aluminum electrolytic capacitor |
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| CN2007101943173A CN101221855B (en) | 2007-12-14 | 2007-12-14 | Method for manufacturing formed foil used for medium-high pressure aluminum electrolytic capacitor |
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| CN101221855A true CN101221855A (en) | 2008-07-16 |
| CN101221855B CN101221855B (en) | 2010-06-02 |
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| CN101777432A (en) * | 2010-03-23 | 2010-07-14 | 扬州宏远电子有限公司 | Forming process of anode foils for extra-high voltage aluminium electrolytic capacitors |
| CN102610390A (en) * | 2011-01-20 | 2012-07-25 | 严民 | Method for forming ultrahigh-voltage anode foil for aluminum electrolytic capacitors |
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| CN102610390B (en) * | 2011-01-20 | 2014-02-19 | 严民 | Method for forming ultrahigh-voltage anode foil for aluminum electrolytic capacitors |
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