CN103882506A - Additive for ultimate formation liquid of middle and high pressure formed foil and adding method thereof - Google Patents

Additive for ultimate formation liquid of middle and high pressure formed foil and adding method thereof Download PDF

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Publication number
CN103882506A
CN103882506A CN201210562426.7A CN201210562426A CN103882506A CN 103882506 A CN103882506 A CN 103882506A CN 201210562426 A CN201210562426 A CN 201210562426A CN 103882506 A CN103882506 A CN 103882506A
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Prior art keywords
additive
high pressure
salt
acid
forming liquid
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宋洪洲
陆宝琳
杨林桑
黄胜权
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Guangxi Hezhou Guidong Electronic Technology Co Ltd
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Guangxi Hezhou Guidong Electronic Technology Co Ltd
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Abstract

The invention discloses an additive for an ultimate formation liquid of middle and high pressure formed foil and an adding method thereof, the additive is a long-carbon-chain dicarboxylic acid or a salt thereof, and comprises one or more than one from azelaic acid, ammonium hydrogen azelate, sebacic acid and ammonium sebacate, and the additive content is 0.001-0.500wt%. According to the method by adding the additive into the ultimate formation liquid, hydration resistance of the middle and high pressure formed foil can be effectively improved, and the formed foil is more stable in performance.

Description

A kind of medium-high pressure chemical foil is additive and the addition means thereof of level forming liquid eventually
Technical field
The invention belongs to electronic material manufacturing technology field, be specifically related to a kind of medium-high pressure chemical foil additive and addition means thereof of level forming liquid eventually.
Background technology
At present, medium-high pressure chemical foil adopts three grades, level Four or Pyatyi to change into production conventionally, and level forming liquid is generally prepared by boric acid and salt thereof or ammoniacal liquor eventually.Adopt after the Waste Acid From Hua Cheng Foil hydration-treated that this eventually level forming liquid produces Tr(60 pressure rising time) large compared with the amplitude of ging up pressure rising time after long, long-time storage, thus affect the seasoned production of derived product aluminium electrolutic capacitor.Tr(60) be the technical indicator of stability after evaluation Waste Acid From Hua Cheng Foil hydration-treated.
Summary of the invention
The present invention overcomes the existing medium-high pressure chemical foil deficiency of level forming liquid eventually, provides a kind of and can improve water-fast additive and the addition means thereof that closes performance, makes the whole level of the medium-high pressure chemical foil forming liquid that Waste Acid From Hua Cheng Foil performance is more stable of Waste Acid From Hua Cheng Foil.
The present invention achieves the above object by the following technical programs: a kind of medium-high pressure chemical foil is the additive of level forming liquid eventually, described additive, for long carbochain di-carboxylic acid or its salt, comprises one or more in nonane diacid, nonane diacid hydrogen ammonium, sebacic acid, ammonium sebacate; Described additive level is 0.001~0.500wt%.
Described medium-high pressure chemical foil is the addition means of the additive of level forming liquid eventually, comprises the steps:
Middle high-pressure etched foil is boiled to processing in pure water, then carrying out I and II at the forming liquid that contains boric acid, citric acid and salt thereof changes into, then taking boric acid and salt thereof as main solute, add one or more in 0.001~0.500wt% nonane diacid, nonane diacid hydrogen ammonium, sebacic acid, ammonium sebacate forming liquids of level eventually that are additive to carry out the 20~40min that changes into of the third stage or third and fourth grade or third and fourth, Pyatyi; Heat-treat again, middle processing, repeatedly change into 3 times, aftertreatment.
Applicable Waste Acid From Hua Cheng Foil specification comprises 200~900Vf product.
Advantage of the present invention is:
In the immovable situation of forming liquid above, adding long carbochain di-carboxylic acid or its salt in level forming liquid eventually, after changing into processing, after medium-high pressure chemical foil hydration-treated pressure rising time Tr(60) shortened 4~12s, performance is more stable.
Embodiment
Below in conjunction with specific embodiment, technical scheme of the present invention is described in further detail, but embodiments of the present invention are not limited to this.
Embodiment 1
Middle pressure 200Vf changes into.Middle pressure etched foil boils in pure water processes 5min, then carry out at the forming liquid that contains boric acid, citric acid and salt thereof that one-level constant voltage 70V changes into 10min, secondary constant voltage 170V changes into 10min, then be main solute at boric acid and salt thereof, the forming liquid that adds 0.500wt% sebacic acid to make additive carries out third stage constant voltage 180V and changes into 20min.Heat-treat again, middle processing, repeatedly change into 3 times, aftertreatment.
The different forming liquids of level are eventually produced Waste Acid From Hua Cheng Foil and are detected data:
Table 1
Figure BDA00002631581200021
Find out from the experimental result of table 1, adopt the present invention to close rear pressure rising time of Tr(60 than the Waste Acid From Hua Cheng Foil of prior art water-fast) shorten 4s.
Embodiment 2
High pressure 530Vf changes into.High pressure etched foil boils in pure water processes 10min, then carry out at the forming liquid that contains boric acid, citric acid and salt thereof that one-level constant voltage 150V changes into 10min, secondary constant voltage 300V changes into 10min, be main solute at boric acid and salt thereof, the forming liquid that adds 0.05wt% nonane diacid to make additive carries out third stage constant voltage 450V and changes into 10min; Then be main solute at boric acid and salt thereof, the forming liquid that adds 0.03wt% nonane diacid hydrogen ammonium to make additive carries out fourth stage constant voltage 505V and changes into 25min; Heat-treat again, middle processing, repeatedly change into 3 times, aftertreatment.
Table 2
Find out from the experimental result of table 2, adopt the present invention to close rear pressure rising time of Tr(60 than the Waste Acid From Hua Cheng Foil of prior art water-fast) shorten 7s.
Embodiment 3
660Vf changes into.High pressure etched foil boils in the pure water of 95 DEG C processes 12min, then carry out at the forming liquid that contains boric acid, citric acid and salt thereof that one-level constant voltage 200V changes into 12min, secondary constant voltage 400V changes into 12min, be main solute at boric acid and salt thereof, the forming liquid that adds 0.03wt% nonane diacid to make additive carries out third stage constant voltage 600V and changes into 15min; Then be main solute at boric acid and salt thereof, the forming liquid that adds 0.01wt% nonane diacid hydrogen ammonium to make additive carries out fourth stage constant voltage 640V and changes into 30min; Heat-treat again, middle processing, repeatedly change into 3 min, aftertreatment.
Table 3
Figure BDA00002631581200031
Find out from the experimental result of table 3, adopt the present invention to close rear pressure rising time of Tr(60 than the Waste Acid From Hua Cheng Foil of prior art water-fast) shorten 10s.
Embodiment 4
900Vf changes into.High pressure etched foil boils in the pure water of 95 DEG C processes 15min, then carry out at the forming liquid that contains boric acid, citric acid and salt thereof that one-level constant voltage 240V changes into 20min, secondary constant voltage 480V changes into 20min, be main solute at boric acid and salt thereof, the forming liquid that adds 0.02wt% sebacic acid to make additive carries out third stage constant voltage 680V and changes into 30min; Then be main solute at boric acid and salt thereof, the forming liquid that adds 0.01wt% sebacic acid to make additive carries out fourth stage constant voltage 780V and changes into 30min; Then be main solute at boric acid and salt thereof, the forming liquid that adds 0.001wt ammonium sebacate to make additive carries out level V constant voltage 880V and changes into 40min; Heat-treat again, middle processing, repeatedly change into 3 min, aftertreatment.
Table 4
Figure BDA00002631581200032
Find out from the experimental result of table 4, adopt the present invention to close rear pressure rising time of Tr(60 than the Waste Acid From Hua Cheng Foil of prior art water-fast) shorten 12s.
Above-mentioned described specific embodiment is only to the explanation for example of the present invention's spirit, those skilled in the art can make various amendments to described specific embodiment, supplement or similar substituting, but can't depart from spirit of the present invention or the defined scope of appended claims.

Claims (2)

1. a medium-high pressure chemical foil additive for level forming liquid eventually, is characterized in that, described additive, for long carbochain di-carboxylic acid or its salt, comprises one or more in nonane diacid, nonane diacid hydrogen ammonium, sebacic acid, ammonium sebacate; Described additive level is 0.001~0.500wt%.
2. the medium-high pressure chemical foil according to claim 1 addition means of the additive of level forming liquid eventually, is characterized in that, comprises the steps:
Middle high-pressure etched foil is boiled to processing in pure water, then carrying out I and II at the forming liquid that contains boric acid, citric acid and salt thereof changes into, then taking boric acid and salt thereof as main solute, add one or more in 0.001~0.500wt% nonane diacid, nonane diacid hydrogen ammonium, sebacic acid, ammonium sebacate forming liquids of level eventually that are additive to carry out the 20~40min that changes into of the third stage or third and fourth grade or third and fourth, Pyatyi; Heat-treat again, middle processing, repeatedly change into 3 times, aftertreatment.
CN201210562426.7A 2012-12-21 2012-12-21 Additive for ultimate formation liquid of middle and high pressure formed foil and adding method thereof Pending CN103882506A (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105154952A (en) * 2015-09-01 2015-12-16 广西贺州市桂东电子科技有限责任公司 Formation method of ultrahigh-pressure electronic aluminum foil
CN105239128A (en) * 2015-09-01 2016-01-13 广西贺州市桂东电子科技有限责任公司 Ultrahigh pressure formed foil forming liquid and preparation method
CN113990667A (en) * 2021-10-27 2022-01-28 宝兴县剑锋制箔电子有限公司 Formation method of electrode foil

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CN1511326A (en) * 2001-01-15 2004-07-07 宇部兴产株式会社 Electrolysis solution for electrolytic capacitors
EP1826297A2 (en) * 2006-02-23 2007-08-29 Greatbatch Ltd. Anodizing electrolytes using a dual acid system for high voltage electrolytic capacitor anodes
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CN101819886A (en) * 2010-04-27 2010-09-01 四川中雅科技有限公司 Method for manufacturing electrode foil capable of preventing current jump during formation
CN101826397A (en) * 2010-04-27 2010-09-08 四川中雅科技有限公司 Five-stage manufacturing method of electrode foil for medium-high voltage aluminium electrolytic capacitor
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US3767541A (en) * 1971-06-29 1973-10-23 Gen Electric Anodized film for electrolytic capacitor and method for preparation thereof
JPH03126216A (en) * 1989-10-11 1991-05-29 Matsushita Electric Ind Co Ltd Manufacture of electrode foil for aluminum electrolytic capacitor
JPH0474406A (en) * 1990-07-16 1992-03-09 Matsushita Electric Ind Co Ltd Manufacture of electrode foil for aluminum electrolytic capacitor
US6197184B1 (en) * 1998-10-29 2001-03-06 Pacesetter, Inc. Method of producing high quality oxide for electrolytic capacitors
US6299752B1 (en) * 1999-03-10 2001-10-09 Pacesetter, Inc. Very high volt oxide formation of aluminum for electrolytic capacitors
JP2001135636A (en) * 1999-11-04 2001-05-18 Mitsubishi Chemicals Corp Chemical solution for forming metal oxide coating
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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105154952A (en) * 2015-09-01 2015-12-16 广西贺州市桂东电子科技有限责任公司 Formation method of ultrahigh-pressure electronic aluminum foil
CN105239128A (en) * 2015-09-01 2016-01-13 广西贺州市桂东电子科技有限责任公司 Ultrahigh pressure formed foil forming liquid and preparation method
CN105154952B (en) * 2015-09-01 2018-03-27 广西贺州市桂东电子科技有限责任公司 A kind of chemical synthesizing method of ultrahigh voltage electron aluminium foil
CN105239128B (en) * 2015-09-01 2018-03-30 广西贺州市桂东电子科技有限责任公司 A kind of super-pressure Waste Acid From Hua Cheng Foil forms liquid and compound method
CN113990667A (en) * 2021-10-27 2022-01-28 宝兴县剑锋制箔电子有限公司 Formation method of electrode foil

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Application publication date: 20140625