CN113611536A - Manufacturing method for reducing foil dust of low-voltage electrode foil - Google Patents

Manufacturing method for reducing foil dust of low-voltage electrode foil Download PDF

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Publication number
CN113611536A
CN113611536A CN202110912683.8A CN202110912683A CN113611536A CN 113611536 A CN113611536 A CN 113611536A CN 202110912683 A CN202110912683 A CN 202110912683A CN 113611536 A CN113611536 A CN 113611536A
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Prior art keywords
foil
agar powder
percent
corrosion
solution
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Inventor
刘慧�
周红炎
金学军
何桂丽
王贵州
宋双喜
肖飞
龚煜
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Sichuan Zhongya Technology Co ltd
Nantong Haixing Electronics LLC
Nantong Haiyi Electronics Co Ltd
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Sichuan Zhongya Technology Co ltd
Nantong Haixing Electronics LLC
Nantong Haiyi Electronics Co Ltd
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Priority to CN202110912683.8A priority Critical patent/CN113611536A/en
Publication of CN113611536A publication Critical patent/CN113611536A/en
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    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01GCAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
    • H01G9/00Electrolytic capacitors, rectifiers, detectors, switching devices, light-sensitive or temperature-sensitive devices; Processes of their manufacture
    • H01G9/0029Processes of manufacture
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01GCAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
    • H01G9/00Electrolytic capacitors, rectifiers, detectors, switching devices, light-sensitive or temperature-sensitive devices; Processes of their manufacture
    • H01G9/004Details
    • H01G9/04Electrodes or formation of dielectric layers thereon
    • H01G9/048Electrodes or formation of dielectric layers thereon characterised by their structure
    • H01G9/055Etched foil electrodes

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  • Engineering & Computer Science (AREA)
  • Power Engineering (AREA)
  • Microelectronics & Electronic Packaging (AREA)
  • Manufacturing & Machinery (AREA)
  • Cleaning And De-Greasing Of Metallic Materials By Chemical Methods (AREA)
  • Battery Electrode And Active Subsutance (AREA)

Abstract

The invention discloses a manufacturing method for reducing foil dust of a low-voltage electrode foil, which comprises the following steps: step (1), soaking the aluminum foil in 0.1-0.5 wt% sodium hydroxide solution for 1-4 min; step (2), alternating current is carried out to generate hole corrosion for 30s-2min in a mixed solution containing 0.01wt% -0.2 wt% of agar powder, 1wt% -10wt% of hydrochloric acid and 0.01wt% -0.1wt% of sulfuric acid; step (3), alternating current electric reaming corrosion is carried out for 6min to 10min in a mixed solution containing 0.1wt percent to 0.4wt percent of agar powder, 1wt percent to 10wt percent of hydrochloric acid, 0.01wt percent to 0.1wt percent of sulfuric acid and 0.05wt percent to 0.25wt percent of phosphoric acid; step (4), soaking for 2min-4min by adopting a nitric acid solution with the weight of 0.5-1.2 percent; step (5), drying after pure water cleaning; and (3) adding agar powder into the pore-forming corrosive liquid obtained in the step (2) and/or adding agar powder into the pore-expanding corrosive liquid obtained in the step (3). The invention aims to effectively improve the capacity of the electrode foil by adding agar powder into the electrolytic bath solution, promote aluminum powder to be dissolved in the mixed acid bath solution and reduce foil ash residue of the low-voltage electrode foil.

Description

Manufacturing method for reducing foil dust of low-voltage electrode foil
Technical Field
The invention relates to a manufacturing method of an electrode foil for an aluminum electrolytic capacitor, and particularly discloses a manufacturing method for reducing low-voltage electrode foil ash.
Background
The high-purity aluminum electrode foil used by the low-voltage aluminum electrolytic capacitor is obtained by alternating current electrochemical surface-expanding corrosion. The high-purity aluminum foil is subjected to an alternating current electrolytic corrosion process, spongy corrosion holes are formed in the surface of the high-purity aluminum foil in a certain thickness, a large amount of aluminum powder is separated out from the surface of the high-purity aluminum foil due to the electrolytic corrosion, one part of the aluminum powder is dissolved in acid liquor, one part of the aluminum powder is washed out in the subsequent water washing process, and the other part of the aluminum powder remains in the aluminum foil corrosion holes and finally becomes foil dust, so that the capacity and the contact resistance of the electrode foil are influenced to a certain extent.
In the prior art, in the manufacturing process of the high-purity aluminum electrode foil, a tap water spraying mode is generally adopted for cleaning, aluminum powder on the shallow surface of the aluminum foil can be cleaned, and aluminum powder in deep etching holes cannot be effectively cleaned through the mode.
Disclosure of Invention
The invention aims to overcome the defects and provide the manufacturing method for reducing the low-voltage electrode foil ash, which effectively improves the capacity of the electrode foil and promotes the dissolution of aluminum powder.
The purpose of the invention is realized by the following technical scheme:
a manufacturing method for reducing foil dust of a low-voltage electrode foil comprises the following steps:
step (1), soaking the aluminum foil in 0.1-0.5 wt% sodium hydroxide solution for 1-4 min;
step (2), performing alternating current power-on holing corrosion for 30s-2min in holing corrosion solution;
step (3), performing AC electric reaming corrosion in the reaming corrosion solution for 6-10 min;
step (4), soaking for 2min-4min by adopting a nitric acid solution with the weight of 0.5-1.2 percent;
step (5), drying after pure water cleaning;
and (3) adding agar powder into the hair hole corrosive liquid in the step (2) and/or adding agar powder into the hole expanding corrosive liquid in the step (3).
Further, the holing corrosion solution in the step (2) is a mixed solution of 0.01wt% to 0.2wt% of agar powder, 1wt% to 10wt% of hydrochloric acid, and 0.01wt% to 0.1wt% of sulfuric acid.
Further, the reaming corrosion solution in the step (3) is a mixed solution of 0.1wt% to 0.4wt% of agar powder, 1wt% to 10wt% of hydrochloric acid, 0.01wt% to 0.1wt% of sulfuric acid and 0.05wt% to 0.25wt% of phosphoric acid.
Further, the step (2) is: performing alternating current power generation hole corrosion for 1min and 30s in a mixed solution containing 0.05wt% of agar powder, 6wt% of hydrochloric acid and 0.03wt% of sulfuric acid;
further, in the step (3), alternating current electric reaming corrosion is carried out for 8min in a mixed solution of 0.3wt% of agar powder, 8wt% of hydrochloric acid, 0.05wt% of sulfuric acid and 0.1wt% of phosphoric acid.
Further, the purity of the aluminum foil is 99.99%, and the thickness of the aluminum foil is 104 μm.
Further, after the step (3), the method also comprises a step (3-4): and (4) cleaning the electrode foil obtained in the step (3) for 60 seconds by using tap water at the temperature of 25 ℃.
Further, the step (5) is drying treatment after the electrode foil is placed in pure water at 25 ℃ for cleaning for 6 min.
The invention has the following beneficial effects: the invention aims to effectively improve the capacity of the electrode foil by adding agar powder into the electrolytic bath solution, promote aluminum powder to be dissolved in the mixed acid bath solution and reduce foil ash residue of the low-voltage electrode foil.
Detailed Description
The technical solution of the present invention is further explained by the specific embodiments.
The invention can realize a manufacturing method for reducing foil dust of a low-voltage electrode by the following technical scheme, which comprises the following steps: step (1), soaking the aluminum foil in 0.1-0.5 wt% sodium hydroxide solution for 1-4 min; step (2), performing alternating current power-on holing corrosion for 30s-2min in holing corrosion solution; step (3), performing AC electric reaming corrosion in the reaming corrosion solution for 6-10 min; step (4), soaking for 2min-4min by adopting a nitric acid solution with the weight of 0.5-1.2 percent; step (5), drying after pure water cleaning; and (3) adding agar powder into the hair hole corrosive liquid in the step (2) and/or adding agar powder into the hole expanding corrosive liquid in the step (3).
Further, the components of the etching solution are preferably selected, and the method comprises the following steps: step (1), soaking the aluminum foil in 0.1-0.5 wt% sodium hydroxide solution for 1-4 min; step (2), alternating current is carried out to generate hole corrosion for 30s-2min in a mixed solution containing 0.01wt% -0.2 wt% of agar powder, 1wt% -10wt% of hydrochloric acid and 0.01wt% -0.1wt% of sulfuric acid; step (3), alternating current electric reaming corrosion is carried out for 6min to 10min in a mixed solution containing 0.1wt percent to 0.4wt percent of agar powder, 1wt percent to 10wt percent of hydrochloric acid, 0.01wt percent to 0.1wt percent of sulfuric acid and 0.05wt percent to 0.25wt percent of phosphoric acid; step (4), soaking for 2min-4min by adopting a nitric acid solution with the weight of 0.5-1.2 percent; step (5), drying after pure water cleaning; and (3) adding agar powder into the pore-forming corrosive liquid obtained in the step (2) and/or adding agar powder into the pore-expanding corrosive liquid obtained in the step (3).
In order to better verify the technical effect of the patent technology, the manufacturing method is subjected to the following test comparison of specific parameters:
a manufacturing method for reducing foil dust of a low-voltage electrode foil comprises the following steps:
(1) soaking an aluminum foil with the purity of 99.99% and the thickness of 104 mu m in 0.5wt% of sodium hydroxide solution for 2 min;
(2) carrying out alternating current hole-making corrosion on the anode foil obtained in the step (1) for 1min30s in a mixed solution which is respectively added with 0.01wt%, 0.05wt%, 0.10wt%, 0.15wt%, 0.20wt% agar powder, 6wt% hydrochloric acid and 0.03wt% sulfuric acid;
(3) adding the anode foil obtained in the step (2) into a mixed solution of 0.1wt%, 0.2wt%, 0.3wt%, 0.4wt% agar powder, 8wt% hydrochloric acid, 0.05wt% sulfuric acid and 0.1wt% phosphoric acid respectively, and performing alternating current electric reaming corrosion for 8 min;
(4) cleaning the anode foil obtained in the step (3) for 60 seconds by using tap water at the temperature of 25 ℃;
(5) soaking the electrode foil obtained in the step (4) in a 1.2wt% nitric acid solution for 2min30 s;
(6) and (5) placing the electrode foil obtained in the step (5) into pure water at 25 ℃ for cleaning for 6min, and then drying.
Example 1: the concentration of the agar powder in the liquid of the pore-forming corrosion tank is 0.01wt%, and the concentration of the agar powder in the liquid of the pore-expanding corrosion tank is 0.1 wt%.
Example 2: the concentration of the agar powder in the liquid of the pore-forming corrosion tank is 0.05wt%, and the concentration of the agar powder in the liquid of the pore-expanding corrosion tank is 0.1 wt%.
Example 3: the concentration of the agar powder in the liquid of the pore-forming corrosion tank is 0.10wt%, and the concentration of the agar powder in the liquid of the pore-expanding corrosion tank is 0.1 wt%.
Example 4: the concentration of the agar powder in the liquid of the pore-forming corrosion tank is 0.15wt%, and the concentration of the agar powder in the liquid of the pore-expanding corrosion tank is 0.1 wt%.
Example 5: the concentration of the agar powder in the liquid of the pore-forming corrosion tank is 0.20wt%, and the concentration of the agar powder in the liquid of the pore-expanding corrosion tank is 0.1 wt%.
Example 6: the concentration of the agar powder in the liquid of the pore-forming corrosion tank is 0.05wt%, and the concentration of the agar powder in the liquid of the pore-expanding corrosion tank is 0.2 wt%.
Example 7: the concentration of the agar powder in the liquid of the pore-forming corrosion tank is 0.05wt%, and the concentration of the agar powder in the liquid of the pore-expanding corrosion tank is 0.3 wt%.
Example 8: the concentration of the agar powder in the liquid of the pore-forming corrosion tank is 0.05wt%, and the concentration of the agar powder in the liquid of the pore-expanding corrosion tank is 0.4 wt%.
Comparing the concentrations of the agar powder in the pore-forming corrosion tank solutions of the examples 1, 2, 3, 4 and 5:
performing alternating current power generation on an aluminum foil with the thickness of 104 mu m and the purity of 99.99 percent in a mixed solution of hydrochloric acid and sulfuric acid containing 0.01 to 0.2 weight percent of agar powder to corrode for 1min30 s; performing alternating current electric reaming corrosion for 8min in a mixed solution of hydrochloric acid, sulfuric acid and phosphoric acid containing 0.1wt% of agar powder; soaking the mixture in 1.2wt% nitric acid solution for 2min to obtain a solution of 30 s; and finally, drying after pure water cleaning. And (3) testing the electrostatic capacity of the electrode foil, and simultaneously testing the content of cleaning water aluminum in the starting hole corrosion tank and the reaming corrosion tank by an ICP (emission spectrometer).
Comparing the concentrations of the agar powder in the reaming corrosion tank solutions of the examples 2, 6, 7 and 8:
performing alternating current power generation on 104 mu m-thick aluminum foil with the purity of 99.99% in a mixed solution of hydrochloric acid and sulfuric acid containing 0.05wt% of agar powder to perform hole corrosion for 1min30 s; alternating current and electric reaming corrosion is carried out in a mixed solution of hydrochloric acid, sulfuric acid and phosphoric acid containing 0.1-0.4 wt% of agar powder for 8 min; soaking the mixture in 1.2wt% nitric acid solution for 2min to obtain a solution of 30 s; and finally, drying after pure water cleaning. And (3) testing the electrostatic capacity of the electrode foil, and simultaneously carrying out ICP (emission spectrometer) test on the aluminum content of cleaning water in the starting hole corrosion tank and the reaming corrosion tank.
The conventional example:
performing alternating current power-on pore corrosion on 104 mu m-thick aluminum foil with the purity of 99.99% in a mixed solution containing hydrochloric acid and sulfuric acid for 1min30 s; performing AC electric reaming corrosion for 8min in a mixed solution containing hydrochloric acid, sulfuric acid and phosphoric acid; soaking the mixture in 1.2wt% nitric acid solution for 2min to obtain a solution of 30 s; and finally, drying after pure water cleaning. And (3) testing the electrostatic capacity of the electrode foil, and simultaneously testing the content of cleaning water aluminum in the starting hole corrosion tank and the reaming corrosion tank by an ICP (emission spectrometer).
The above comparison results in data as shown in table 1:
Figure 695538DEST_PATH_IMAGE001
and (3) comparing the concentrations of the agar powder in the liquid of the perforation corrosion tank:
as can be seen from table 1, under the condition that the concentration of agar powder in the fixed reaming corrosion solution is 0.1wt%, when the concentrations of agar powder in the reaming corrosion solution are 0.01wt%, 0.05wt%, 0.10wt%, 0.15wt% and 0.20wt%, the capacity increases first and then decays, the aluminum content of the cleaning water in the starting hole tank gradually decreases, and when the concentration of agar powder in the reaming corrosion solution is 0.05wt%, the capacity is highest and the aluminum content of the cleaning water is maintained at a low level. With the further increase of the concentration of the agar powder in the pore solution, the capacity is greatly attenuated, and the aluminum content of the cleaning water is only slightly reduced.
Therefore, the comprehensive performance is best when the solubility of the agar powder in the pore-forming etching solution is 0.05wt% under the condition that the concentration of the agar powder in the fixed pore-expanding etching solution is 0.1 wt%.
And (3) comparing the concentrations of the agar powder in the reaming corrosion tank liquid:
as can be seen from table 1, under the condition that the concentration of agar powder in the fixed pore-forming corrosion solution is 0.05wt%, and the concentrations of agar powder in the pore-expanding corrosion solution are 0.1wt%, 0.2wt%, 0.3wt% and 0.4wt%, the capacity rises first and then decays, the aluminum content of the washing water exiting from the pore-expanding tank gradually decreases, and when the concentration of agar powder in the pore-expanding corrosion solution is 0.3wt%, the capacity is the highest, and the aluminum content of the washing water is maintained at a low level. With the further increase of the concentration of the agar powder in the reaming solution, the capacity is greatly attenuated, and the aluminum content of the cleaning water is only slightly reduced.
Therefore, when the concentration of the agar powder in the fixed pore-forming corrosion solution is 0.05wt%, and the solubility of the agar powder in the pore-forming corrosion solution is 0.3wt%, the comprehensive performance is best.
The optimal manufacturing method by comparing the patent technology comprises the following steps: the manufacturing method for reducing the foil dust of the low-voltage electrode foil comprises the following steps: soaking 104 mu m-thick aluminum foil with the purity of 99.99% in 0.5wt% sodium hydroxide solution for 2 min; adding 0.05wt% agar powder in a mixed solution of 6wt% hydrochloric acid and 0.03wt% sulfuric acid, and performing alternating current power hole etching for 1min30 s; adding 0.3wt% agar powder, 8wt% hydrochloric acid, 0.05wt% sulfuric acid and 0.1wt% phosphoric acid into the mixed solution, and performing AC electric reaming corrosion for 8 min; soaking the mixture in 1.2wt% nitric acid solution for 2min to obtain a solution of 30 s; cleaning with pure water at 25 deg.C for 6min, and drying.

Claims (8)

1. A manufacturing method for reducing foil dust of a low-voltage electrode foil comprises the following steps:
step (1), soaking the aluminum foil in 0.1-0.5 wt% sodium hydroxide solution for 1-4 min;
step (2), performing alternating current power-on holing corrosion for 30s-2min in holing corrosion solution;
step (3), performing AC electric reaming corrosion in the reaming corrosion solution for 6-10 min;
step (4), soaking for 2min-4min by adopting a nitric acid solution with the weight of 0.5-1.2 percent;
step (5), drying after pure water cleaning;
the method is characterized in that: and (3) adding agar powder into the hair hole corrosive liquid in the step (2) and/or adding agar powder into the hole expanding corrosive liquid in the step (3).
2. The method for reducing foil dust of a low voltage electrode according to claim 1, wherein: the holing corrosion solution in the step (2) is a mixed solution of 0.01-0.2 wt% of agar powder, 1-10 wt% of hydrochloric acid and 0.01-0.1 wt% of sulfuric acid.
3. The method for reducing foil dust of a low voltage electrode according to claim 2, wherein: the reaming corrosion solution in the step (3) is a mixed solution of 0.1-0.4 wt% of agar powder, 1-10 wt% of hydrochloric acid, 0.01-0.1 wt% of sulfuric acid and 0.05-0.25 wt% of phosphoric acid.
4. The method for reducing foil dust of a low voltage electrode according to claim 3, wherein: the step (2) is as follows: and performing alternating current power generation hole corrosion for 1min and 30s in a mixed solution containing 0.05wt% of agar powder, 6wt% of hydrochloric acid and 0.03wt% of sulfuric acid.
5. The method for reducing foil dust of a low voltage electrode according to claim 4, wherein: the step (3) is as follows: performing AC electric reaming corrosion for 8min in a mixed solution of 0.3wt% agar powder, 8wt% hydrochloric acid, 0.05wt% sulfuric acid and 0.1wt% phosphoric acid.
6. The method for reducing foil dust of a low voltage electrode according to claim 5, wherein: the purity of the aluminum foil is 99.99%, and the thickness of the aluminum foil is 104 mu m.
7. The method for reducing foil dust of a low voltage electrode according to claim 6, wherein: after the step (3), further comprising a step (3-4): and (4) cleaning the electrode foil obtained in the step (3) for 60 seconds by using tap water at the temperature of 25 ℃.
8. The method for reducing foil dust of a low voltage electrode according to claim 7, wherein: and (5) placing the electrode foil in pure water at 25 ℃ for cleaning for 6min, and then drying.
CN202110912683.8A 2021-08-10 2021-08-10 Manufacturing method for reducing foil dust of low-voltage electrode foil Pending CN113611536A (en)

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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB314160A (en) * 1928-04-18 1929-06-27 Telegraph Condenser Co Ltd Improvements in or relating to electrolytic condensers
CN1886811A (en) * 2004-04-13 2006-12-27 如碧空株式会社 Electrolytic capacitor and electrolytic solution for driving the same
JP2009290084A (en) * 2008-05-30 2009-12-10 Nichicon Corp Method for manufacturing electrode foil for electrolytic capacitor
CN107591247A (en) * 2017-08-30 2018-01-16 南通海星电子股份有限公司 A kind of low contact resistance low-voltage aluminum electrolytic capacitor electrode foil corrosion method

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB314160A (en) * 1928-04-18 1929-06-27 Telegraph Condenser Co Ltd Improvements in or relating to electrolytic condensers
CN1886811A (en) * 2004-04-13 2006-12-27 如碧空株式会社 Electrolytic capacitor and electrolytic solution for driving the same
JP2009290084A (en) * 2008-05-30 2009-12-10 Nichicon Corp Method for manufacturing electrode foil for electrolytic capacitor
CN107591247A (en) * 2017-08-30 2018-01-16 南通海星电子股份有限公司 A kind of low contact resistance low-voltage aluminum electrolytic capacitor electrode foil corrosion method

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Application publication date: 20211105