CN105350064A - Corrosion process method of anode foil for solid aluminum electrolytic capacitor - Google Patents

Corrosion process method of anode foil for solid aluminum electrolytic capacitor Download PDF

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Publication number
CN105350064A
CN105350064A CN201510874532.2A CN201510874532A CN105350064A CN 105350064 A CN105350064 A CN 105350064A CN 201510874532 A CN201510874532 A CN 201510874532A CN 105350064 A CN105350064 A CN 105350064A
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Prior art keywords
corrosion
electrolytic capacitor
variable frequency
aluminum electrolytic
frequency
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CN201510874532.2A
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Chinese (zh)
Inventor
马坤松
相志明
王磊
裴韩
韩枫
周鑫
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YANGZHOU HONGYUAN ELECTRONICS CO Ltd
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YANGZHOU HONGYUAN ELECTRONICS CO Ltd
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Priority to CN201510874532.2A priority Critical patent/CN105350064A/en
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    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23G—CLEANING OR DE-GREASING OF METALLIC MATERIAL BY CHEMICAL METHODS OTHER THAN ELECTROLYSIS
    • C23G1/00—Cleaning or pickling metallic material with solutions or molten salts
    • C23G1/02—Cleaning or pickling metallic material with solutions or molten salts with acid solutions
    • C23G1/12—Light metals
    • C23G1/125—Light metals aluminium
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25F—PROCESSES FOR THE ELECTROLYTIC REMOVAL OF MATERIALS FROM OBJECTS; APPARATUS THEREFOR
    • C25F3/00—Electrolytic etching or polishing
    • C25F3/02—Etching
    • C25F3/04—Etching of light metals
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
    • H01G9/00—Electrolytic capacitors, rectifiers, detectors, switching devices, light-sensitive or temperature-sensitive devices; Processes of their manufacture
    • H01G9/0029—Processes of manufacture
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
    • H01G9/00—Electrolytic capacitors, rectifiers, detectors, switching devices, light-sensitive or temperature-sensitive devices; Processes of their manufacture
    • H01G9/004—Details
    • H01G9/04—Electrodes or formation of dielectric layers thereon
    • H01G9/042—Electrodes or formation of dielectric layers thereon characterised by the material
    • H01G9/045—Electrodes or formation of dielectric layers thereon characterised by the material based on aluminium
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
    • H01G9/00—Electrolytic capacitors, rectifiers, detectors, switching devices, light-sensitive or temperature-sensitive devices; Processes of their manufacture
    • H01G9/004—Details
    • H01G9/04—Electrodes or formation of dielectric layers thereon
    • H01G9/048—Electrodes or formation of dielectric layers thereon characterised by their structure
    • H01G9/055—Etched foil electrodes

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  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Power Engineering (AREA)
  • Microelectronics & Electronic Packaging (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Metallurgy (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Mechanical Engineering (AREA)
  • Electrochemistry (AREA)
  • Manufacturing & Machinery (AREA)
  • Fixed Capacitors And Capacitor Manufacturing Machines (AREA)

Abstract

The invention provides a corrosion process method of an anode foil for a solid aluminum electrolytic capacitor. The process is that a soft annealed aluminum foil is subjected to AC variable-frequency corrosion through a mixed solution after pre-treatment, wherein the mixed solution contains 2 to 20wt% of hydrochloric acid, 0.02 to 0.2wt% of sulfuric acid, and 0.02 to 2wt% of aluminum trichloride; then the aluminum foil is subjected to intermediate treatment through an aqueous solution containing 0.5 to 10wt% of phosphoric acid or other acidic salts; the AC variable-frequency corrosion is repeatedly carried out at a plurality of times according to different waveforms and the process that frequency gradually varies from high to low (40 to 5Hz), so as to achieve multi-stage hole expansion corrosion for the aluminum foil; finally the aluminum foil is chemically cleaned. The corroded foil obtained by the aforementioned process is high in specific volume and high in mechanical strength and is applicable to the production of solid aluminum electrolytic capacitor.

Description

A kind of etching process method of solid-state aluminum electrolytic capacitor anode foils
Technical field
The present invention relates to a kind of complete processing of anode foils, be specifically related to a kind of etching process method of solid-state aluminum electrolytic capacitor anode foils.
Background technology
Solid-state aluminum electrolytic capacitor anode foils needs anode foils unit surface to have higher electrostatic capacity, in order to expand its effective surface area, increasing the electrostatic capacity of unit surface, generally processing aluminium foil with galvanic corrosion.About the research improving area expanding rate aspect has many reports, past technique uses 50Hz AC corrosion, or change the method that supply frequency reaches expansion pit size, but these existing sizes to technology pit and the degree of depth wayward, not reaching solid-state aluminum electrolytic capacitor anode foils needs extended surface effect.
Summary of the invention
Goal of the invention: for above-mentioned existing Problems existing and deficiency, the invention provides a kind of soft state annealing aluminium foil, the multistage AC variable frequency corrosion technology of different wave and frequency is adopted for different steps, erode away hole relatively uniform, there is comparatively Fabrication of High Specific Capacitance, better physical strength, be applicable to the etching process method of production solid-state aluminum electrolytic capacitor anode foils.
Technical scheme: for achieving the above object, the present invention by the following technical solutions: a kind of etching process method of solid-state aluminum electrolytic capacitor anode foils, comprises the following steps:
(1) pre-treatment: aluminium foil is immersed containing 1 ~ 10wt% phosphorus aqueous acid, and 40 ~ 240s is soaked at 30 ~ 90 DEG C;
(2) AC variable frequency corrosion: the aluminium foil after pre-treatment immerses in the mixing solutions containing 2 ~ 20wt% hydrochloric acid, 0.2 ~ 2wt ‰ sulfuric acid and 0.2 ~ 20wt ‰ aluminum chloride and carries out AC variable frequency corrosion, wherein, corrosion temperature is 6 ~ 60 DEG C, current density is 10 ~ 100A/dm 2, frequency 40 ~ 50Hz, etching time 10 ~ 100 seconds;
(3) intermediate treatment: the aluminium foil after AC variable frequency corrosion is immersed again in the aqueous solution containing 0.5 ~ 10wt% phosphoric acid or its acid salt, and 40 ~ 240s is soaked at 30 ~ 990 DEG C;
(4) multistage reaming corrosion: in the range of frequency of 8 ~ 50Hz, carries out repetitious AC variable frequency corrosion according to the mode of frequency stairway degression gradually, carries out multistage reaming corrosion to aluminium foil; Need through an intermediate treatment between every two-stage reaming corrosion in this process, and directly enter matting after last step reaming corrosion;
(5) matting: it is 30 ~ 90 DEG C that the aluminium foil after reaming being corroded immerses temperature, soaks 40 ~ 240 seconds containing in 2 ~ 20wt% sulfuric acid and the aqueous solution.
As preferably, in step (2), the current waveform of AC variable frequency corrosion is as shown in formula (1):
Y = a 1 x + h 0 &le; x < t 1 d t 1 &le; x < t 2 - a 1 x + h t 2 &le; x < t 3 - a 1 x - h t 3 &le; x < t 4 - d t 4 &le; x < t 5 a 1 x - h t 5 &le; x < t 6 - - - ( 1 )
Wherein, Y is current value, and x is the time in wave period, a 1, d and h be constant parameter value, t 1, t 2, t 3, t 4, t 5, t 6for the time point in wave period.
As preferably, the described multistage reaming corrosion of step (4) is through 7 grades of AC variable frequency corrosions, and the current waveform of every grade of AC variable frequency corrosion is successively as shown in formula (2) ~ (8):
Y = a 2 x + h 0 &le; x < t 1 d t 1 &le; x < t 2 - a 2 x + h t 2 &le; x < t 3 - a 2 x - h t 3 &le; x < t 4 - d t 4 &le; x < t 5 a 2 x - h t 5 &le; x < t 6 - - - ( 2 )
Y = a 1 x + h 0 &le; x < t 1 d t 1 &le; x < t 2 - a 1 x + h t 2 &le; x < t 3 - d t 3 &le; x < t 4 a 1 x - h t 4 &le; x < t 5 - - - ( 3 )
Y = a 2 x + h 0 &le; x < t 1 d t 1 &le; x < t 2 - a 2 x + h t 2 &le; x < t 3 - d t 3 &le; x < t 4 a 2 x - h t 4 &le; x < t 5 - - - ( 4 )
Y = a 3 x + h 0 &le; x < t 1 d t 1 &le; x < t 2 - a 3 x + h t 2 &le; x < t 3 - d t 3 &le; x < t 4 a 3 x - h t 4 &le; x < t 5 - - - ( 5 )
Y = a 1 x 0 &le; x < t 1 - a 1 x + d t 1 &le; x < t 2 a 1 x - d t 2 &le; x < t 3 - - - ( 6 )
Y = a 2 x 0 &le; x < t 1 - a 2 x + d t 1 &le; x < t 2 a 2 x - d t 2 &le; x < t 3 - - - ( 7 )
Y = a 3 x 0 &le; x < t 1 - a 3 x + d t 1 &le; x < t 2 a 3 x - d t 2 &le; x < t 3 - - - ( 8 ) .
Wherein, Y is current value, and x is the time in wave period, a 1, a 2, a 3, d and h be positive number constant parameter value, t 1, t 2, t 3, t 4, t 5, t 6for the time point in wave period; Wherein a 1> a 2> a 3, and d > h.
As preferably, described step (4) etching time is 20 ~ 90 seconds.
Beneficial effect: compared with prior art, the present invention forms by the etched foil that above-mentioned technique obtains that rear specific volume is high, physical strength good, is applicable to production solid-state aluminum electrolytic capacitor.
Accompanying drawing explanation
Fig. 1 is the ac power waveform schematic diagram in AC variable frequency corrosion of the present invention each stage.
Embodiment
Below in conjunction with the drawings and specific embodiments, illustrate the present invention further, these embodiments should be understood only be not used in for illustration of the present invention and limit the scope of the invention, after having read the present invention, the amendment of those skilled in the art to the various equivalent form of value of the present invention has all fallen within the application's claims limited range.
Below by production 115um aluminium foil actual process process, the present invention is specifically described, is necessary to herein means out: following examples are only used to further illustrate the present invention, can not limiting the scope of the invention be interpreted as.
In the present invention, during AC variable frequency corrosion, each stage AC wave shape is all different, and as shown in Figure 1, the corresponding formula of waveform A, B, C, D, E, F, G, H eight kinds of waveforms is followed successively by (1) ~ (8).
Embodiment 1:
Obtain the aluminium foil of 115 μm, 21Vf:C=120 ~ 122uf/cm 2, bend-resistance 84 times.
Embodiment 2:
Obtain the aluminium foil of 115 μm, 21Vf:C=116 ~ 118uf/cm 2, bend-resistance 88 times.
Embodiment 3:
Obtain the aluminium foil of 115 μm, 21Vf:C=110 ~ 112uf/cm 2; Bend-resistance 92 times.
The present invention adopts soft state annealing aluminium foil, the multistage AC variable frequency corrosion technology of different wave and frequency is adopted for different steps, erode away hole relatively uniform, have under the prerequisite compared with Fabrication of High Specific Capacitance, the physical strength simultaneously obtained, is applicable to the etching process method of production solid-state aluminum electrolytic capacitor anode foils.

Claims (4)

1. an etching process method for solid-state aluminum electrolytic capacitor anode foils, is characterized in that comprising the following steps:
(1) pre-treatment: aluminium foil is immersed containing 1 ~ 10wt% phosphorus aqueous acid, and 40 ~ 240s is soaked at 30 ~ 90 DEG C;
(2) AC variable frequency corrosion: the aluminium foil after pre-treatment immerses in the mixing solutions containing 2 ~ 20wt% hydrochloric acid, 0.2 ~ 2wt ‰ sulfuric acid and 0.2 ~ 20wt ‰ aluminum chloride and carries out AC variable frequency corrosion, wherein, corrosion temperature is 6 ~ 60 DEG C, current density is 10 ~ 100A/dm 2, frequency 40 ~ 50Hz, etching time 10 ~ 100 seconds;
(3) intermediate treatment: the aluminium foil after AC variable frequency corrosion is immersed again in the aqueous solution containing 0.5 ~ 10wt% phosphoric acid or its acid salt, and 40 ~ 240s is soaked at 30 ~ 990 DEG C;
(4) multistage reaming corrosion: in the range of frequency of 8 ~ 50Hz, carries out repetitious AC variable frequency corrosion according to the mode of frequency stairway degression gradually, carries out multistage reaming corrosion to aluminium foil; Need through an intermediate treatment between every two-stage reaming corrosion in this process, and directly enter matting after last step reaming corrosion;
(5) matting: it is 30 ~ 90 DEG C that the aluminium foil after reaming being corroded immerses temperature, soaks 40 ~ 240 seconds containing in 2 ~ 20wt% sulfuric acid and the aqueous solution.
2. the etching process method of solid-state aluminum electrolytic capacitor anode foils according to claim 1, is characterized in that: in step (2), the current waveform of AC variable frequency corrosion is as shown in formula (1):
Y = a 1 x + h 0 &le; x < t 1 d t 1 &le; x < t 2 - a 1 x + h t 2 &le; x < t 3 - a 1 x - h t 3 &le; x < t 4 - d t 4 &le; x < t 5 a 1 x - h t 5 &le; x < t 6 - - - ( 1 )
Wherein, Y is current value, and x is the time in wave period, a 1, d and h be constant parameter value, t 1, t 2, t 3, t 4, t 5, t 6for the time point in wave period.
3. the etching process method of solid-state aluminum electrolytic capacitor anode foils according to claim 1, it is characterized in that: the described multistage reaming corrosion of step (4) is through 7 grades of AC variable frequency corrosions, and the current waveform of every grade of AC variable frequency corrosion is successively as shown in formula (2) ~ (8):
Y = a 2 x + h 0 &le; x < t 1 d t 1 &le; x < t 2 - a 2 x + h t 2 &le; x < t 3 - a 2 x - h t 3 &le; x < t 4 - d t 4 &le; x < t 5 a 2 x - h t 5 &le; x < t 6 - - - ( 2 )
Y = a 1 x + h 0 &le; x < t 1 d t 1 &le; x < t 2 - a 1 x + h t 2 &le; x < t 3 - d t 3 &le; x < t 4 a 1 x - h t 4 &le; x < t 5 - - - ( 3 )
Y = a 2 x + h 0 &le; x < t 1 d t 1 &le; x < t 2 - a 2 x + h t 2 &le; x < t 3 - d t 3 &le; x < t 4 a 2 x - h t 4 &le; x < t 5 - - - ( 4 )
Y = a 3 x + h 0 &le; x < t 1 d t 1 &le; x < t 2 - a 3 x + h t 2 &le; x < t 3 - d t 3 &le; x < t 4 a 3 x - h t 4 &le; x < t 5 - - - ( 5 )
Y = a 1 x 0 &le; x < t 1 - a 1 x + d t 1 &le; x < t 2 a 1 x - d t 2 &le; x < t 3 - - - ( 6 )
Y = a 2 x 0 &le; x < t 1 - a 2 x + d t 1 &le; x < t 2 a 2 x - d t 2 &le; x < t 3 - - - ( 7 )
Y = a 3 x 0 &le; x < t 1 - a 3 x + d t 1 &le; x < t 2 a 3 x - d t 2 &le; x < t 3 - - - ( 8 ) .
Wherein, Y is current value, and x is the time in wave period, a 1, a 2, a 3, d and h be positive number constant parameter value, t 1, t 2, t 3, t 4, t 5, t 6for the time point in wave period; Wherein a 1> a 2> a 3, and d > h.
4. the etching process method of solid-state aluminum electrolytic capacitor anode foils according to claim 1, is characterized in that: described step (4) etching time is 20 ~ 90 seconds.
CN201510874532.2A 2015-12-03 2015-12-03 Corrosion process method of anode foil for solid aluminum electrolytic capacitor Pending CN105350064A (en)

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Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106981367A (en) * 2017-04-18 2017-07-25 扬州宏远电子有限公司 The follow-on solid-state capacitor electrode aluminium foil processing method of one kind post processing
CN107123549A (en) * 2017-04-18 2017-09-01 扬州宏远电子有限公司 A kind of pre-treating method for improving solid-state capacitor electrode aluminium foil specific volume
CN110085455A (en) * 2019-03-20 2019-08-02 东莞东阳光科研发有限公司 The method for promoting low pressure corrosive aluminum foil specific volume
CN110923779A (en) * 2019-11-27 2020-03-27 东莞东阳光科研发有限公司 Ultrahigh pressure etched foil and etching method thereof
CN111370232A (en) * 2020-03-24 2020-07-03 东莞东阳光科研发有限公司 Preparation method of electrode foil for low-voltage aluminum electrolytic capacitor
CN113279046A (en) * 2021-05-20 2021-08-20 浙江丰川电子环保科技股份有限公司 Rapid chemical corrosion process for anode aluminum foil for electrolytic capacitor
WO2022247364A1 (en) * 2021-04-29 2022-12-01 南通海星电子股份有限公司 Method for preparing nano microporous structure aluminum electrode foil for automotive electronics
CN117265629A (en) * 2023-09-22 2023-12-22 惠州市冠业新材料科技有限公司 Electrochemical corrosion process for current collector aluminum foil of supercapacitor
CN117612868A (en) * 2024-01-18 2024-02-27 南通南辉电子材料股份有限公司 Method for manufacturing medium-pressure corrosion foil

Cited By (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106981367A (en) * 2017-04-18 2017-07-25 扬州宏远电子有限公司 The follow-on solid-state capacitor electrode aluminium foil processing method of one kind post processing
CN107123549A (en) * 2017-04-18 2017-09-01 扬州宏远电子有限公司 A kind of pre-treating method for improving solid-state capacitor electrode aluminium foil specific volume
CN110085455A (en) * 2019-03-20 2019-08-02 东莞东阳光科研发有限公司 The method for promoting low pressure corrosive aluminum foil specific volume
CN110923779A (en) * 2019-11-27 2020-03-27 东莞东阳光科研发有限公司 Ultrahigh pressure etched foil and etching method thereof
CN111370232A (en) * 2020-03-24 2020-07-03 东莞东阳光科研发有限公司 Preparation method of electrode foil for low-voltage aluminum electrolytic capacitor
CN111370232B (en) * 2020-03-24 2022-01-11 东莞东阳光科研发有限公司 Preparation method of electrode foil for low-voltage aluminum electrolytic capacitor
WO2022247364A1 (en) * 2021-04-29 2022-12-01 南通海星电子股份有限公司 Method for preparing nano microporous structure aluminum electrode foil for automotive electronics
CN113279046A (en) * 2021-05-20 2021-08-20 浙江丰川电子环保科技股份有限公司 Rapid chemical corrosion process for anode aluminum foil for electrolytic capacitor
CN117265629A (en) * 2023-09-22 2023-12-22 惠州市冠业新材料科技有限公司 Electrochemical corrosion process for current collector aluminum foil of supercapacitor
CN117265629B (en) * 2023-09-22 2024-04-16 惠州市冠业新材料科技有限公司 Electrochemical corrosion process for current collector aluminum foil of supercapacitor
CN117612868A (en) * 2024-01-18 2024-02-27 南通南辉电子材料股份有限公司 Method for manufacturing medium-pressure corrosion foil
CN117612868B (en) * 2024-01-18 2024-04-26 南通南辉电子材料股份有限公司 Method for manufacturing medium-pressure corrosion foil

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Application publication date: 20160224