CN107967996B - A kind of chemical synthesizing method of mash welder capacitor anode foils - Google Patents
A kind of chemical synthesizing method of mash welder capacitor anode foils Download PDFInfo
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- CN107967996B CN107967996B CN201711129339.1A CN201711129339A CN107967996B CN 107967996 B CN107967996 B CN 107967996B CN 201711129339 A CN201711129339 A CN 201711129339A CN 107967996 B CN107967996 B CN 107967996B
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-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
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
- C25D11/02—Anodisation
- C25D11/04—Anodisation of aluminium or alloys based thereon
- C25D11/12—Anodising more than once, e.g. in different baths
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
- C25D11/02—Anodisation
- C25D11/04—Anodisation of aluminium or alloys based thereon
- C25D11/16—Pretreatment, e.g. desmutting
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
- C25D11/02—Anodisation
- C25D11/04—Anodisation of aluminium or alloys based thereon
- C25D11/18—After-treatment, e.g. pore-sealing
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-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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- Chemical Kinetics & Catalysis (AREA)
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- Organic Chemistry (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Fixed Capacitors And Capacitor Manufacturing Machines (AREA)
Abstract
The invention discloses a kind of chemical synthesizing methods of mash welder capacitor anode foils, including boil processing, level Four chemical conversion, heat treatment, phosphoric acid processing, repair chemical conversion, post-processing, drying again.Its innovative point is: boiling processing using citric acid and its ammonium salt solution composition boils treatment fluid, the short time boils processing, then low temperature is melted into, anode foil oxide film is made and is substantially free of porous aluminium hydroxide outer layer, have the characteristics that low, resistance to rush of current is lost and resistance to temperature characteristic is good, life characteristics are quite stable, are suitable for production mash welder capacitor；Conventional anodes foil cannot compare completely.
Description
Technical field
The invention belongs to anode foil for aluminum electrolytic capacitor manufacturing technology fields, and in particular to a kind of mash welder capacitor sun
The chemical synthesizing method of pole foil.
Background technique
The chemical synthesizing method of conventional medium-high voltage aluminum electrolytic capacitor anode foils generally comprises and boils processing, multistage chemical conversion, heat
It handles, be melted into again, phosphoric acid processing, the processes such as be melted into, post-process, drying again；Wherein boiling processing is that etched foil is placed in 95 DEG C
5~15min is boiled in above pure water, and is melted into temperature at 85 DEG C or more, finally obtains fine and close, the good medium of insulation performance
Oxidation film；This anode foils capacitance is big, surface hydration thickness of oxidation film, loss tangent (tg δ) are high, internal resistance is big, calorific value
Greatly, the resistance to rush of current ability of oxidation film and resistance to temperature characteristic are relatively poor, are not suitable for production rapidly charge and discharge class capacitor
Device.
Energy-storage capacitor of the mash welder capacitor as high voltage rapidly charge and discharge, charge and discharge time interval is very short, wink
Between charging and discharging currents it is very big；If loss is high, internal resistance is big, short time internal heat generation power is with regard to big, and capacitor then heats up rapidly, meeting
Lead to internal a large amount of deflate and rouses bottom or even pop.The capacitors count of one spot welding machine equipment installation is more, moment charge and discharge electricity
Very big, risk height is flowed, therefore very high to anode foils quality requirement；Mash welder capacitor requires loss with anode foils
Low, resistance to rush of current and the good feature of resistance to temperature characteristic, life characteristics want quite stable, it is desirable that are totally different from conventional anodes
Foil.
Summary of the invention
To solve the above-mentioned problems, the present invention provides a kind of chemical synthesizing method of mash welder capacitor anode foils；The present invention
The anode foil oxide film surface of production is substantially free of porous aluminium hydroxide outer layer, has and low, resistance to rush of current and resistance to temperature rise is lost
The good feature of characteristic, life characteristics are quite stable；Suitable for production mash welder capacitor.
Technical scheme is as follows:
A kind of chemical synthesizing method of mash welder capacitor anode foils is provided, comprising the following steps:
Step 1: treatment fluid is boiled using citric acid and its ammonium salt solution composition, specifically by citric acid and dihydrogen citrate
Ammonium or diammonium hydrogen citrate or ammonium citrate solution composition, boiling liquid conductivity are 20~200 μ s/cm.
Step 2: the etched foil of through borrosion hole structure is placed in the boiling liquid being made of citric acid and its ammonium salt,
1~5min of processing is boiled at 85~95 DEG C.
Step 3: it is five boron of 4~6wt% boric acid and 0.01~0.3wt% that the etched foil for being boiled processing, which is placed in concentration,
In sour ammonium mixed solution, carry out level Four chemical conversion at a temperature of 40~60 DEG C, level Four formation voltage be respectively answer alive 30%,
60%, 90%, 100%, the chemical conversion time is 8~30min.
Step 4: being heat-treated to the aluminium foil by level Four chemical conversion, heat treatment temperature is 450~500 DEG C, when heat treatment
Between be 1~3min.
Step 5: carrying out chemical conversion reparation to thermally treated aluminium foil, chemical conversion repair time is 6~10min.
Step 6: the aluminium foil for being melted into reparation is placed in the phosphoric acid solution of 5~9wt%, handles 4 at 60~75 DEG C
~8min.
It is repaired Step 7: carrying out secondary chemical conversion, chemical conversion repair time is 6~10min.
Step 8: carrying out secondary heat treatment, treatment temperature is 450~500 DEG C, and the processing time is 1~3min.
It is repaired Step 9: carrying out chemical conversion three times, chemical conversion repair time is 6~10min.
Step 10: by the aluminium foil for being melted into reparation be placed in the phosphoric acid solution of 0.06~0.1wt% under room temperature processing 2~
5min。
Step 11: mash welder capacitor is made in 150~250 DEG C of 2~3min of drying in the aluminium foil post-processed through peroxophosphoric acid
Device anode foils.
Preferably, the treatment fluid that boils is made of citric acid and its ammonium salt solution, specifically includes citric acid and citric acid
Ammonium dihydrogen or diammonium hydrogen citrate or ammonium citrate solution composition.
Preferably, the treatment fluid conductivity of boiling is 20~200 μ s/cm.
Preferably, the treatment temperature of boiling is 85~95 DEG C.
Preferably, described to boil the processing time for 1~5min.
Preferably, the chemical conversion temperature is 40~60 DEG C.
Beneficial effects of the present invention:
Etched foil citric acid and its ammonium salt aqueous solution short time is boiled processing, and citric acid and its ammonium salt inhibit and dissolution
Aluminium foil surface hydrated film featheriness layer, then low temperature is melted into, and anode foil oxide film obtained is substantially free of outside porous aluminium hydroxide
Layer has the characteristics that low, the resistance to rush of current of loss and resistance to temperature characteristic are good, and life characteristics are quite stable, can reach production spot welding
The requirement of electromechanical container.And conventional chemical synthesizing method handles etched foil through boiling pure water, high temperature is melted into, anode foils obtained are complete
It cannot compare.
Detailed description of the invention:
Fig. 1 is conventional anodes foil oxide film surface SEM photograph (30000 times)
Fig. 2 is anode foil oxide film of the present invention surface SEM photograph (30000 times)
Specific embodiment
Below with reference to embodiment, the technical solution of the present invention is further described in detail, but embodiments of the present invention are unlimited
In this.
Embodiment 1
One example of the chemical synthesizing method of mash welder capacitor anode foils of the present invention, include the following steps: by
It is that 20 μ s/cm boil treatment fluid that through borrosion hole structure erosion foil, which is placed in and forms conductivity by citric acid and ammonium citrate solution,
In, handle 1min at 95 DEG C, then in 6% boric acid and 0.2wt% ammonium pentaborate mixed solution, temperature 60 C, voltage 180V
Under the conditions of carry out first order chemical conversion, chemical conversion constant voltage time be 8min；Then molten in 6% boric acid and the mixing of 0.1wt% ammonium pentaborate
In liquid, second level chemical conversion is carried out under the conditions of temperature 60 C, voltage 360V, chemical conversion constant voltage time is 8min, then in 5% boric acid and
In 0.05wt% ammonium pentaborate mixed solution, third level chemical conversion is carried out under the conditions of temperature 60 C, voltage 530V, is melted into constant voltage time
For 8min, then in 4% boric acid and 0.02wt% ammonium pentaborate mixed solution, temperature 60 C, voltage 590V under the conditions of carry out
Fourth stage chemical conversion, chemical conversion constant voltage time are 20min, and paillon is then carried out heat treatment 3min at 450 DEG C, and then chemical conversion is repaired
6min then handles 8min at 75 DEG C of 5wt% phosphoric acid solution, then is melted into and repairs 6min, is then heat-treated at 450 DEG C
3min, then be melted into and repair 6min, 2min then is handled in 0.1wt% phosphoric acid solution, finally dries 3min at 150 DEG C.
475V1000 μ F mash welder capacitor is made in obtained anode foils, rapidly charge discharge life is carried out and tests.
The relevant parameter of 1 anode foils of table, capacitor
Find out from 1 result of embodiment, it is smaller than the conventional anodes foil loss tangent (tg δ) of the prior art using the present invention
42%；Capacitor progress is made, and rapidly charge discharge life test, charge and discharge number are 35 times high, temperature rise low 40 after capacitor charging/discharging
℃。
Embodiment 2
One example of the chemical synthesizing method of mash welder capacitor anode foils of the present invention, include the following steps: by
It is boiling for 100 μ s/cm that through borrosion hole structure erosion foil, which is placed in by citric acid and diammonium hydrogen citrate solution composition conductivity,
In treatment fluid, 2.5min is handled at 90 DEG C, then in 5% boric acid and 0.2wt% ammonium pentaborate mixed solution, temperature 50 C,
First order chemical conversion is carried out under the conditions of voltage 190V, chemical conversion constant voltage time is 10min, then in five boric acid of 5% boric acid and 0.1wt%
In ammonium mixed solution, second level chemical conversion is carried out under the conditions of temperature 50 C, voltage 380V, chemical conversion constant voltage time is 10min, is then existed
In 5% boric acid and 0.05wt% ammonium pentaborate mixed solution, third level chemical conversion is carried out under the conditions of temperature 50 C, voltage 570V, is changed
It is 10min at constant voltage time, then in 4% boric acid and 0.015wt% ammonium pentaborate mixed solution, temperature 50 C, voltage
Fourth stage chemical conversion is carried out under the conditions of 630V, chemical conversion constant voltage time is 25min；Then paillon is heat-treated at 480 DEG C
2min, then be melted into and repair 8min, 6min then is handled at 70 DEG C of 7wt% phosphoric acid solution, then be melted into and repair 8min, then existed
Heat treatment 2min is carried out at 480 DEG C, then is melted into and repairs 8min, then 3min is handled in 0.08% phosphoric acid solution, finally at 200 DEG C
Lower drying 2min.
475V1000 μ F mash welder capacitor is made in obtained anode foils, rapidly charge discharge life is carried out and tests.
The relevant parameter of 2 anode foils of table, capacitor
Find out from 2 result of embodiment, it is smaller than the conventional anodes foil loss tangent (tg δ) of the prior art using the present invention
46%；Capacitor progress is made, and rapidly charge discharge life test, charge and discharge number are 39 times high, temperature rise low 40 after capacitor charging/discharging
℃。
Embodiment 3
One example of the chemical synthesizing method of mash welder capacitor anode foils of the present invention, include the following steps: by
It is boiling for 200 μ s/cm that through borrosion hole structure erosion foil, which is placed in by citric acid and ammonium dihydrogen citrate solution composition conductivity,
In treatment fluid, 5min is handled at 85 DEG C, then in 6% boric acid and 0.2wt% ammonium pentaborate mixed solution, 40 DEG C of temperature, electricity
First order chemical conversion is carried out under the conditions of pressure 195V, chemical conversion constant voltage time is 12min；Then in 6% boric acid and 0.1wt% ammonium pentaborate
In mixed solution, second level chemical conversion is carried out under the conditions of 40 DEG C of temperature, voltage 390V, chemical conversion constant voltage time is 12min；Then exist
In 5% boric acid and 0.05wt% ammonium pentaborate mixed solution, third level chemical conversion is carried out under the conditions of 40 DEG C of temperature, voltage 585V, is changed
It is 12min at constant voltage time；Then in 4% boric acid and 0.01wt% ammonium pentaborate mixed solution, 40 DEG C of temperature, voltage 650V
Under the conditions of carry out fourth stage chemical conversion, chemical conversion constant voltage time be 30min；Then paillon is subjected at 500 DEG C heat treatment 1min, connect
Chemical conversion repair 10min, then handle 4min at 65 DEG C of 9wt% phosphoric acid solution, then be melted into repair 10min, then at 500 DEG C
Under carry out heat treatment 1min, then be melted into repair 10min, then 0.06wt% phosphoric acid solution handle 5min, finally at 250 DEG C
Dry 2min.
475V1000 μ F mash welder capacitor is made in obtained anode foils, rapidly charge discharge life is carried out and tests.
The relevant parameter of 3 anode foils of table, capacitor
Find out from 3 result of embodiment, it is smaller than the conventional anodes foil loss tangent (tg δ) of the prior art using the present invention
46%；Capacitor progress is made, and rapidly charge discharge life test, charge and discharge number are 47 times high, temperature rise low 40 after capacitor charging/discharging
℃。
It can be seen that conventional anodes foil oxide film has thicker porous aluminium hydroxide outer layer from Fig. 1,2 anode foils surface SEM photographs
(featheriness outer layer)；And anode foil oxide film of the present invention is substantially free of porous aluminium hydroxide outer layer, loss is low, advantageously reduces hair
Heat greatly improves resistance to rush of current and resistance to temperature rise ability, prolongs the service life.It should be pointed out that above-described embodiment is only to say
Bright technical concepts and features of the invention, its object is to those skilled in the art can understand the contents of the present invention simultaneously
Implement accordingly, it is not intended to limit the scope of the present invention.Equivalence changes made by all Spirit Essences according to the present invention or
Modification, should be covered by the protection scope of the present invention.
Claims (1)
1. a kind of chemical synthesizing method of mash welder capacitor anode foils, which comprises the following steps:
Step 1: boil treatment fluid using citric acid and its ammonium salt solution composition, specifically by citric acid and ammonium dihydrogen citrate or
Diammonium hydrogen citrate or ammonium citrate solution composition, boiling treatment fluid conductivity is 20~200 μ s/cm；
It is boiled in treatment fluid Step 2: being placed in the etched foil of through borrosion hole structure by what citric acid and its ammonium salt formed,
1~5min of processing is boiled at 85~95 DEG C；
Step 3: it is that 4~6wt% boric acid and 0.01~0.3wt% ammonium pentaborate mix that the etched foil for being boiled processing, which is placed in concentration,
Close in solution, carry out level Four chemical conversion at a temperature of 40~60 DEG C, level Four formation voltage be respectively answer alive 30%, 60%,
90%, 100%, the chemical conversion time is 8~30min；
Step 4: being heat-treated to the aluminium foil by level Four chemical conversion, heat treatment temperature is 450~500 DEG C, and heat treatment time is
1~3min；
Step 5: carrying out chemical conversion reparation to thermally treated aluminium foil, chemical conversion repair time is 6~10min；
Step 6: the aluminium foil for being melted into reparation is placed in the phosphoric acid solution that volume ratio is 3~6%, at 60~75 DEG C
Manage 4~8min；
It is repaired Step 7: carrying out secondary chemical conversion, chemical conversion repair time is 6~10min；
Step 8: carrying out secondary heat treatment, treatment temperature is 450~500 DEG C, and the processing time is 1~3min；
It is repaired Step 9: carrying out chemical conversion three times, chemical conversion repair time is 6~10min；
It is handled Step 10: the aluminium foil for being melted into reparation is placed in the phosphoric acid solution that volume ratio is 0.05~0.1% under room temperature
2~5min；
Step 11: the aluminium foil post-processed through peroxophosphoric acid to be made mash welder capacitor and use in 150~250 DEG C of 2~3min of drying
Anode foils.
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| CN109036852B (en) * | 2018-08-13 | 2020-09-18 | 浙江华义瑞东新材料有限公司 | Three-dimensional porous aluminum electrode foil and preparation method thereof |
| CN111139508B (en) * | 2019-01-23 | 2021-11-05 | 东莞东阳光科研发有限公司 | Chemical conversion solution, chemical conversion method, and anode foil |
| CN110295385A (en) * | 2019-06-21 | 2019-10-01 | 广西贺州市桂东电子科技有限责任公司 | A kind of modularization anode foils chemical synthesizing method |
| CN112103084B (en) * | 2020-08-17 | 2021-10-15 | 新疆众和股份有限公司 | Anode foil and preparation method thereof |
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| JPS6362312A (en) * | 1986-09-03 | 1988-03-18 | 日通工株式会社 | Method of forming anode of solid electrolytic capacitor |
| US6299752B1 (en) * | 1999-03-10 | 2001-10-09 | Pacesetter, Inc. | Very high volt oxide formation of aluminum for electrolytic capacitors |
| CN101246779B (en) * | 2008-02-22 | 2010-08-18 | 乳源瑶族自治县东阳光化成箔有限公司 | Production method of medium and high pressure formed foil |
| CN101707141A (en) * | 2009-11-09 | 2010-05-12 | 广西贺州市桂东电子科技有限责任公司 | Method for manufacturing anodic foil of aluminum electrolytic capacitor |
| CN102011167B (en) * | 2010-09-26 | 2012-01-11 | 广西贺州市桂东电子科技有限责任公司 | Electron aluminum foil initial section formation liquid additive and adding method thereof |
| CN102610390B (en) * | 2011-01-20 | 2014-02-19 | 严民 | Method for forming ultrahigh-voltage anode foil for aluminum electrolytic capacitors |
| CN104103428B (en) * | 2013-04-01 | 2018-04-03 | 东莞东阳光科研发有限公司 | A kind of manufacture method of aluminium electrolutic capacitor high pressure high-dielectric formed foil |
| CN103243369B (en) * | 2013-04-10 | 2015-09-30 | 宜都东阳光化成箔有限公司 | A kind of raising used in aluminium electrolytic capactiance mesohigh anode aluminium foil chemical synthesis technology |
| CN107287639A (en) * | 2017-07-11 | 2017-10-24 | 新疆金泰新材料技术有限公司 | A kind of Fabrication of High Specific Capacitance, high warpage, the chemical synthesizing method of Low dark curient electrode foil |
| CN107287638A (en) * | 2017-07-11 | 2017-10-24 | 新疆金泰新材料技术有限公司 | A kind of chemical synthesizing method of large ripple current-resistant electrode foil |
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