CN107502937B - Reduce the chemical synthesizing method of low-pressure chemical synthesis foil leakage current - Google Patents
Reduce the chemical synthesizing method of low-pressure chemical synthesis foil leakage current Download PDFInfo
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- CN107502937B CN107502937B CN201710682549.7A CN201710682549A CN107502937B CN 107502937 B CN107502937 B CN 107502937B CN 201710682549 A CN201710682549 A CN 201710682549A CN 107502937 B CN107502937 B CN 107502937B
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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
- 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
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C28/00—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D
- C23C28/04—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D only coatings of inorganic non-metallic material
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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
- C25D11/06—Anodisation of aluminium or alloys based thereon characterised by the electrolytes used
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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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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G13/00—Apparatus specially adapted for manufacturing capacitors; Processes specially adapted for manufacturing capacitors not provided for in groups H01G4/00 - H01G11/00
Abstract
The present invention relates to a kind of chemical synthesizing method for reducing low-pressure chemical synthesis foil leakage current, the method includes dipping, primary chemical conversion, Passivation Treatment, secondary chemical conversion, three times it is melted into, washes and dry.The electrode foil product leakage current that the method for the present invention obtains significantly reduces, and extends capacitor life-span, and the chemical conversion time shortens, high production efficiency.
Description
Technical field
The present invention relates to the chemical synthesizing method for reducing capacitor anode foils leakage current, it is particularly suitable for reducing low-pressure chemical synthesis foil
The chemical synthesizing method of leakage current.
Background technique
The manufacture of low-voltage aluminum electrolytic capacitor electrode foil need to form one layer of fine and close oxidation film in aluminium foil surface, as
The working media of capacitor.For its method frequently with formation processing method, so-called chemical conversion treatment is at chemistry or electrochemical method
Metal surface is managed, obtains the coating of metallic compound, purpose has improvement corrosion resistance, painting adhesion, metal coloring and chemistry
The effects of grinding.
Chemical conversion system mainly has boric acid to form liquid system at present, phosphoric acid forms liquid system, adipic acid forms liquid system.Institute's body
System haves the defects that different degrees of.
Chinese patent application CN200810154857.3 discloses a kind of low voltage low leakage aluminum electrolysis capacitor electrode
The chemical synthesizing method of foil, comprising the following steps: the 1) aluminium foil after corrosion is placed in temperature is 60~90 DEG C, and mass concentration is adipic acid
In the aqueous solution of ammonium 0.3%~6% and boric acid 1~3%, level-one chemical conversion is carried out；It 2) is 60~90 DEG C in temperature, mass concentration is
In the aqueous solution of ammonium adipate 0.1%~3% and boric acid 1~3%, second level chemical conversion is carried out；3) aluminium foil after being melted into second level is set
It is 50~80 DEG C in temperature, is impregnated 60~120 seconds in the ammonium dihydrogen phosphate aqueous solution that mass concentration is 0.2%~2%；4) it impregnates
Aluminium foil afterwards carries out depolarising processing in heat-treatment furnace；It 5) is 60~90 DEG C in temperature, mass concentration is ammonium adipate 0.1%
~3% and boric acid 1~3% aqueous solution in, be melted into after progress.
Chinese patent application CN200610039700.7 discloses a kind of reduction electrode foil current-leakage for aluminium electrolysis capacitor
Chemical synthesizing method, it is characterized in that: first by purity be 99.99% etched foil be placed in 98 DEG C or more of pure water impregnate 10~15
Minute carry out hydration-treated, then, by this aluminium foil concentration 0.05%~0.5% ammonium pentaborate and 1~10% boric acid 60
Level-one chemical conversion is carried out in~90 DEG C of aqueous solution, and in 0.05%~0.5% ammonium pentaborate and 1~10% boric acid 60~90
DEG C aqueous solution in carry out second level chemical conversion, to repair the defects of anode oxide film, by the heat for carrying out 3 minutes at 500 DEG C
Processing carries out depolarising processing, hereafter, will depolarising treated that aluminium foil is placed in 50~80 DEG C of liquid temperature and the five of 0.05%~2%
Ammonium borate and 1~10% boric acid solution in impregnate 40~100 seconds, later, in 1~10% 60~90 DEG C of boric acid of aqueous solution
Chemical conversion treatment after middle progress, forms required anode oxide film on the surface of aluminium foil.
Chinese patent application CN201210282473.6 discloses a kind of chemical conversion treatment for reducing low-pressure chemical synthesis foil leakage current
Method, which comprises the following steps: A, aluminium foil is placed in the adipate aqueous solution that mass ratio is 0.5~2%,
It is taken out after being impregnated 3 minutes under conditions of 40~60 DEG C；B, quality will be placed in by impregnated aluminium foil in adipate aqueous solution
In the aqueous solution for the adipate that percentage is 3~10%, 65~80 DEG C, current density are 20mA/ ㎝ 2, voltage is 48V's
Under the conditions of, it is melted into 20 minutes, takes out and carry out first wash；C, the aluminium foil after first wash is put into mass percent is 1
~8% phosphate aqueous solution is 50~80 DEG C in temperature, carries out 1~5 minute Passivation Treatment, take out and carry out second wash；
D, the aluminium foil after second wash is placed in adipate that mass percent is 1~5% and mass percent is 0.1~1%
Dihydric phosphate mixed aqueous solution in, 85 DEG C, current density 20mA/cm2, voltage be 48V under conditions of, chemical conversion 5
Minute, it takes out and carries out third time washing；E, the aluminium foil after washing third time carries out 400~550 DEG C of high-temperature heat treatment 1~5
Minute, it is subsequently placed in the biphosphate saline solution that mass percent is 0.1~1%, in 85 DEG C, current density 20mA/
It under conditions of cm2, voltage are 48V, is melted into 5 minutes, takes out, carry out the 4th washing, then dry.
The manufacturing method of anode foils disclosed in the prior art, product leaks electricity, and flow rate is still higher, and there are further improved
Space, and production efficiency is low.
Summary of the invention
The purpose of the present invention is to overcome the above shortcomings, and it is small to provide a kind of product leakage current, improves capacitor and uses
Service life, the chemical synthesizing method of the reduction low-pressure chemical synthesis foil leakage current of high production efficiency.
The purpose of the present invention is achieved through the following technical solutions.
The present invention relates to a kind of chemical synthesizing methods for reducing low-pressure chemical synthesis foil leakage current comprising following steps:
A, the 3,5- dihydroxy-benzoic acid aqueous solution for being 0.5~1% by chemical attack treated aluminium foil is placed in mass ratio
In, it is taken out after impregnating 1-3 minutes at room temperature；
B, will in 3,5- dihydroxy-benzoic acid aqueous solution impregnated aluminium foil be placed in mass percent be 0.5~2.5%
Azelate aqueous solution in, in 60~75 DEG C, current density 35-45mA/cm2, voltage be 40-50V under conditions of, change
At 5-20 minutes, takes out and carry out first wash；
C, by the aluminium foil after first wash be put into mass percent be 1~3% phosphate aqueous solution, temperature be 30~
50 DEG C, 1~3 minute Passivation Treatment is carried out, takes out and carries out second wash；
D, the aluminium foil after second wash is placed in azelate and the mass percent that mass percent is 0.1~1%
In mixed aqueous solution for 0.1~0.5% strontium phosphate, in 70-80 DEG C, current density 45-55mA/cm2, voltage 50-
It under conditions of 60V, is melted into 2-4 minutes, takes out and carry out third time washing；
E, the aluminium foil after washing third time carries out high-temperature heat treatment 1~3 minute of 400-600 DEG C, is subsequently placed in quality
In the strontium phosphate aqueous solution that percentage is 0.1~0.5%, in 70-80 DEG C, current density 55-65mA/cm2, voltage 60-
It under conditions of 70V, is melted into 2-4 minutes, takes out, carry out the 4th washing, then dry, obtain product.
In chemical synthesizing method of the present invention, wherein the azelate is ammonium azelate, azelaic acid sodium or azelaic acid
Potassium.It is preferred that ammonium azelate or azelaic acid sodium.More preferable azelaic acid sodium.
As a preferred implementation manner, the present invention relates to it is a kind of reduce low-pressure chemical synthesis foil leakage current chemical synthesizing method,
The following steps are included:
A, the 3,5- dihydroxy-benzoic acid aqueous solution for being 0.6~1% by chemical attack treated aluminium foil is placed in mass ratio
In, it is taken out after impregnating 1-3 minutes at room temperature；
B, will in 3,5- dihydroxy-benzoic acid aqueous solution impregnated aluminium foil be placed in mass percent be 0.8~2.0%
Azelate aqueous solution in, in 62~72 DEG C, current density 37-43mA/cm2, voltage be 42-48V under conditions of, change
At 7-17 minutes, takes out and carry out first wash；
C, the aluminium foil after first wash is put into the phosphate aqueous solution that mass percent is 1.2~2.6%, is in temperature
34~46 DEG C, 1.5~2.5 minutes Passivation Treatments are carried out, takes out and carries out second wash；
D, the aluminium foil after second wash is placed in the azelate and quality percentage that mass percent is 0.3~0.8%
Than in the mixed aqueous solution for 0.2~0.4% strontium phosphate, in 72-78 DEG C, current density 46-53mA/cm2, voltage be
It under conditions of 52-58V, is melted into 2-4 minutes, takes out and carry out third time washing；
E, the aluminium foil after washing third time carries out high-temperature heat treatment 1~3 minute of 460-540 DEG C, is subsequently placed in quality
In the strontium phosphate aqueous solution that percentage is 0.2~0.4%, in 72-78 DEG C, current density 57-62mA/cm2, voltage 63-
It under conditions of 67V, is melted into 2.5-3.5 minutes, takes out, carry out the 4th washing, then dry, obtain product.
In embodiment of the invention preferred, wherein in above-mentioned steps A, by chemical attack treated aluminium foil
It is placed in 3, the 5- dihydroxy-benzoic acid aqueous solution that mass ratio is 0.8%, is taken out after impregnating 2 minutes at room temperature.
In preferred embodiment of the invention, wherein, will be in 3,5- dihydroxy-benzoic acid water in above-mentioned steps B
Impregnated aluminium foil is placed in the aqueous solution for the azelate that mass percent is 1.5% in solution, is in 70 DEG C, current density
40mA/cm2, voltage be 45V under conditions of, be melted into 10 minutes, take out carry out first wash.
In preferred embodiment of the invention, wherein in above-mentioned steps C, the aluminium foil after first wash is put
Enter the phosphate aqueous solution that mass percent is 2%, is 40 DEG C in temperature, carries out 2 minutes Passivation Treatments, take out and carry out second
Washing.
In preferred embodiment of the invention, wherein in above-mentioned steps D, the aluminium foil after second wash is set
In mass percent be 0.7% azelate and mass percent be 0.3% strontium phosphate mixed aqueous solution in, 75
DEG C, current density 47mA/cm2, voltage be 54V under conditions of, be melted into 2.5 minutes, take out carry out third time washing.
In embodiment of the invention preferred, wherein in above-mentioned steps E, aluminium foil after third time is washed into
The high-temperature heat treatment that 500 DEG C of row 2 minutes is subsequently placed in the strontium phosphate aqueous solution that mass percent is 0.4%, in 75 DEG C, electricity
Current density is 58mA/cm2, voltage be 66V under conditions of, be melted into 2-4 minute, take out, carry out the 4th time wash, then dry,
Obtain product.
In very particularly preferred embodiment of the invention, the chemical synthesizing method of reduction low-pressure chemical synthesis foil leakage current of the invention includes
Following steps:
A, in 3, the 5- dihydroxy-benzoic acid aqueous solution for being 0.8% by chemical attack treated aluminium foil is placed in mass ratio,
It is taken out after impregnating 2 minutes at room temperature.
B, by 3,5- dihydroxy-benzoic acid aqueous solution impregnated aluminium foil be placed in mass percent be 1.5% nonyl two
In the aqueous solution of sour sodium, in 70 DEG C, current density 40mA/cm2, voltage be 45V under conditions of, be melted into 10 minutes, take out into
Row first wash.
C, the aluminium foil after first wash is put into the phosphate aqueous solution that mass percent is 2%, is 40 DEG C in temperature, into
2 minutes Passivation Treatments of row are taken out and carry out second wash.
D, the aluminium foil after second wash is placed in azelaic acid sodium that mass percent is 0.7% and mass percent is
In the mixed aqueous solution of 0.3% strontium phosphate, in 75 DEG C, current density 47mA/cm2, voltage be 54V under conditions of, chemical conversion
It 2.5 minutes, takes out and carries out third time washing.
E, the aluminium foil after washing third time carries out high-temperature heat treatment 2 minutes of 500 DEG C, and being subsequently placed in mass percent is
In 0.4% strontium phosphate aqueous solution, in 75 DEG C, current density 58mA/cm2, under conditions of voltage is 66V, chemical conversion 2-4 point
Clock takes out, and carries out the 4th washing, then dries, obtain product.
In the method for the invention, it is found surprisingly that, 3,5- dihydroxy-benzoic acid dipping solutions are melted into molten with azelate
The fit applications of liquid, azelate+strontium phosphate mixing chemical solution and strontium phosphate chemical solution, and it is each to cooperate screening to obtain
Specific current density and voltage conditions, the electric leakage flow rate of obtained product substantially reduce in chemical conversion treatment, and due to chemical conversion
The production efficiency of the shortening of time, anode foils greatly improves.
Specific embodiment
In order to deepen the understanding of the present invention, the present invention will be described in further detail with reference to the examples below, the embodiment
For explaining only the invention, it is not intended to limit the scope of the present invention..
Embodiment 1
Aluminium foil that learn from else's experience excessive erosion, that purity is 99.9%, is placed in 3, the 5- dihydroxy benzenes that mass ratio is 0.8% for aluminium foil
In aqueous formic acid, taken out after impregnating 2 minutes at room temperature；It will be impregnated in 3,5- dihydroxy-benzoic acid aqueous solution
Aluminium foil be placed in mass percent be 1.5% azelaic acid sodium aqueous solution in, in 70 DEG C, current density 40mA/cm2, electricity
It under conditions of pressure is 45V, is melted into 10 minutes, takes out and carry out first wash；Aluminium foil after first wash is put into quality hundred
Divide the phosphate aqueous solution than being 2%, is 40 DEG C in temperature, carries out 2 minutes Passivation Treatments, taking-up carries out second wash；It will
Aluminium foil after second wash is placed in the azelaic acid sodium that mass percent is 0.7% and the strontium phosphate that mass percent is 0.3%
Mixed aqueous solution in, in 75 DEG C, current density 47mA/cm2, voltage be 54V under conditions of, be melted into 2.5 minutes, take out into
Row third time is washed；Aluminium foil after third time is washed carries out high-temperature heat treatment 2 minutes of 500 DEG C, is subsequently placed in quality percentage
Than in the strontium phosphate aqueous solution for 0.4%, in 75 DEG C, current density 58mA/cm2, voltage be 66V under conditions of, be melted into 2-4
Minute, it takes out, carries out the 4th washing, then dry, obtain product.
Embodiment 2
Aluminium foil that learn from else's experience excessive erosion, that purity is 99.9%, is placed in 3, the 5- dihydroxy benzenes that mass ratio is 0.6% for aluminium foil
In aqueous formic acid, taken out after impregnating 3 minutes at room temperature；It will be impregnated in 3,5- dihydroxy-benzoic acid aqueous solution
Aluminium foil be placed in mass percent be 0.8% azelaic acid sodium aqueous solution in, in 62 DEG C, current density 37mA/cm2, electricity
It under conditions of pressure is 42V, is melted into 17 minutes, takes out and carry out first wash；Aluminium foil after first wash is put into quality hundred
Divide the phosphate aqueous solution than being 1.2%, is 34 DEG C in temperature, carries out 2.5 minutes Passivation Treatments, taking-up carries out second of water
It washes；Aluminium foil after second wash is placed in the azelaic acid sodium that mass percent is 0.3% and the phosphorus that mass percent is 0.2%
In the mixed aqueous solution of sour strontium, in 72 DEG C, current density 46mA/cm2, voltage be 52V under conditions of, be melted into 4 minutes, take out
Carry out third time washing；
E, the aluminium foil after washing third time carries out high-temperature heat treatment 3 minutes of 460 DEG C, and being subsequently placed in mass percent is
In 0.2% strontium phosphate aqueous solution, in 72 DEG C, current density 57mA/cm2, voltage be 63V under conditions of, be melted into 3.5 points
Clock takes out, and carries out the 4th washing, then dries, obtain product.
Embodiment 3
Aluminium foil that learn from else's experience excessive erosion, that purity is 99.9%, is placed in 3, the 5- dihydroxy benzenes first that mass ratio is 1% for aluminium foil
In aqueous acid, taken out after impregnating 1 minute at room temperature；It will be impregnated in 3,5- dihydroxy-benzoic acid aqueous solution
Aluminium foil is placed in the aqueous solution for the azelaic acid sodium that mass percent is 2.0%, in 72 DEG C, current density 43mA/cm2, voltage
It under conditions of 48V, is melted into 7 minutes, takes out and carry out first wash；Aluminium foil after first wash is put into mass percent
For 2.6% phosphate aqueous solution, it is 46 DEG C in temperature, carries out 1.5 minutes Passivation Treatments, take out and carry out second wash；It will
Aluminium foil after second wash is placed in the azelaic acid sodium that mass percent is 0.8% and the strontium phosphate that mass percent is 0.4%
Mixed aqueous solution in, in 78 DEG C, current density 53mA/cm2, voltage be 58V under conditions of, be melted into 2 minutes, take out carry out
Third time is washed；
E, the aluminium foil after washing third time carries out high-temperature heat treatment 1 minute of 540 DEG C, and being subsequently placed in mass percent is
In 0.4% strontium phosphate aqueous solution, in 78 DEG C, current density 62mA/cm2, voltage be 67V under conditions of, be melted into 2.5 points
Clock takes out, and carries out the 4th washing, then dries, obtain product.
Embodiment 4
Aluminium foil that learn from else's experience excessive erosion, that purity is 99.9%, is placed in 3, the 5- dihydroxy benzenes that mass ratio is 0.6% for aluminium foil
In aqueous formic acid, taken out after impregnating 3 minutes at room temperature；It will be impregnated in 3,5- dihydroxy-benzoic acid aqueous solution
Aluminium foil be placed in mass percent be 0.6% azelaic acid sodium aqueous solution in, in 61 DEG C, current density 36mA/cm2, electricity
It under conditions of pressure is 42V, is melted into 18 minutes, takes out and carry out first wash；Aluminium foil after first wash is put into quality hundred
Divide the phosphate aqueous solution than being 1.2%, is 32 DEG C in temperature, carries out 2.8 minutes Passivation Treatments, taking-up carries out second of water
It washes；Aluminium foil after second wash is placed in the azelaic acid sodium that mass percent is 0.2% and the phosphorus that mass percent is 0.4%
In the mixed aqueous solution of sour strontium, in 72 DEG C, current density 44mA/cm2, voltage be 51V under conditions of, be melted into 4 minutes, take out
Carry out third time washing；Aluminium foil after third time is washed carries out high-temperature heat treatment 3 minutes of 420 DEG C, is subsequently placed in quality hundred
Divide in the strontium phosphate aqueous solution than being 0.2%, in 72 DEG C, current density 55mA/cm2, voltage be 61V under conditions of, chemical conversion 4
Minute, it takes out, carries out the 4th washing, then dry, obtain product.
Embodiment 5
Aluminium foil that learn from else's experience excessive erosion, that purity is 99.9%, is placed in 3, the 5- dihydroxy benzenes that mass ratio is 0.9% for aluminium foil
In aqueous formic acid, taken out after impregnating 1 minute at room temperature；It will be impregnated in 3,5- dihydroxy-benzoic acid aqueous solution
Aluminium foil be placed in mass percent be 2.5% azelaic acid sodium aqueous solution in, in 75 DEG C, current density 44mA/cm2, electricity
It under conditions of pressure is 50V, is melted into 6 minutes, takes out and carry out first wash；Aluminium foil after first wash is put into quality percentage
Than the phosphate aqueous solution for 3%, it is 50 DEG C in temperature, carries out 1 minute Passivation Treatment, take out and carry out second wash；By
Aluminium foil after secondary washing is placed in the mixed of the azelaic acid sodium that mass percent is 1% and the strontium phosphate that mass percent is 0.1%
In Heshui solution, in 80 DEG C, current density 54mA/cm2, voltage be 59V under conditions of, be melted into 2 minutes, take out carry out third
Secondary washing；Aluminium foil after third time is washed carries out high-temperature heat treatment 1 minute of 600 DEG C, and being subsequently placed in mass percent is
In 0.5% strontium phosphate aqueous solution, in 80 DEG C, current density 65mA/cm2, voltage be 70V under conditions of, be melted into 2 minutes,
It takes out, carries out the 4th washing, then dry, obtain product.
Comparative example 1
It is water-soluble to be placed in the adipic acid sodium that mass ratio is 0.5% by aluminium foil that learn from else's experience excessive erosion, that purity is 99.9% for aluminium foil
In liquid, taken out after being impregnated 3 minutes under conditions of 50 DEG C；Quality hundred will be placed in by impregnated aluminium foil in adipic acid sodium water solution
Divide than being 20mA/ ㎝ in 72 DEG C, current density in the aqueous solution for 8% adipic acid sodium2, voltage be 48V under conditions of, change
At 20 minutes, takes out and carry out first wash；It is water-soluble that aluminium foil after first wash is put into the phosphoric acid that mass percent is 6%
Liquid is 55 DEG C, carries out 1~5 minute Passivation Treatment, takes out and carry out second wash in temperature；By the aluminium after second wash
Foil is placed in the mixed aqueous solution of the adipic acid sodium that mass percent is 2% and the dihydric phosphate that mass percent is 0.1%,
In 85 DEG C, current density 20mA/cm2, voltage be 48V under conditions of, be melted into 5 minutes, take out carry out third time washing；By
Aluminium foil after washing three times carries out high-temperature heat treatment 3 minutes of 480 DEG C, is subsequently placed in the di(2-ethylhexyl)phosphate that mass percent is 0.1%
In hydrogen salt aqueous solution, in 85 DEG C, current density 20mA/cm2, voltage be 48V under conditions of, be melted into 5 minutes, take out, carry out
4th washing, is then dried.
Comparative example 2
It is water-soluble to be placed in the adipic acid sodium that mass ratio is 0.8% by aluminium foil that learn from else's experience excessive erosion, that purity is 99.9% for aluminium foil
In liquid, taken out after being impregnated 3 minutes under conditions of 60 DEG C；Quality hundred will be placed in by impregnated aluminium foil in adipic acid sodium water solution
Divide than being 20mA/ ㎝ in 78 DEG C, current density in the aqueous solution for 5% adipic acid sodium2, voltage be 48V under conditions of, change
At 20 minutes, takes out and carry out first wash；It is water-soluble that aluminium foil after first wash is put into the phosphoric acid that mass percent is 6%
Liquid is 55 DEG C, carries out 1~5 minute Passivation Treatment, takes out and carry out second wash in temperature；By the aluminium after second wash
Foil is placed in the mixed aqueous solution of the adipic acid sodium that mass percent is 4% and the dihydric phosphate that mass percent is 0.5%,
In 85 DEG C, current density 20mA/cm2, voltage be 48V under conditions of, be melted into 5 minutes, take out carry out third time washing；By
Aluminium foil after washing three times carries out high-temperature heat treatment 3 minutes of 500 DEG C, is subsequently placed in the di(2-ethylhexyl)phosphate that mass percent is 0.2%
In hydrogen salt aqueous solution, in 85 DEG C, current density 20mA/cm2, voltage be 48V under conditions of, be melted into 5 minutes, take out, carry out
4th washing, is then dried.
By electrode foil that 1-5 of the embodiment of the present invention is obtained compared with the electrode foil that comparative example 1-2 is obtained carries out performance, as a result
It is as in the table below:
Said determination result is not difficult to find out that the magnitude of leakage current for the electrode foil that the method for the present invention obtains is far smaller than comparative example side
Method, 1 method of embodiment must beat the magnitude of leakage current of even electrode foil as minimum, be most preferred method.In addition, the method for the present invention obtains
The electrode foil arrived capacity after storage 60 days is substantially unchanged, and the capacity for the electrode foil that control methods obtains then decreases.
Although detailed description has been made to the present invention, and some specific examples are listed, to those skilled in the art
For member, as long as it does not depart from the spirit of the invention, and the various adjustment done to this method are regarded as being included in model of the invention
In enclosing.
Claims (7)
1. a kind of chemical synthesizing method for reducing low-pressure chemical synthesis foil leakage current, which comprises the following steps:
A, in 3, the 5- dihydroxy-benzoic acid aqueous solution for being 0.5~1% by chemical attack treated aluminium foil is placed in mass ratio,
It is taken out after being impregnated 1-3 minutes under conditions of room temperature；
B, by 3,5- dihydroxy-benzoic acid aqueous solution impregnated aluminium foil be placed in mass percent be 0.5~2.5% nonyl
In the aqueous solution of diacid salt, in 60~75 DEG C, current density 35-45mA/cm2, voltage be 40-50V under conditions of, be melted into 5-
It 20 minutes, takes out and carries out first wash；
C, the aluminium foil after first wash is put into the phosphate aqueous solution that mass percent is 1~3%, is 30~50 in temperature
DEG C, 1~3 minute Passivation Treatment is carried out, takes out and carries out second wash；
D, the aluminium foil after second wash is placed in azelate that mass percent is 0.1~1% and mass percent is 0.1
In the mixed aqueous solution of~0.5% strontium phosphate, in 70-80 DEG C, current density 45-55mA/cm2, voltage be 50-60V
Under the conditions of, it is melted into 2-4 minutes, takes out and carry out third time washing；
E, the aluminium foil after washing third time carries out high-temperature heat treatment 1~3 minute of 460-540 DEG C, is subsequently placed in quality percentage
Than in the strontium phosphate aqueous solution for 0.1~0.5%, in 70-80 DEG C, current density 55-65mA/cm2, voltage be 60-70V
Under the conditions of, it is melted into 2-4 minutes, takes out, carry out the 4th washing, then dry.
2. chemical synthesizing method according to claim 1, which is characterized in that in step, by chemical attack treated aluminium foil
It is placed in 3, the 5- dihydroxy-benzoic acid aqueous solution that mass ratio is 0.6~1%, is taken after impregnating 1-3 minutes at room temperature
Out.
3. chemical synthesizing method according to claim 1, which is characterized in that in stepb, will be in 3,5- dihydroxy-benzoic acid water
In solution impregnated aluminium foil be placed in mass percent be 0.8~2.0% azelate aqueous solution in, 62~72 DEG C,
Current density is 37-43mA/cm2, voltage be 42-48V under conditions of, be melted into 7-17 minute, take out progress first wash.
4. chemical synthesizing method according to claim 1, which is characterized in that in step C, the aluminium foil after first wash is put
Enter the phosphate aqueous solution that mass percent is 1.2~2.6%, is 34~46 DEG C in temperature, carries out passivation in 1.5~2.5 minutes
Processing takes out and carries out second wash.
5. chemical synthesizing method according to claim 1, which is characterized in that in step D, the aluminium foil after second wash is set
In mass percent be 0.3~0.8% azelate and mass percent be 0.2~0.4% strontium phosphate mixing it is water-soluble
In liquid, in 72-78 DEG C, current density 46-53mA/cm2, voltage be 52-58V under conditions of, be melted into 2-4 minutes, take out into
Row third time is washed.
6. chemical synthesizing method according to claim 1, which is characterized in that in step E, by third time wash after aluminium foil into
460-540 DEG C of row of high-temperature heat treatment 1~3 minute is subsequently placed in the strontium phosphate aqueous solution that mass percent is 0.2~0.4%
In, in 72-78 DEG C, current density 57-62mA/cm2, voltage be 63-67V under conditions of, be melted into 2.5-3.5 minute, taking-up,
The 4th washing is carried out, is then dried.
7. chemical synthesizing method according to claim 1, it is characterised in that: the azelate is ammonium azelate, azelaic acid sodium
Or azelaic acid potassium.
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| US4113579A (en) * | 1977-04-28 | 1978-09-12 | Sprague Electric Company | Process for producing an aluminum electrolytic capacitor having a stable oxide film |
| CN1117182C (en) * | 2001-01-19 | 2003-08-06 | 江苏中联科技集团有限公司 | Three-stage process for preparing electrode foil used for middle-and high-voltage aluminium-electrolytic capacitor |
| CN1117185C (en) * | 2001-01-19 | 2003-08-06 | 江苏中联科技集团有限公司 | Four-stage process for preparing electrode foil of middle-and high-voltage aluminium-electrolytic capacitor |
| CN101819886B (en) * | 2010-04-27 | 2011-09-07 | 四川中雅科技有限公司 | Method for manufacturing electrode foil capable of preventing current jump during formation |
| CN101826397B (en) * | 2010-04-27 | 2011-09-07 | 四川中雅科技有限公司 | Five-stage manufacturing method of electrode foil for medium-high voltage aluminium electrolytic capacitor |
| CN102129913A (en) * | 2010-12-27 | 2011-07-20 | 东莞宏强电子有限公司 | Preparation method of sheet type aluminum electrolytic capacitor |
| CN102800483B (en) * | 2012-08-10 | 2015-05-20 | 南通海星电子股份有限公司 | Formation processing method for reducing leaking current of low-voltage formation foil |
| CN103151174B (en) * | 2013-03-06 | 2016-03-30 | 佛山科学技术学院 | The manufacture method of electrode foil of high-pressure aluminum electrolytic capacitor |
| CN103258649B (en) * | 2013-05-15 | 2016-04-13 | 南通海星电子股份有限公司 | Improve the formation processing method of low-pressure chemical synthesis foil resistance to water |
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