CN108376611A - A kind of production method of no foil ash medium-high pressure chemical foil - Google Patents
A kind of production method of no foil ash medium-high pressure chemical foil Download PDFInfo
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- CN108376611A CN108376611A CN201711486774.XA CN201711486774A CN108376611A CN 108376611 A CN108376611 A CN 108376611A CN 201711486774 A CN201711486774 A CN 201711486774A CN 108376611 A CN108376611 A CN 108376611A
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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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- 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
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Abstract
The present invention discloses a kind of production method of no foil ash medium-high pressure chemical foil, including mesohigh etched foil is successively carried out pre-treatment, multistage chemical conversion treatment, high-temperature roasting is handled, primary chemical conversion repair process, secondary chemical conversion repair process, secondary high-temperature calcination process, it is melted into repair process and post-processing three times, between the primary chemical conversion repair process and secondary chemical conversion repair process, it is handled in addition, the middle processing, it is that the etched foil after primary chemical conversion repair process is used into phosphoric acid solution pickling, a concentration of 1.4 ~ the 2.0mol/L of phosphoric acid solution, pickling temperature is 60 ~ 80 DEG C, pickling time is 8 ~ 20min.Present invention firstly discovers that existing relationship between foil ash and aluminium electrolutic capacitor performance, removes Waste Acid From Hua Cheng Foil ashes by adding processing step in phosphoric acid pickling, can improve dust Control and aluminium electrolutic capacitor punch-through that aluminium electrolutic capacitor manufacture cuts process.
Description
Technical field
The present invention relates to anode foil for aluminum electrolytic capacitor corrosion technology field, especially a kind of no foil ash mesohigh chemical conversion
The production method of foil.
Background technology
Long-life and miniaturization are the inexorable trends of aluminium electrolutic capacitor development.By to having the high-purity of { 100 } texture
Aluminium foil carries out electrolytic etching to expand its specific surface area, improve specific capacitance, is that aluminium electrolutic capacitor minimizes most effective technology
Approach.
Currently, the chemical synthesis technology of mesohigh aluminium foil generally comprises pre-treatment, level-one chemical conversion treatment, two level chemical conversion treatment, three
Grade chemical conversion treatment, level Four chemical conversion treatment, high-temperature roasting processing are once melted into repair process, middle processing, secondary chemical conversion reparation
Processing, secondary high-temperature calcination process are melted into 12 steps of repair process and post-processing three times.Mesohigh aluminium foil surface forms densification
Crystal type oxidation film, be the key that obtain high quality Waste Acid From Hua Cheng Foil.The main function of pre-treatment is to generate aqua oxidation film, is carried
High Waste Acid From Hua Cheng Foil static capacity；The effect of multistage chemical conversion treatment is that hydrated film is allowed gradually to be converted into crystal type oxidation film；High-temperature roasting
The effect of processing is that most of oxidation film is made to be converted into γ '-Al2O3 ；Repeatedly the effect of chemical conversion repair process is to repair oxidation
Film；The main function of post-processing generates phosphoric acid composite membrane, improves the anti-hydration of Waste Acid From Hua Cheng Foil.
It is that the pellumina of a part has been dissolved with phosphoric acid after post-processing to have research at present, generates phosphating coat.These objects
Matter may make alumite to reduce aquation sensitivity, to play passivation, improve Waste Acid From Hua Cheng Foil and its capacitor production
The resistance to hydrability of product, such as application number 200710124278.X and 200610063522.1, but not yet find by remove foil ash this
One approach improves the research of aluminium electrolutic capacitor performance.
Invention content
Present invention aim to address above-mentioned technical problems, provide a kind of foil ash that can remove Waste Acid From Hua Cheng Foil remained on surface, drop
Low Waste Acid From Hua Cheng Foil leakage current and the production method without foil ash medium-high pressure chemical foil for improving Waste Acid From Hua Cheng Foil electrical property.
To realize above-mentioned purpose, the technical scheme is that：
A kind of production method of no foil ash medium-high pressure chemical foil, including mesohigh etched foil is successively subjected to pre-treatment, multipolarity
At processing, high-temperature roasting processing, once it is melted into repair process, secondary chemical conversion repair process, secondary high-temperature calcination process, three
Secondary chemical conversion repair process and post-processing, between the primary chemical conversion repair process and secondary chemical conversion repair process, in addition
Reason, the middle processing are to use phosphoric acid solution pickling, the phosphoric acid solution dense etched foil after primary chemical conversion repair process
Degree is 1.4 ~ 2.0mol/L, and pickling temperature is 60 ~ 80 DEG C, and pickling time is 8 ~ 20min.
As further technical solution, pre-treatment described above, be by mesohigh etched foil be placed on temperature be 92 DEG C with
On pure water in impregnate 3 ~ 20min.
As further technical solution, multistage chemical conversion treatment described above, step includes：
（1）Level-one chemical conversion treatment：The level-one that 85 ~ 90 DEG C of temperature is placed in by the etched foil after pre-treatment is melted into corrosive liquid
In, apply 50 ~ 200V voltages, constant pressure handles 5 ~ 10min；The level-one is melted into corrosive liquid, be boric acid that mass content is 3% and
The mixed solution of 0.5 ~ 1 ‰ trace mineral supplements；It is set to produce the oxidation film of certain proof voltage.
（2）Two level chemical conversion treatment：The two level of 85 ~ 90 DEG C of temperature will be placed in by the etched foil after level-one chemical conversion treatment
At 100 ~ 380V voltages are applied in corrosive liquid, constant pressure handles 5 ~ 10min；It is 3% that the two level chemical conversion corrosive liquid, which is mass content,
Boric acid and 0.5 ~ 1 ‰ trace mineral supplements mixed solution；It is set to produce the oxidation film of certain proof voltage.
（3）Three-level chemical conversion treatment：The three-level of 85 ~ 90 DEG C of temperature will be placed in by the etched foil after two level chemical conversion treatment
At 180 ~ 660V voltages are applied in corrosive liquid, constant pressure handles 5 ~ 15min；It is 5% that the three-level chemical conversion corrosive liquid, which is mass content,
Boric acid and 0.5 ~ 1 ‰ trace mineral supplements mixed solution；It is set to produce the oxidation film of certain proof voltage.
（4）Level Four chemical conversion treatment：Etched foil after three-level chemical conversion treatment is placed in the level Four chemical conversion of 85 ~ 90 DEG C of temperature
Apply 200 ~ 750V voltages in corrosive liquid, constant pressure handles 15 ~ 30min；It is 5% that the level Four chemical conversion corrosive liquid, which is mass content,
The mixed solution of boric acid and 0.5 ~ 1 ‰ trace mineral supplements, makes it produce the oxidation film of certain proof voltage.
As further technical solution, high-temperature roasting processing described above, being will be after level Four chemical conversion treatment
Etched foil carries out high-temperature roasting at 450 ~ 550 DEG C, and roasting time is 2 ~ 3min.
As further technical solution, primary chemical conversion repair process described above, is that will pass through at a high-temperature roasting
Etched foil after reason, which is placed in the primary chemical conversion reparation liquid of 85 ~ 90 DEG C of temperature, applies 200 ~ 750V voltages, and constant pressure processing 5 ~
Liquid is repaired in 10min, the primary chemical conversion, is the mixed solution of boric acid and 0.5 ~ 1 ‰ trace mineral supplements that mass content is 5%,
Its alumina diaphragm defect opened in high-temperature roasting processing is set to be repaired.
As further technical solution, secondary chemical conversion repair process described above is the corruption after being handled in passing through
Erosion foil be placed in 85 ~ 90 DEG C of temperature secondary chemical conversion repair liquid in apply 200 ~ 750V voltages, constant pressure handle 5 ~ 10min, described two
Liquid is repaired in secondary chemical conversion, is the mixed solution of boric acid and 0.5 ~ 1 ‰ trace mineral supplements that mass content is 5%, is made it in middle processing
The alumina diaphragm defect of opening is repaired.
As further technical solution, secondary high-temperature calcination process described above, be by secondary chemical conversion repair process it
Etched foil afterwards carries out high-temperature roasting at 450 ~ 550 DEG C, and roasting time is 2 ~ 3min.
As further technical solution, the above is melted into repair process three times, is that will pass through at secondary high-temperature roasting
Etched foil after reason, which is placed in the reparation liquid of chemical conversion three times of 85 ~ 90 DEG C of temperature, applies 200 ~ 750V voltages, and constant pressure processing 5 ~
Liquid is repaired in 10min, the chemical conversion three times, is the mixed solution of boric acid and 0.5 ~ 1 ‰ trace mineral supplements that mass content is 5%,
Its alumina diaphragm defect opened in secondary high-temperature calcination process is set to be repaired.
As further technical solution, the above post-processing is to be placed in the etched foil of chemical conversion repair process three times
4 ~ 12min is handled in 70 ~ 80 DEG C of phosphoric acid,diluted or phosphate solution.
As further technical solution, trace mineral supplement described above is one kind or two in ammonium pentaborate and citric acid
Kind combination.
The used mesohigh etched foil of the present invention is the mesohigh etched foil of average effective pore >=1.2 μm.
It has been investigated that the essence of medium-high pressure chemical foil foil ash of the present invention is the outermost porous type oxygen of anode oxide film
Change film and least a portion of aluminium powder, Porosity anodic oxide film short texture, without insulation characterisitic, in aluminium electrolutic capacitor, excessive
The presence of Porosity anodic oxide film, will increase the leakage current of aluminium electrolutic capacitor, while increase the thickness of anode oxide film, cause
Capacity declines, and is unfavorable for improving aluminium electrolytic capacitor product stability.The present invention medium-high pressure chemical foil oxidation film together with
Aluminum substrate is cut into ultra-thin cross sectional slice together, in perspective Electronic Speculum（TEM）Lower observation, it is possible to find aluminium anode oxide film is divided into Barrier
And porous type, internal layer are Barrier, outer layer is porous type, is in featheriness.When aluminium electrolutic capacitor applies DC voltage, will see
The variation of charging current is observed, starts very big, the then gradually decline with charging time extension, but do not terminate in zero, but arrives certain
Reach relatively stable state after one numerical value, this final value is known as leakage current, and anode foils leakage current value reflects the exhausted of oxidation film
Edge characteristic.Aluminium anodes Porosity anodic oxide film, without insulation characterisitic, it directly influences anode foils leakage in the amount of anode foils
Current value.Aluminium anodes Porosity anodic oxide film density only has 2.3g/cm3, excessive Porosity anodic oxide film increases anode oxide film
Thickness, cause specific volume relatively low, in addition, in aluminium electrolutic capacitor, blocked up anode foils Surface porous oxidation film can hinder
Electrolyte penetrates into anode foil oxide film Tunnel-hole, and effective ratio is caused to hold drop.It, can be in medium-high pressure chemical foil manufacturing process
Foil ash is eliminated by way of pickling, that is, eliminates Porosity anodic oxide film, but if pickling is not thorough, also more porous type oxygen
Change film not dissolve, medium-high pressure chemical foil is after drying, and surface can also remain the aluminium powder of many grey, by adjusting mesohigh
The pickling parameter of Waste Acid From Hua Cheng Foil production process achievees the purpose that appropriate removal medium-high pressure chemical foil foil ash.
Compared with prior art, beneficial effects of the present invention are：Present invention firstly discovers that foil ash and aluminium electrolutic capacitor
Existing relationship between energy removes Waste Acid From Hua Cheng Foil ashes by adding processing step in phosphoric acid pickling, can improve aluminium electrolutic capacitor
Manufacture cuts the dust Control and aluminium electrolutic capacitor punch-through of process；Medium-high pressure chemical foil ashes is removed, may also reach up
Reduction Waste Acid From Hua Cheng Foil leakage current and raising etched foil specific volume conversion ratio, this is that have with what is minimized the solution aluminium electrolutic capacitor long-life
One of effect approach.
Specific implementation mode
With reference to embodiment, the present invention is described in further detail.
Comparative example 1
（1）Pre-treatment：It is 96 DEG C that mesohigh etched foil, which is placed on temperature, and pure water of the resistance more than 1M Ω impregnates 12min；
（2）Level-one chemical conversion treatment：By the etched foil after pre-treatment be placed in temperature be 90 DEG C, mass content be 3% boric acid and
The mixed solution of 0.5 ‰ ammonium pentaborates, applies 150V voltages, and constant pressure handles 10min；
（3）Two level chemical conversion treatment：It is 90 DEG C that etched foil after level-one chemical conversion treatment, which is placed in temperature, and mass content is 3% boric acid
With the mixed solution of 0.5 ‰ ammonium pentaborates, apply 310V voltages, constant pressure handles 10min；
（4）Three-level chemical conversion treatment：It is 90 DEG C that etched foil after two level chemical conversion treatment, which is placed in temperature, and mass content is 5% boric acid
With the mixed solution of 0.5 ‰ ammonium pentaborates, apply 470V voltages, constant pressure handles 15min；
（5）Level Four chemical conversion treatment：It is 90 DEG C that etched foil after three-level chemical conversion treatment, which is placed in temperature, and mass content is 5% boric acid
With the mixed solution of 0.5 ‰ ammonium pentaborates, apply 530V voltages, constant pressure handles 25min；
（6）High-temperature roasting is handled：Etched foil after level Four chemical conversion treatment is placed in the high temperature furnace that temperature is 500 DEG C and is roasted
Burn 2min；
（7）Primary chemical conversion repair process：It is 90 DEG C that etched foil after high-temperature roasting is handled, which is placed in temperature, mass content
For the mixed solution of 5% boric acid and 0.5 ‰ ammonium pentaborates, apply 530V voltages, constant pressure handles 10min；
（8）Secondary chemical conversion repair process：It is 90 DEG C that etched foil after primary repair, which is placed in temperature, and mass content is 5% boric acid
With the mixed solution of 0.5 ‰ ammonium pentaborates, apply 530V voltages, constant pressure handles 10min；
（9）Secondary high-temperature calcination process：Etched foil after secondary chemical conversion treatment is placed in the high temperature furnace that temperature is 500 DEG C and is roasted
Burn 2min；
（10）It is melted into repair process three times：It is 90 DEG C that etched foil after secondary high-temperature calcination process, which is placed in temperature, and quality contains
Amount is the mixed solution of 5% boric acid and 0.5 ‰ ammonium pentaborates, applies 530V voltages, and constant pressure handles 10min；
（11）Post-processing：Etched foil after three-level chemical conversion is repaired is placed on 80 DEG C, handles 8min in 0.4% sodium radio-phosphate,P-32 solution.
Comparative example 2
（1）Pre-treatment：It is 96 DEG C that mesohigh etched foil, which is placed on temperature, and pure water of the resistance more than 1M Ω impregnates 12min；
（2）Level-one chemical conversion treatment：By the etched foil after pre-treatment be placed in temperature be 90 DEG C, mass content be 3% boric acid and
The mixed solution of 0.5 ‰ ammonium pentaborates, applies 150V voltages, and constant pressure handles 10min；
（3）Two level chemical conversion treatment：It is 90 DEG C that etched foil after level-one chemical conversion treatment, which is placed in temperature, and mass content is 3% boric acid
With the mixed solution of 0.5 ‰ ammonium pentaborates, apply 310V voltages, constant pressure handles 10min；
（4）Three-level chemical conversion treatment：It is 90 DEG C that etched foil after two level chemical conversion treatment, which is placed in temperature, and mass content is 5% boric acid
With the mixed solution of 0.5 ‰ ammonium pentaborates, apply 470V voltages, constant pressure handles 15min；
（5）Level Four chemical conversion treatment：It is 90 DEG C that etched foil after three-level chemical conversion treatment, which is placed in temperature, and mass content is 5% boric acid
With the mixed solution of 0.5 ‰ ammonium pentaborates, apply 530V voltages, constant pressure handles 25min；
（6）High-temperature roasting is handled：Etched foil after level Four chemical conversion treatment is placed in the high temperature furnace that temperature is 500 DEG C and is roasted
Burn 2min；
（7）Primary chemical conversion repair process：It is 90 DEG C that etched foil after high-temperature roasting is handled, which is placed in temperature, mass content
For the mixed solution of 5% boric acid and 0.5 ‰ ammonium pentaborates, apply 530V voltages, constant pressure handles 10min；
（8）Middle processing：Etched foil uses phosphoric acid solution pickling, phosphoric acid solution a concentration of after repair process will be once melted into
1.0mol/L, pickling temperature are 55 DEG C, pickling time 7min；
（9）Secondary chemical conversion repair process：It is 90 DEG C that etched foil after primary repair, which is placed in temperature, and mass content is 5% boric acid
With the mixed solution of 0.5 ‰ ammonium pentaborates, apply 530V voltages, constant pressure handles 10min；
（10）Secondary high-temperature calcination process：Etched foil after secondary chemical conversion treatment is placed in the high temperature furnace that temperature is 500 DEG C
Roast 2min；
（11）It is melted into repair process three times：It is 90 DEG C that etched foil after secondary high-temperature calcination process, which is placed in temperature, and quality contains
Amount is the mixed solution of 5% boric acid and 0.5 ‰ ammonium pentaborates, applies 530V voltages, and constant pressure handles 10min；
（12）Post-processing：Etched foil after three-level chemical conversion is repaired is placed on 80 DEG C, handles 8min in 0.4% sodium radio-phosphate,P-32 solution.
Embodiment 1
A kind of production method of no foil ash medium-high pressure chemical foil, step are：
（1）Pre-treatment：It is 96 DEG C that mesohigh etched foil, which is placed on temperature, and pure water of the resistance more than 1M Ω impregnates 12min；
（2）Level-one chemical conversion treatment：By the etched foil after pre-treatment be placed in temperature be 90 DEG C, mass content be 3% boric acid and
The mixed solution of 0.5 ‰ ammonium pentaborates, applies 150V voltages, and constant pressure handles 10min；
（3）Two level chemical conversion treatment：It is 90 DEG C that etched foil after level-one chemical conversion treatment, which is placed in temperature, and mass content is 3% boric acid
With the mixed solution of 0.5 ‰ ammonium pentaborates, apply 310V voltages, constant pressure handles 10min；
（4）Three-level chemical conversion treatment：It is 90 DEG C that etched foil after two level chemical conversion treatment, which is placed in temperature, and mass content is 5% boric acid
With the mixed solution of 0.5 ‰ ammonium pentaborates, apply 470V voltages, constant pressure handles 15min；
（5）Level Four chemical conversion treatment：It is 90 DEG C that etched foil after three-level chemical conversion treatment, which is placed in temperature, and mass content is 5% boric acid
With the mixed solution of 0.5 ‰ ammonium pentaborates, apply 530V voltages, constant pressure handles 25min；
（6）High-temperature roasting is handled：Etched foil after level Four chemical conversion treatment is placed in the high temperature furnace that temperature is 500 DEG C and is roasted
Burn 2min；
（7）Primary chemical conversion repair process：It is 90 DEG C that etched foil after high-temperature roasting is handled, which is placed in temperature, mass content
For the mixed solution of 5% boric acid and 0.5 ‰ ammonium pentaborates, apply 530V voltages, constant pressure handles 10min；
（8）Middle processing：Etched foil uses phosphoric acid solution pickling, phosphoric acid solution a concentration of after repair process will be once melted into
1.4mol/L, pickling temperature are 60 DEG C, pickling time 20min；
（9）Secondary chemical conversion repair process：It is 90 DEG C that etched foil after primary repair, which is placed in temperature, and mass content is 5% boric acid
With the mixed solution of 0.5 ‰ ammonium pentaborates, apply 530V voltages, constant pressure handles 10min；
（10）Secondary high-temperature calcination process：Etched foil after secondary chemical conversion treatment is placed in the high temperature furnace that temperature is 500 DEG C
Roast 2min；
（11）It is melted into repair process three times：It is 90 DEG C that etched foil after secondary high-temperature calcination process, which is placed in temperature, and quality contains
Amount is the mixed solution of 5% boric acid and 0.5 ‰ ammonium pentaborates, applies 530V voltages, and constant pressure handles 10min；
（12）Post-processing：Etched foil after three-level chemical conversion is repaired is placed on 80 DEG C, handles 8min in 0.4% sodium radio-phosphate,P-32 solution.
Embodiment 2
A kind of production method of no foil ash medium-high pressure chemical foil, step are：
（1）Pre-treatment：It is 96 DEG C that mesohigh etched foil, which is placed on temperature, and pure water of the resistance more than 1M Ω impregnates 12min；
（2）Level-one chemical conversion treatment：By the etched foil after pre-treatment be placed in temperature be 90 DEG C, mass content be 3% boric acid and
The mixed solution of 0.8 ‰ ammonium pentaborates, applies 150V voltages, and constant pressure handles 10min；
（3）Two level chemical conversion treatment：It is 90 DEG C that etched foil after level-one chemical conversion treatment, which is placed in temperature, and mass content is 3% boric acid
With the mixed solution of 0.5 ‰ ammonium pentaborates, apply 310V voltages, constant pressure handles 10min；
（4）Three-level chemical conversion treatment：It is 90 DEG C that etched foil after two level chemical conversion treatment, which is placed in temperature, and mass content is 5% boric acid
With the mixed solution of 0.5 ‰ ammonium pentaborates, apply 470V voltages, constant pressure handles 15min；
（5）Level Four chemical conversion treatment：It is 90 DEG C that etched foil after three-level chemical conversion treatment, which is placed in temperature, and mass content is 5% boric acid
With the mixed solution of 0.5 ‰ ammonium pentaborates, apply 530V voltages, constant pressure handles 25min；
（6）High-temperature roasting is handled：Etched foil after level Four chemical conversion treatment is placed in the high temperature furnace that temperature is 500 DEG C and is roasted
Burn 2min；
（7）Primary chemical conversion repair process：It is 90 DEG C that etched foil after high-temperature roasting is handled, which is placed in temperature, mass content
For the mixed solution of 5% boric acid and 0.5 ‰ ammonium pentaborates, apply 530V voltages, constant pressure handles 10min；
（8）Middle processing：Etched foil uses phosphoric acid solution pickling, phosphoric acid solution a concentration of after repair process will be once melted into
1.8mol/L, pickling temperature are 65 DEG C, pickling time 10min；
（9）Secondary chemical conversion repair process：It is 90 DEG C that etched foil after primary repair, which is placed in temperature, and mass content is 5% boric acid
With the mixed solution of 0.5 ‰ ammonium pentaborates, apply 530V voltages, constant pressure handles 10min；
（10）Secondary high-temperature calcination process：Etched foil after secondary chemical conversion treatment is placed in the high temperature furnace that temperature is 500 DEG C
Roast 2min；
（11）It is melted into repair process three times：It is 90 DEG C that etched foil after secondary high-temperature calcination process, which is placed in temperature, and quality contains
Amount is the mixed solution of 5% boric acid and 0.5 ‰ ammonium pentaborates, applies 530V voltages, and constant pressure handles 10min；
（12）Post-processing：Etched foil after three-level chemical conversion is repaired is placed on 80 DEG C, handles 8min in 0.4% sodium radio-phosphate,P-32 solution.
Embodiment 3
A kind of production method of no foil ash medium-high pressure chemical foil, step are：
（1）Pre-treatment：It is 96 DEG C that mesohigh etched foil, which is placed on temperature, and pure water of the resistance more than 1M Ω impregnates 12min；
（2）Level-one chemical conversion treatment：It is 90 DEG C that etched foil after pre-treatment, which is placed in temperature, and mass content is 3% boric acid and 1 ‰
The mixed solution of ammonium pentaborate, applies 150V voltages, and constant pressure handles 10min；
（3）Two level chemical conversion treatment：It is 90 DEG C that etched foil after level-one chemical conversion treatment, which is placed in temperature, and mass content is 3% boric acid
With the mixed solution of 0.5 ‰ ammonium pentaborates, apply 310V voltages, constant pressure handles 10min；
（4）Three-level chemical conversion treatment：It is 90 DEG C that etched foil after two level chemical conversion treatment, which is placed in temperature, and mass content is 5% boric acid
With the mixed solution of 0.5 ‰ ammonium pentaborates, apply 470V voltages, constant pressure handles 15min；
（5）Level Four chemical conversion treatment：It is 90 DEG C that etched foil after three-level chemical conversion treatment, which is placed in temperature, and mass content is 5% boric acid
With the mixed solution of 0.5 ‰ ammonium pentaborates, apply 530V voltages, constant pressure handles 25min；
（6）High-temperature roasting is handled：Etched foil after level Four chemical conversion treatment is placed in the high temperature furnace that temperature is 500 DEG C and is roasted
Burn 2min；
（7）Primary chemical conversion repair process：It is 90 DEG C that etched foil after high-temperature roasting is handled, which is placed in temperature, mass content
For the mixed solution of 5% boric acid and 0.5 ‰ ammonium pentaborates, apply 530V voltages, constant pressure handles 10min；
（8）Middle processing：Etched foil uses phosphoric acid solution pickling, phosphoric acid solution a concentration of after repair process will be once melted into
2.0mol/L, pickling temperature are 70 DEG C, pickling time 8min；
（9）Secondary chemical conversion repair process：It is 90 DEG C that etched foil after primary repair, which is placed in temperature, and mass content is 5% boric acid
With the mixed solution of 0.5 ‰ ammonium pentaborates, apply 530V voltages, constant pressure handles 10min；
（10）Secondary high-temperature calcination process：Etched foil after secondary chemical conversion treatment is placed in the high temperature furnace that temperature is 500 DEG C
Roast 2min；
（11）It is melted into repair process three times：It is 90 DEG C that etched foil after secondary high-temperature calcination process, which is placed in temperature, and quality contains
Amount is the mixed solution of 5% boric acid and 0.5 ‰ ammonium pentaborates, applies 530V voltages, and constant pressure handles 10min；
（12）Post-processing：Etched foil after three-level chemical conversion is repaired is placed on 80 DEG C, handles 8min in 0.4% sodium radio-phosphate,P-32 solution.
The testing result of comparative example 1, comparative example 2 and embodiment 1-3 is as shown in table 1：
Table 1
As can be seen from Table 1, handling the comparative example 1 of phosphoric acid acid pickling step in not using, Porosity anodic oxide film and aluminium powder are not dissolved also,
Foil ash is also coated over inside oxidation film, carries out foil ash detection, foil ash unobvious, but leakage current value height instead.Comparative example 2 is to add
Adding middle processing step, but not in the protection data of the present invention, Porosity anodic oxide film has only been dissolved a part with aluminium powder, into
Row foil ash detects, and foil ash is serious, and leakage current value is also very high.By the method for the present invention treated Waste Acid From Hua Cheng Foil, foil ash noresidue changes
It has been apt to dust Control and aluminium electrolutic capacitor punch-through that aluminium electrolutic capacitor manufacture cuts process, meanwhile, leakage current value phase
53.3% ~ 61.3% is had dropped for comparative example 1, improves the specific volume conversion ratio of Waste Acid From Hua Cheng Foil.
It is last it is to be noted that：The pre-treatment of the present invention, multistage chemical conversion treatment are repeatedly melted into repair process, are repeatedly high
Warm calcination process and post-processing are the conventional treatment means of this field, therefore not detailed in embodiment repeat and illustrate.With
Upper embodiment is merely illustrative of the technical solution of the present invention, rather than its limitations.Although with reference to the foregoing embodiments to the present invention into
Go detailed description, it will be understood by those of ordinary skill in the art that：It still can be to recorded in foregoing embodiments
Technical solution is modified or equivalent replacement of some of the technical features；And these modifications or replacements, do not make
The essence of corresponding technical solution is detached from the spirit and scope of various embodiments of the present invention technical solution.
Claims (10)
1. a kind of production method of no foil ash medium-high pressure chemical foil, it is characterised in that：Including mesohigh etched foil is successively carried out
Pre-treatment, high-temperature roasting processing, is once melted into repair process, secondary chemical conversion repair process, secondary height at multistage chemical conversion treatment
Warm calcination process is melted into repair process and post-processing three times, in the primary chemical conversion repair process and secondary chemical conversion repair process
Between, it is handled in addition, the middle processing, is that the etched foil after primary chemical conversion repair process is used into phosphoric acid solution pickling,
A concentration of 1.4 ~ the 2.0mol/L of phosphoric acid solution, pickling temperature are 60 ~ 80 DEG C, and pickling time is 8 ~ 20min.
2. a kind of production method of no foil ash medium-high pressure chemical foil according to claim 1, it is characterised in that：Place before described
Reason is that mesohigh etched foil is placed in the pure water that temperature is 92 DEG C or more to impregnate 3 ~ 20min.
3. a kind of production method of no foil ash medium-high pressure chemical foil according to claim 1, it is characterised in that：The multistage
Chemical conversion treatment, step include：
（1）Level-one chemical conversion treatment：The level-one that 85 ~ 90 DEG C of temperature is placed in by the etched foil after pre-treatment is melted into corrosive liquid
In, apply 50 ~ 200V voltages, constant pressure handles 5 ~ 10min；The level-one is melted into corrosive liquid, be boric acid that mass content is 3% and
The mixed solution of 0.5 ~ 1 ‰ trace mineral supplements；
（2）Two level chemical conversion treatment：The two level that 85 ~ 90 DEG C of temperature is placed in by the etched foil after level-one chemical conversion treatment is melted into rotten
It loses and applies 100 ~ 380V voltages in liquid, constant pressure handles 5 ~ 10min；The two level is melted into corrosive liquid, is the boron that mass content is 3%
The mixed solution of acid and 0.5 ~ 1 ‰ trace mineral supplements；
（3）Three-level chemical conversion treatment：The three-level that 85 ~ 90 DEG C of temperature is placed in by the etched foil after two level chemical conversion treatment is melted into rotten
It loses and applies 180 ~ 660V voltages in liquid, constant pressure handles 5 ~ 15min；The three-level is melted into corrosive liquid, is the boron that mass content is 5%
The mixed solution of acid and 0.5 ~ 1 ‰ trace mineral supplements；
（4）Level Four chemical conversion treatment：The level Four that etched foil after three-level chemical conversion treatment is placed in 85 ~ 90 DEG C of temperature is melted into corrosion
Apply 200 ~ 750V voltages in liquid, constant pressure handles 15 ~ 30min；The level Four is melted into corrosive liquid, is the boric acid that mass content is 5%
With the mixed solution of 0.5 ~ 1 ‰ trace mineral supplements.
4. a kind of production method of no foil ash medium-high pressure chemical foil according to claim 1, it is characterised in that：It is described primary
High-temperature roasting is handled, and is that the etched foil after level Four chemical conversion treatment is carried out high-temperature roasting at 450 ~ 550 DEG C, roasting time is
2~3min。
5. a kind of production method of no foil ash medium-high pressure chemical foil according to claim 1, it is characterised in that：It is described primary
Be melted into repair process, be by by a high-temperature roasting processing after etched foil be placed in 85 ~ 90 DEG C of temperature it is primary be melted into repair
Apply 200 ~ 750V voltages in multiple liquid, constant pressure handles 5 ~ 10min, and liquid is repaired in the primary chemical conversion, is the boron that mass content is 5%
The mixed solution of acid and 0.5 ~ 1 ‰ trace mineral supplements.
6. a kind of production method of no foil ash medium-high pressure chemical foil according to claim 1, it is characterised in that：It is described secondary
Be melted into repair process, be in passing through handle after etched foil be placed in 85 ~ 90 DEG C of temperature secondary chemical conversion repair liquid in apply
200 ~ 750V voltages, constant pressure handle 5 ~ 10min, and liquid is repaired in the secondary chemical conversion, be mass content for 5% boric acid and 0.5 ~
The mixed solution of 1 ‰ trace mineral supplements.
7. a kind of production method of no foil ash medium-high pressure chemical foil according to claim 1, it is characterised in that：It is described secondary
High-temperature roasting is handled, and is that the etched foil after secondary chemical conversion repair process is carried out high-temperature roasting at 450 ~ 550 DEG C, when roasting
Between be 2 ~ 3min.
8. a kind of production method of no foil ash medium-high pressure chemical foil according to claim 1, it is characterised in that：It is described three times
It is melted into repair process, is to repair the chemical conversion three times for being placed in 85 ~ 90 DEG C of temperature by the etched foil after secondary high-temperature calcination process
Apply 200 ~ 750V voltages in multiple liquid, constant pressure handles 5 ~ 10min, and liquid is repaired in the chemical conversion three times, is the boron that mass content is 5%
The mixed solution of acid and 0.5 ~ 1 ‰ trace mineral supplements.
9. a kind of production method of no foil ash medium-high pressure chemical foil according to claim 1, it is characterised in that：Place after described
Reason is that the etched foil of chemical conversion repair process three times is placed in 4 ~ 12min of processing in 70 ~ 80 DEG C of phosphoric acid,diluted or phosphate solution.
10. a kind of production method of no foil ash medium-high pressure chemical foil according to claim 3 or 5 or 6 or 8, feature exist
In：The trace mineral supplement combines for one or both of ammonium pentaborate and citric acid.
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| CN109797424A (en) * | 2018-12-28 | 2019-05-24 | 广西贺州市桂东电子科技有限责任公司 | A kind of method handled in mesohigh anode aluminium foil Pyatyi hair engaging aperture corrosion |
| CN110055571A (en) * | 2019-04-18 | 2019-07-26 | 宜都东阳光化成箔有限公司 | A kind of preprocessing solution and chemical synthesis technology improving aluminium electrolutic capacitor medium-high pressure chemical foil capacity |
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Application publication date: 20180807 |