CN110016702A - A kind of aluminium electrolutic capacitor super-pressure Waste Acid From Hua Cheng Foil chemical synthesis technology - Google Patents
A kind of aluminium electrolutic capacitor super-pressure Waste Acid From Hua Cheng Foil chemical synthesis technology Download PDFInfo
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- CN110016702A CN110016702A CN201910314067.5A CN201910314067A CN110016702A CN 110016702 A CN110016702 A CN 110016702A CN 201910314067 A CN201910314067 A CN 201910314067A CN 110016702 A CN110016702 A CN 110016702A
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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
- C25D11/08—Anodisation of aluminium or alloys based thereon characterised by the electrolytes used containing inorganic acids
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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
- C25D11/10—Anodisation of aluminium or alloys based thereon characterised by the electrolytes used containing organic acids
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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
Abstract
The present invention relates to a kind of aluminium electrolutic capacitor super-pressure Waste Acid From Hua Cheng Foil chemical synthesis technologies, by improving existing boric acid chemical synthesis technology, after high-purity aluminum foil after corrosion extended surface is carried out hydration reaction, in the mixed liquor that level-one second level electrolyte is boric acid, citric acid and ammonium pentaborate, three-level level Four electrolyte is boric acid, level Four chemical conversion is carried out in the mixed liquor of tetramethylammonium hydroxide and mannitol, and suitable phosphoric acid processing intensity is selected in post-processing, the voltage of Waste Acid From Hua Cheng Foil can be made to reach 1200 V, to further expand the application field of Waste Acid From Hua Cheng Foil.
Description
Technical field
The present invention relates to " aluminium electrolutic capacitors " to use anode aluminium foil field, specially a kind of aluminium electrolutic capacitor super-pressure
Waste Acid From Hua Cheng Foil chemical synthesis technology.
Background technique
Aluminium electrolutic capacitor is by carrying out to the high-purity aluminum foil after corrosion extended surface with anode aluminium foil (also referred to as Waste Acid From Hua Cheng Foil)
A series of chemical synthesis technologies such as electrochemical anodic oxidation manufacture.Waste Acid From Hua Cheng Foil of the proof voltage in 750V or more is referred to as super-pressure
At foil, important one of the developing direction in Waste Acid From Hua Cheng Foil field was had become in recent years.Produce the relatively conventional chemical conversion of super-pressure Waste Acid From Hua Cheng Foil
Process flow is: the high-purity aluminum foil after corrosion extended surface is placed in 90-100 DEG C of deionized water impregnates 10-20 minutes first, and
Aluminium foil is placed in afterwards in the aqueous solution of ammonium pentaborate of boric acid and 0.001-1% that concentration is 1-10%, in 80-95 DEG C of temperature,
With 20-100mA/ (cm)2Segmentation chemical conversion is carried out under conditions of electric current, is then depolarized in phosphate aqueous solution and burning piece furnace
Processing, and the paillon after depolarising processing is repaired and is melted into again, it finally takes out, aluminium foil handles 2-5 at 60-150 DEG C
Minute drying.
Super-pressure Waste Acid From Hua Cheng Foil in process of production, since the formation voltage of application is excessively high, it is existing easily to there is serious scintillation
As being mainly reflected in the arrival voltage of Waste Acid From Hua Cheng Foil once the generation of this phenomenon can adversely affect the quality of Waste Acid From Hua Cheng Foil product
It is relatively low, capacity is relatively low and performance is poor etc., eventually lead to the work electricity that its manufactured aluminium electrolytic capacitor product can bear
It forces down and the service life is bad, the field greatly limited their application.In addition with aerospace, frequency converter, the neck such as super large power supply
The fast development in domain, the requirement that can bear operating voltage to used ultra-high voltage aluminum electrolytic capacitor is higher and higher, urgently
Need the super-pressure Waste Acid From Hua Cheng Foil product of 1000V or more, and mesh this Waste Acid From Hua Cheng Foil product be very in the market it is rare, the main reason is that not having
There is the chemical synthesis technology of suitable production 1000V or more super-pressure Waste Acid From Hua Cheng Foil to ask to solve scintillation phenomenon occurred in formation process etc.
Topic.
Summary of the invention
In view of the deficiency of above-mentioned existing production technology, the purpose of the present invention is to provide a kind of aluminium electrolutic capacitor superelevation
Waste Acid From Hua Cheng Foil chemical synthesis technology is pressed, by improving existing pure boration architectonical, selects boric acid, tetramethylammonium hydroxide and mannitol
Combined electrolyte is melted into, and the scintillation phenomenon of formation process can be effectively alleviated, and improves the arrival voltage value 50- of Waste Acid From Hua Cheng Foil
100V, capacity boost, and can be reduced the consumption of electric energy in formation process, save the cost.
It is another object of the present invention to: a kind of aluminium electrolutic capacitor super-pressure Waste Acid From Hua Cheng Foil chemical synthesis technology is provided, can be incited somebody to action
The voltage class of super-pressure Waste Acid From Hua Cheng Foil is extended to 1200V.
The invention adopts the following technical scheme:
Dipping: it is soaked 10-20 minutes in 97 DEG C of pure water with the aluminium foil after electrolysis corrosion treatment；
Level-one chemical conversion: boric acid concentration 10-100g/L, citric acid concentration 0.1-10g/L, ammonium pentaborate concentration are 1-
20g/L, 80-95 DEG C of tank liquor temperature, formation voltage 200-400V, current density 20-100mA/cm2, it is melted into time 5-15 minutes；
Second level chemical conversion: boric acid concentration 10-100g/L, citric acid concentration 0.01-10g/L, ammonium pentaborate concentration are
0.1-10g/L, 80-95 DEG C of tank liquor temperature, formation voltage 400-750V, current density 20-100mA/cm2, it is melted into time 5-15
Minute；
Three-level chemical conversion: boric acid concentration 10-100g/L, tetramethylammonium hydroxide concentration are 0.02-1g/L, mannitol concentration
For 0.01-1g/L, 80-95 DEG C of tank liquor temperature, formation voltage 600-1100V, current density 20-100mA/cm2, it is melted into the time
10-20 minutes；
Level Four is melted into for the first time: boric acid concentration 10-100g/L, and tetramethylammonium hydroxide concentration is 0.01-0.5g/L, sweet
Dew determining alcohol be 0.01-1g/L, 80-95 DEG C of tank liquor temperature, formation voltage 700-1200V, current density 20-100mA/cm2, change
At time 10-30 minute；
First time high-temperature process: by level Four for the first time the aluminium foil that was melted into 400-580 DEG C processing 1-3 minutes；
Second of chemical conversion of level Four: the paillon that first time high-temperature process is crossed is 10-100g/L, tetramethyl hydrogen in boric acid concentration
Oxidation ammonium concentration be 0.01-0.5g/L, mannitol concentration 0.01-1g/L, 80-95 DEG C of tank liquor temperature, formation voltage 700-
1200V, current density 20-100mA/cm2, it is melted into time 5-15 minutes；
Phosphoric acid processing: the paillon that level Four was melted into for the second time 45-70 in the phosphate aqueous solution that concentration is 30-60ml/L
DEG C impregnate 3-12 minutes；
Level Four third time be melted into: by the processed paillon of phosphoric acid boric acid concentration be 10-100g/L, tetramethylammonium hydroxide
Concentration is 0.01-0.5g/L, mannitol concentration 0.01-1g/L, 80-95 DEG C of tank liquor temperature, formation voltage 700-1200V, electricity
Current density 20-100mA/cm2, it is melted into time 5-15 minutes；
Second of high-temperature process: by the level Four aluminium foil that was melted into of third time 400-580 DEG C processing 1-3 minutes；
Level Four the 4th time chemical conversion: the paillon that second of high-temperature process is crossed is 10-100g/L, tetramethyl hydrogen in boric acid concentration
Oxidation ammonium concentration be 0.01-0.5g/L, mannitol concentration 0.01-1g/L, 80-95 DEG C of tank liquor temperature, formation voltage 700-
1200V, current density 20-100mA/cm2, it is melted into time 5-15 minutes；
The paillon that level Four the 4th time is melted into is handled at 60-150 DEG C 2-5 minutes after pure water cleans finally and is dried.
The invention has the following advantages:
1, the present invention search out a kind of effective solution for alleviating the scintillation phenomenon in super-pressure Waste Acid From Hua Cheng Foil production process and
Technique.In three-level, level Four chemical synthesis technology step, since the formation voltage value of application is higher, it is easy to produce scintillation phenomenon, is passed through
Three-level, level Four electrolyte use boric acid, and the mixed liquor of tetramethylammonium hydroxide and mannitol utilizes tetramethylammonium hydroxide and sweet
Revealing alcohol has preferable hydrophily, can generate absorption with the aqua oxidation film of aluminium foil surface, can effectively reduce interface and its attached
Close negative ion concentration improves flash over voltage, effectively alleviates the scintillation phenomenon in super-pressure Waste Acid From Hua Cheng Foil production process.
2, the present invention searches out the solution and technique of a kind of raising super-pressure Waste Acid From Hua Cheng Foil arrival voltage value.In three-level, level Four
In chemical synthesis technology step, by boric acid, the combined electrolyte of tetramethylammonium hydroxide and mannitol is melted into, effective slow
The scintillation phenomenon in super-pressure Waste Acid From Hua Cheng Foil production process is solved, tetramethylammonium hydroxide can effectively improve the surface of its solution
Power guarantees that electrolyte preferably enters chemical conversion in the cavity of aluminium foil and forms more effective oxidation film, and in adjustable electrolyte
PH value tends to faintly acid can preferably protect established oxidation film to be not dissolved to neutrality, and select suitable phosphoric acid processing
Intensity compares with existing boric acid chemical synthesis technology and the arrival voltage value 50-100V of Waste Acid From Hua Cheng Foil can be improved.
3, level-one, second level tank liquor select the mixed liquor of boric acid, citric acid, ammonium pentaborate, and the addition of citric acid can dissolve knot
The not high oxidation film of brilliant degree, increases the degree of crystallinity of oxidation film, and in addition the introducing of citric acid leads to the molten of partial oxide film
Solution, can slow down the chocking-up degree of tiny tunnel micropore, be conducive to the performance of extended surface effect, promote the increase of capacitor.
4, it is handled after second of chemical conversion of level Four in phosphate aqueous solution depolarising, the intensity for depolarizing processing is inadequate, will lead to
Segmental defect, which cannot be exposed, to be repaired, and the decaying of voltage and capacity is caused, and depolarising processing excessively, will lead to oxidation film
Excessive dissolution, influence the arrival voltage and capacity of Waste Acid From Hua Cheng Foil.The concentration that phosphoric acid limits is very crucial, in the present invention after level Four chemical conversion
Paillon phosphate aqueous solution concentration be 50ml/L phosphate aqueous solution in 60 DEG C immersion 6-8 minutes, the arrival of Waste Acid From Hua Cheng Foil can be made
Voltage and capacity reach optimum value.
5, super-pressure chemical synthesis technology is mentioned in the present invention, due to the alleviation of scintillation phenomenon in production process, to can be improved
Added voltage, improves the arrival voltage of Waste Acid From Hua Cheng Foil, the voltage class of super-pressure Waste Acid From Hua Cheng Foil can be made to be extended in formation process
1200V。
6, super-pressure chemical synthesis technology is mentioned in the present invention, due to the alleviation of scintillation phenomenon in production process, chemical conversion can be reduced
The consumption of electric energy in the process, save the cost.
7, super-pressure chemical synthesis technology is mentioned in the present invention, due to the alleviation of scintillation phenomenon in production process, chemical conversion can be promoted
The capacity of foil.
Specific embodiment
Combined with specific embodiments below, further details of elaboration is made to the present invention, but embodiments of the present invention are not
It is confined to the range of embodiment expression.These embodiments are merely to illustrate the present invention, range and is not intended to limit the present invention.
Embodiment 1
Step 1: taking, by electrolytic etching, treated that 99.99% aluminium foil soaks 15 minutes in 97 DEG C of pure water；
Step 2: with boric acid concentration being 50g/L in level-one, citric acid concentration 5g/L, ammonium pentaborate concentration is 10g/L,
85 DEG C of tank liquor temperature, formation voltage 220V, current density 50mA/cm2, it is melted into the time 8 minutes；
Step 3: with boric acid concentration being 50g/L in second level, citric acid concentration 1g/L, ammonium pentaborate concentration is 6g/L, slot
85 DEG C of liquid temperature, formation voltage 450V, current density 35mA/cm2, it is melted into the time 8 minutes；
Step 4: with boric acid concentration being 50g/L in three-level, tetramethylammonium hydroxide concentration is 0.35g/L, mannitol concentration
For 1g/L, 85 DEG C of tank liquor temperature, formation voltage 670V, current density 35mA/cm2, it is melted into the time 15 minutes；
Step 5: with boric acid concentration being 80g/L in level Four first time chemical conversion, tetramethylammonium hydroxide concentration is 0.25g/L,
Mannitol concentration is 0.5g/L, 85 DEG C of tank liquor temperature, formation voltage 740V, current density 35mA/cm2, it is melted into the time 20 minutes；
Step 6: the aluminium foil that level Four was melted into for the first time is handled 2 minutes at 550 DEG C；
Step 7: with boric acid concentration being 80g/L in second of chemical conversion of level Four, tetramethylammonium hydroxide concentration is 0.25g/L,
Mannitol concentration is 0.5g/L, 85 DEG C of tank liquor temperature, formation voltage 740V, current density 30mA/cm2, it is melted into the time 8 minutes；
Step 8: the paillon that level Four was melted into for the second time impregnates 6 for 65 DEG C in the phosphate aqueous solution that concentration is 50ml/L
Minute；
Step 9: with boric acid concentration being 80g/L in the chemical conversion of level Four third time, tetramethylammonium hydroxide concentration is 0.25g/L,
Mannitol concentration is 0.5g/L, 85 DEG C of tank liquor temperature, formation voltage 740V, current density 30mA/cm2, it is melted into the time 8 minutes；
Step 10: the aluminium foil that level Four third time was melted into is handled 2 minutes at 550 DEG C；
Step 11: tetramethylammonium hydroxide concentration is in level Four the 4th time chemical conversion with being 80g/L with boric acid concentration
0.25g/L, mannitol concentration 0.5g/L, 85 DEG C of tank liquor temperature, formation voltage 740V, current density 30mA/cm2, when chemical conversion
Between 8 minutes；
It is dried step 12: the paillon that level Four the 4th time is melted into is handled at 100 DEG C 2 minutes after pure water cleans.
Embodiment 2
Embodiment 2 is removed step 8: the paillon that level Four was melted into for the second time is in the phosphate aqueous solution that concentration is 50ml/L
60 DEG C are impregnated 6 minutes；Difference, remaining step are same as Example 1 with embodiment 1.
Comparative example 1
Comparative example 1 selects the chemical synthesis technology system of pure boric acid, except following steps and embodiment 1 have difference:
Step 2: with boric acid concentration be 50g/L in level-one, ammonium pentaborate concentration is 10g/L, 85 DEG C of tank liquor temperature, chemical conversion
Voltage 220V, current density 50mA/cm2, it is melted into the time 8 minutes；
Step 3: with boric acid concentration be 50g/L in second level, ammonium pentaborate concentration is 6g/L, 85 DEG C of tank liquor temperature, chemical conversion electricity
Press 450V, current density 35mA/cm2, it is melted into the time 8 minutes；
Step 4: with boric acid concentration be 50g/L in three-level, ammonium pentaborate concentration is 0.6g/L, 85 DEG C of tank liquor temperature, chemical conversion
Voltage 670V, current density 35mA/cm2, it is melted into the time 15 minutes；
Step 5: with boric acid concentration being 80g/L in level Four first time chemical conversion, ammonium pentaborate concentration is 0.4g/L, liquid temperature
85 DEG C, formation voltage 740V, current density 35mA/cm2, it is melted into the time 20 minutes；
Step 7: with boric acid concentration being 80g/L in second of chemical conversion of level Four, ammonium pentaborate concentration is 0.4g/L, tank liquor temperature
85 DEG C of degree, formation voltage 740V, current density 30mA/cm2, it is melted into the time 8 minutes；
Step 9: ammonium pentaborate concentration is 0.4g/L, tank liquor in the chemical conversion of level Four third time with being 80g/L with boric acid concentration
85 DEG C of temperature, formation voltage 740V, current density 30mA/cm2, it is melted into the time 8 minutes；
Step 11: ammonium pentaborate concentration is 0.4g/L in level Four the 4th time chemical conversion with being 80g/L with boric acid concentration,
85 DEG C of tank liquor temperature, formation voltage 740V, current density 30mA/cm2, it is melted into the time 8 minutes；
Anode foils parameter made from 1 embodiment of the present invention of table and comparative example compares
As seen from Table 1, in embodiment 1-2 formation process without scintillation, reach voltage, the static capacity under 768V, with than
Compared with example 1 compared to height is intended to, the power consumption under 768V is also reduced.It is high to reach voltage compared with comparative example 1 for especially embodiment 2
64V out, and capacity highest, power consumption are minimum.Illustrate that anode foils prepared by the present invention can be improved arriving for super-pressure Waste Acid From Hua Cheng Foil
Up to voltage and capacity, and electric energy can be saved.Excessively, oxidation film dissolution is excessive for 1 phosphoric acid of embodiment depolarising processing, leads to its arrival
Voltage and capacity are lower than embodiment 2.
Embodiment 3
Step 1: taking, by electrolytic etching, treated that 99.99% aluminium foil soaks 16 minutes in 97 DEG C of pure water；
Step 2: with boric acid concentration being 50g/L in level-one, citric acid concentration 2g/L, ammonium pentaborate concentration is 10g/L,
85 DEG C of tank liquor temperature, formation voltage 260V, current density 50mA/cm2, it is melted into the time 8 minutes；
Step 3: with boric acid concentration being 50g/L in second level, citric acid concentration 0.5g/L, ammonium pentaborate concentration is 1g/L,
85 DEG C of tank liquor temperature, formation voltage 530V, current density 35mA/cm2, it is melted into the time 8 minutes；
Step 4: with boric acid concentration being 50g/L in three-level, tetramethylammonium hydroxide concentration is 0.25g/L, mannitol concentration
For 0.5g/L, 85 DEG C of tank liquor temperature, formation voltage 770V, current density 35mA/cm2, it is melted into the time 20 minutes；
Step 5: with boric acid concentration being 80g/L in level Four first time chemical conversion, tetramethylammonium hydroxide concentration is 0.15g/L,
Mannitol concentration is 0.2g/L, 85 DEG C of liquid temperature, formation voltage 850V, current density 35mA/cm2, it is melted into the time 30 minutes；
Step 6: the aluminium foil that level Four was melted into for the first time is handled 2 minutes at 550 DEG C；
Step 7: with boric acid concentration being 80g/L in second of chemical conversion of level Four, tetramethylammonium hydroxide concentration is 0.15g/L,
Mannitol concentration is 0.2g/L, 85 DEG C of tank liquor temperature, formation voltage 850V, current density 30mA/cm2, it is melted into the time 8 minutes；
Step 8: the paillon that level Four was melted into for the second time impregnates 7 for 65 DEG C in the phosphate aqueous solution that concentration is 50ml/L
Minute；
Step 9: with boric acid concentration being 80g/L in the chemical conversion of level Four third time, tetramethylammonium hydroxide concentration is 0.15g/L,
Mannitol concentration is 0.2g/L, 85 DEG C of tank liquor temperature, formation voltage 850V, current density 30mA/cm2, it is melted into the time 8 minutes；
Step 10: the aluminium foil that level Four third time was melted into is handled 2 minutes at 550 DEG C；
Step 11: tetramethylammonium hydroxide concentration is in level Four the 4th time chemical conversion with being 80g/L with boric acid concentration
0.15g/L, mannitol concentration 0.2g/L, 85 DEG C of tank liquor temperature, formation voltage 850V, current density 30mA/cm2, when chemical conversion
Between 8 minutes；
It is dried step 12: the paillon that level Four the 4th time is melted into is handled at 100 DEG C 2 minutes after pure water cleans.
Embodiment 4
Embodiment 4 is removed step 8: the paillon that level Four was melted into for the second time is in the phosphate aqueous solution that concentration is 50ml/L
60 DEG C are impregnated 7 minutes；Difference, remaining step are same as Example 3 with embodiment 1.
Comparative example 2
Comparative example 1 selects the chemical synthesis technology system of pure boric acid, except following steps and embodiment 3 have difference:
Step 2: with boric acid concentration be 50g/L in level-one, ammonium pentaborate concentration is 10g/L, 85 DEG C of tank liquor temperature, chemical conversion
Voltage 260V, current density 50mA/cm2, it is melted into the time 8 minutes；
Step 3: with boric acid concentration be 50g/L in second level, ammonium pentaborate concentration is 2.5g/L, 85 DEG C of tank liquor temperature, chemical conversion
Voltage 530V, current density 35mA/cm2, it is melted into the time 8 minutes；
Step 4: with boric acid concentration be 50g/L in three-level, ammonium pentaborate concentration is 0.5g/L, 85 DEG C of tank liquor temperature, chemical conversion
Voltage 770V, current density 35mA/cm2, it is melted into the time 15 minutes；
Step 5: with boric acid concentration being 80g/L in level Four first time chemical conversion, ammonium pentaborate concentration is 0.35g/L, liquid temperature
85 DEG C, formation voltage 850V, current density 35mA/cm2, it is melted into the time 20 minutes；
Step 7: with boric acid concentration being 80g/L in second of chemical conversion of level Four, ammonium pentaborate concentration is 0.35g/L, tank liquor temperature
85 DEG C of degree, formation voltage 850V, current density 30mA/cm2, it is melted into the time 8 minutes；
Step 9: ammonium pentaborate concentration is 0.35g/L, tank liquor in the chemical conversion of level Four third time with being 80g/L with boric acid concentration
85 DEG C of temperature, formation voltage 850V, current density 30mA/cm2, it is melted into the time 8 minutes；
Step 11: ammonium pentaborate concentration is 0.35/L in level Four the 4th time chemical conversion with being 80g/L with boric acid concentration,
85 DEG C of tank liquor temperature, formation voltage 850V, current density 30mA/cm2, it is melted into the time 8 minutes；
Anode foils parameter made from 2 embodiment of the present invention of table and comparative example compares
As seen from Table 2, in embodiment 3-4 formation process without scintillation, reach voltage, the static capacity under 880V, with than
Compared with example 2 compared to height is intended to, the power consumption under 880V is also reduced.Especially embodiment 4 is selected, and voltage is reached compared with comparative example 2
It is higher by 80V, and capacity highest, power consumption are minimum.Illustrate that anode foils prepared by the present invention can be improved super-pressure Waste Acid From Hua Cheng Foil
Voltage and capacity are reached, and electric energy can be saved.Excessively, oxidation film dissolution is excessive for 3 phosphoric acid of embodiment depolarising processing, it is caused to arrive
It is lower than embodiment 4 up to voltage and capacity.
Embodiment 5
Step 1: taking, by electrolytic etching, treated that 99.99% aluminium foil soaks 15 minutes in 97 DEG C of pure water；
Step 2: with boric acid concentration being 50g/L in level-one, citric acid concentration 0.6g/L, ammonium pentaborate concentration is 8g/L,
85 DEG C of tank liquor temperature, formation voltage 330V, current density 50mA/cm2, it is melted into the time 10 minutes；
Step 3: with boric acid concentration being 50g/L in second level, citric acid concentration 0.1g/L, ammonium pentaborate concentration is 0.6g/
L, 85 DEG C of tank liquor temperature, formation voltage 650V, current density 35mA/cm2, it is melted into the time 10 minutes；
Step 4: with boric acid concentration being 50g/L in three-level, tetramethylammonium hydroxide concentration is 0.2g/L, mannitol concentration
It is 85 DEG C of 0.1g/L tank liquor temperature, formation voltage 990V, current density 35mA/cm2, it is melted into the time 20 minutes；
Step 5: with boric acid concentration being 80g/L in level Four first time chemical conversion, tetramethylammonium hydroxide concentration is 0.1g/L,
Mannitol concentration is 0.1g/L, 85 DEG C of tank liquor temperature, formation voltage 1150V, current density 35mA/cm2, chemical conversion the time 30 divide
Clock；
Step 6: the aluminium foil that level Four was melted into for the first time is handled 2.5 minutes at 550 DEG C；
Step 7: with boric acid concentration being 80g/L in second of chemical conversion of level Four, tetramethylammonium hydroxide concentration is 0.1g/L,
Mannitol concentration is 0.1g/L, 85 DEG C of tank liquor temperature, formation voltage 1150V, current density 30mA/cm2, chemical conversion the time 10 divide
Clock；
Step 8: the paillon that level Four was melted into for the second time impregnates 8 for 60 DEG C in the phosphate aqueous solution that concentration is 50ml/L
Minute；
Step 9: with boric acid concentration being 80g/L in the chemical conversion of level Four third time, tetramethylammonium hydroxide concentration is 0.1g/L,
Mannitol concentration is 0.1g/L, 85 DEG C of tank liquor temperature, formation voltage 1150V, current density 30mA/cm2, chemical conversion the time 10 divide
Clock；
Step 10: the aluminium foil that level Four third time was melted into is handled 2.5 minutes at 550 DEG C；
Step 11: with boric acid concentration being 80g/L in the 4th chemical conversion of level Four, tetramethylammonium hydroxide concentration is 0.1g/
L, mannitol concentration 0.1g/L, 85 DEG C of tank liquor temperature, formation voltage 1150V, current density 30mA/cm2, chemical conversion the time 10 divide
Clock；
It is dried step 12: the paillon that level Four the 4th time is melted into is handled at 100 DEG C 2 minutes after pure water cleans.
Embodiment 6
Embodiment 6 is removed step 8: the paillon that level Four was melted into for the second time is in the phosphate aqueous solution that concentration is 50ml/L
60 DEG C are impregnated 8 minutes；Difference, remaining step are same as Example 5 with embodiment 5.
Comparative example 3
Comparative example 3 selects the chemical synthesis technology system of pure boric acid, except following steps and embodiment 5 have difference:
Step 2: with boric acid concentration be 50g/L in level-one, ammonium pentaborate concentration is 10g/L, 85 DEG C of tank liquor temperature, chemical conversion
Voltage 330V, current density 50mA/cm2, it is melted into the time 8 minutes；
Step 3: with boric acid concentration be 50g/L in second level, ammonium pentaborate concentration is 1g/L, 85 DEG C of tank liquor temperature, chemical conversion electricity
Press 650V, current density 35mA/cm2, it is melted into the time 8 minutes；
Step 4: with boric acid concentration be 50g/L in three-level, ammonium pentaborate concentration is 0.2g/L, 85 DEG C of tank liquor temperature, chemical conversion
Voltage 990V, current density 35mA/cm2, it is melted into the time 20 minutes；
Step 5: with boric acid concentration being 80g/L in level Four first time chemical conversion, ammonium pentaborate concentration is 0.15g/L, liquid temperature
85 DEG C, formation voltage 1150V, current density 35mA/cm2, it is melted into the time 30 minutes；
Step 7: with boric acid concentration being 80g/L in second of chemical conversion of level Four, ammonium pentaborate concentration is 0.1g/L, tank liquor temperature
85 DEG C of degree, formation voltage 1150V, current density 30mA/cm2, it is melted into the time 8 minutes；
Step 9: ammonium pentaborate concentration is 0.1g/L, tank liquor in the chemical conversion of level Four third time with being 80g/L with boric acid concentration
85 DEG C of temperature, formation voltage 1150V, current density 30mA/cm2, it is melted into the time 8 minutes；
Step 11: ammonium pentaborate concentration is 0.1g/L in level Four the 4th time chemical conversion with being 80g/L with boric acid concentration,
85 DEG C of tank liquor temperature, formation voltage 1150V, current density 30mA/cm2, it is melted into the time 8 minutes；
Anode foils made from 3 embodiment of the present invention of table and comparative example reach voltage and compare
As seen from Table 3, in embodiment 5-6 formation process without scintillation, reach voltage, the static capacity under 1135V, with than
Compared with example 3 compared to height is intended to, the power consumption under 1135V is also reduced.It is high to reach voltage compared with comparative example 3 for especially embodiment 6
95V out, and capacity highest, power consumption are minimum.Illustrate that anode foils prepared by the present invention can be improved arriving for super-pressure Waste Acid From Hua Cheng Foil
Up to voltage, and Waste Acid From Hua Cheng Foil voltage can be made to be higher than 1200V or more.Excessively, oxidation film dissolved for 5 phosphoric acid of embodiment depolarising processing
It is more, cause its arrival voltage and capacity lower than embodiment 6.
Comparative example 4
Comparative example 4 and the differentiated step of embodiment 6:
Step 2: with boric acid concentration be 50g/L in level-one, ammonium pentaborate concentration is 8g/L, 85 DEG C of tank liquor temperature, chemical conversion electricity
Press 330V, current density 50mA/cm2, it is melted into the time 10 minutes；
Step 3: with boric acid concentration be 50g/L in second level, ammonium pentaborate concentration is 0.6g/L, 85 DEG C of tank liquor temperature, chemical conversion
Voltage 650V, current density 35mA/cm2, it is melted into the time 10 minutes；
Comparative example 5
Comparative example 5 and the differentiated step of embodiment 6:
Step 4: with boric acid concentration being 50g/L in three-level, tetramethylammonium hydroxide concentration is 0.2g/L, tank liquor temperature 85
DEG C, formation voltage 990V, current density 35mA/cm2, it is melted into the time 20 minutes；
Step 5: with boric acid concentration being 80g/L in level Four first time chemical conversion, tetramethylammonium hydroxide concentration is 0.1g/L,
85 DEG C of tank liquor temperature, formation voltage 1150V, current density 35mA/cm2, it is melted into the time 30 minutes；
Step 7: with boric acid concentration being 80g/L in second of chemical conversion of level Four, tetramethylammonium hydroxide concentration is 0.1g/L,
85 DEG C of tank liquor temperature, formation voltage 1150V, current density 30mA/cm2, it is melted into the time 10 minutes；
Step 9: with boric acid concentration being 80g/L in the chemical conversion of level Four third time, tetramethylammonium hydroxide concentration is 0.1g/L,
85 DEG C of tank liquor temperature, formation voltage 1150V, current density 30mA/cm2, it is melted into the time 10 minutes；
Step 11: with boric acid concentration being 80g/L in the 4th chemical conversion of level Four, tetramethylammonium hydroxide concentration is 0.1g/
L, 85 DEG C of tank liquor temperature, formation voltage 1150V, current density 30mA/cm2, it is melted into the time 10 minutes；
Comparative example 6
Comparative example 6 and the differentiated step of embodiment 6:
Step 4: with boric acid concentration being 50g/L in three-level, mannitol concentration is 85 DEG C of 0.1g/L tank liquor temperature, chemical conversion electricity
Press 990V, current density 35mA/cm2, it is melted into the time 20 minutes；
Step 5: with boric acid concentration being 80g/L, mannitol concentration 0.1g/L, tank liquor temperature in level Four first time chemical conversion
85 DEG C, formation voltage 1150V, current density 35mA/cm2, it is melted into the time 30 minutes；
Step 7: with boric acid concentration being 80g/L, mannitol concentration 0.1g/L, tank liquor temperature in second of chemical conversion of level Four
85 DEG C, formation voltage 1150V, current density 30mA/cm2, it is melted into the time 10 minutes；
Step 9: with boric acid concentration being 80g/L, mannitol concentration 0.1g/L, tank liquor temperature in the chemical conversion of level Four third time
85 DEG C, formation voltage 1150V, current density 30mA/cm2, it is melted into the time 10 minutes；
Step 11: with boric acid concentration being 80g/L, mannitol concentration 0.1g/L, tank liquor temperature in the 4th chemical conversion of level Four
85 DEG C of degree, formation voltage 1150V, current density 30mA/cm2, it is melted into the time 10 minutes.
Anode foils made from 4 embodiment of the present invention 6 of table and comparative example 4-6 reach voltage and compare
As seen from Table 4, comparative example 4 and embodiment 6 compare, and capacity low 2.9% illustrates to add in level-one second level electrolyte
Citric acid can promote its capacity；Comparative example five, three-level and level Four electrolyte select the mixed liquor of boric acid and tetramethylammonium hydroxide,
Boric acid is selected relative to six three-level of embodiment and level Four electrolyte, the mixed liquor of tetramethylammonium hydroxide and mannitol reaches electricity
Pressure wants low 25V, illustrates that mannitol is wherein playing the role of promoting voltage；Comparative example six, three-level and level Four electrolyte are selected
The mixed liquor of boric acid and mannitol causes solution conductivity in formation process relatively low, causes since mannitol does not provide conductance substantially
It reaches voltage and capacity is also lower than comparative example three, illustrate that the mixed liquor of boric acid and mannitol does not have the effect for promoting voltage.
Claims (9)
1. a kind of aluminium electrolutic capacitor electrolyte of super-pressure Waste Acid From Hua Cheng Foil, the electrolyte includes level-one electrolyte, second level electricity
Solve liquid, three-level electrolyte and level Four electrolyte, it is characterised in that: three-level electrolyte and level Four electrolyte include boric acid, tetramethyl
Ammonium hydroxide: boric acid concentration 10-100g/L, tetramethylammonium hydroxide concentration are 0.02-1g/L；Level Four electrolyte: boric acid is dense
Degree is 10-100g/L, and tetramethylammonium hydroxide concentration is 0.01-0.5g/L.
2. the aluminium electrolutic capacitor according to claim 1 electrolyte of super-pressure Waste Acid From Hua Cheng Foil, it is characterised in that: described three
Grade electrolyte and level Four electrolyte further include mannitol, and mannitol concentration is 0.01-1g/L in three-level electrolyte；Level Four electrolysis
Mannitol concentration is 0.01-1g/L in liquid.
3. the aluminium electrolutic capacitor according to claim 1 electrolyte of super-pressure Waste Acid From Hua Cheng Foil, it is characterised in that: described one
Grade electrolyte and second level electrolyte include boric acid, ammonium pentaborate, and boric acid concentration 10-100g/L, ammonium pentaborate concentration is 1-
20g/L。
4. the aluminium electrolutic capacitor according to claim 3 electrolyte of super-pressure Waste Acid From Hua Cheng Foil, it is characterised in that: described one
It further include citric acid, citric acid concentration 0.1-10g/L in grade electrolyte and second level electrolyte.
5. the chemical conversion that electrolyte according to any one of claims 1-4 is used for aluminium electrolutic capacitor super-pressure Waste Acid From Hua Cheng Foil
Technique, it is characterised in that: the technique is high-purity aluminum foil after corroding extended surface after hydration reaction, is carried out in the electrolytic solution
Level Four chemical conversion, the hydration reaction condition be that the high-purity aluminum foil after corrosion extended surface is placed in 90-100 DEG C of deionized water and impregnates
10-20 minutes.
6. aluminium electrolutic capacitor according to claim 1 super-pressure Waste Acid From Hua Cheng Foil chemical synthesis technology, which is characterized in that level Four
At including four chemical conversions, wherein depolarising is handled in phosphate aqueous solution after second of chemical conversion of level Four, after level Four third time is melted into
It burns and carries out the 4th chemical conversion after carrying out depolarising processing in piece furnace again, finally take out, aluminium foil is handled 2-5 minutes at 60-150 DEG C
Drying.
7. aluminium electrolutic capacitor according to claim 6 super-pressure Waste Acid From Hua Cheng Foil chemical synthesis technology, which is characterized in that level Four
Paillon after secondary chemical conversion 45-70 DEG C immersion 3-12 minutes in the phosphate aqueous solution that phosphate aqueous solution concentration is 30-60ml/L
Carry out depolarising processing.
8. aluminium electrolutic capacitor according to claim 7 super-pressure Waste Acid From Hua Cheng Foil chemical synthesis technology, the paillon after level Four chemical conversion
60 DEG C immersion 6-8 minutes in the phosphate aqueous solution that phosphate aqueous solution concentration is 50ml/L.
9. according to the super-pressure Waste Acid From Hua Cheng Foil chemical synthesis technology of aluminium electrolutic capacitor described in claim 6-8 any one, feature
Be, the technique specifically includes the following steps:
First step dipping: the deionization with the aluminium foil after electrolysis corrosion treatment at 90-100 DEG C impregnates 10-20 minutes；
The chemical conversion of second step level-one: boric acid concentration 10-100g/L, citric acid concentration 0.1-10g/L, ammonium pentaborate concentration are 1-
20g/L, 80-95 DEG C of tank liquor temperature, formation voltage 200-400V, current density 20-100mA/cm2, it is melted into time 5-15 minutes；
The chemical conversion of third step second level: boric acid concentration 10-100g/L, citric acid concentration 0.01-10g/L, ammonium pentaborate concentration are
0.1-10g/L, 80-95 DEG C of tank liquor temperature, formation voltage 400-750V, current density 20-100mA/cm2, it is melted into time 5-15
Minute；
The chemical conversion of 4th step three-level: boric acid concentration 10-100g/L, tetramethylammonium hydroxide concentration are 0.02-1g/L, and sweet dew is pure and strong
Degree is 0.01 80-95 DEG C of -1g/L tank liquor temperature, formation voltage 600-1100V, current density 20-100mA/cm2, it is melted into the time
10-20 minutes；
5th step level Four is melted into for the first time: boric acid concentration 10-100g/L, and tetramethylammonium hydroxide concentration is 0.01-0.5g/L,
Mannitol concentration is 0.01-1g/L, 80-95 DEG C of tank liquor temperature, formation voltage 700-1200V, current density 20-100mA/cm2,
Chemical conversion time 10-30 minutes；
6th step first time high-temperature process: by level Four for the first time the aluminium foil that was melted into 400-580 DEG C processing 1-3 minutes；
7th step level Four, second of chemical conversion: the paillon that first time high-temperature process is crossed is 10-100g/L, tetramethyl in boric acid concentration
Ammonium hydroxide concentration is 0.01-0.5g/L, mannitol concentration 0.01-1g/L, 80-95 DEG C of tank liquor temperature, formation voltage 700-
1200V, current density 20-100mA/cm2, it is melted into time 5-15 minutes；
8th step phosphoric acid processing: the paillon that level Four was melted into for the second time 45- in the phosphate aqueous solution that concentration is 30-60ml/L
70 DEG C immersion 3-12 minutes；
9th level Four third time be melted into: by the processed paillon of phosphoric acid boric acid concentration be 10-100g/L, tetramethylammonium hydroxide
Concentration is 0.01-0.5g/L, mannitol concentration 0.01-1g/L, 80-95 DEG C of tank liquor temperature, formation voltage 700-1200V, electricity
Current density 20-100mA/cm2, it is melted into time 5-15 minutes；
Tenth second of high-temperature process of step: by the level Four aluminium foil that was melted into of third time 400-580 DEG C processing 1-3 minutes；
The chemical conversion of 11st step level Four the 4th time: the paillon that second of high-temperature process is crossed is 10-100g/L, tetramethyl in boric acid concentration
Base ammonium hydroxide concentration be 0.01-0.5g/L, mannitol concentration 0.01-1g/L, 80-95 DEG C of tank liquor temperature, formation voltage
700-1200V, current density 20-100mA/cm2, it is melted into time 5-15 minutes:
The paillon that level Four the 4th time is melted into is handled at 60-150 DEG C 2-5 minutes after pure water cleans and is dried by the 12nd step.
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| CN113026073A (en) * | 2021-01-05 | 2021-06-25 | 南通海星电子股份有限公司 | Formation method of extra-high voltage electrode foil |
| CN114703526A (en) * | 2022-06-07 | 2022-07-05 | 南通海星电子股份有限公司 | Preparation method of high specific volume low-voltage electrode foil for automotive electronics |
| CN114999827A (en) * | 2022-07-19 | 2022-09-02 | 内蒙古丰川电子科技有限公司 | High-voltage formed foil for capacitor and preparation method thereof |
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