CN109859949A - A method of reducing medium-high pressure chemical foil leakage current - Google Patents
A method of reducing medium-high pressure chemical foil leakage current Download PDFInfo
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- CN109859949A CN109859949A CN201810077946.6A CN201810077946A CN109859949A CN 109859949 A CN109859949 A CN 109859949A CN 201810077946 A CN201810077946 A CN 201810077946A CN 109859949 A CN109859949 A CN 109859949A
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Abstract
The present invention provides a kind of method for reducing medium-high pressure chemical foil leakage current, include: by etched foil or lamination foil successively carry out pre-treatment, level Four chemical conversion, heat treatment for the first time, for the first time dipping, for the first time mend formation processing, second dipping, mend formation processing for second, second of heat treatment, third time mends formation processing, third time impregnates and post-processing, obtain Waste Acid From Hua Cheng Foil.The pre-treatment includes hydration-treated and solution impregnation.The present invention is by by the etched foil or lamination foil after hydration-treated, it immerses and carries out solution impregnation in organic acid soln or alkalescent inorganic salt solution, go the outermost loose porous aqua oxidation nitride layer of oxide film dissolving, and improve the property of aqua oxidation film, so that reducing leakage current increases electrolytic capacitor service life.
Description
Technical field
The present invention relates to capacitor electric pole foil manufacturing technology fields, specifically, the present invention relates to a kind of reduction mesohighs
The method of Waste Acid From Hua Cheng Foil leakage current.
Technical background
Three big base components one of of the electrolytic capacitor as electronics industry are big, small in size with capacitance per unit volume amount, again
It measures light, inexpensive and famous, is mainly used for tuning, filtering, bypass, coupling, energy storage and conversion etc..
Electrode foil is the component part of most critical in aluminium electrolutic capacitor, is melted into obtain by etched foil or lamination foil,
It influences capacity, volume, electric leakage, loss, resistance to ripple size, equivalent impedance, pressure resistance, the temperature characterisitic etc. of capacitor.In order to mention
The service life of high aluminium electrolutic capacitor, it is desirable to which its leakage current is small as far as possible, but chemical synthesis technology generally used now obtains
Waste Acid From Hua Cheng Foil leakage current is generally all larger.Because the oxidation film of the Waste Acid From Hua Cheng Foil of prior art manufacture causes to be melted into there are various defects
Foil leakage current is larger, and electrolytic capacitor service life is shorter.The oxidation film has the following deficiencies: 1) impurity defect, such as Fe,
Cu, Si, Cl-Big leakage current can be generated Deng, these impurity, while forming micro cell with aluminum substrate, makes aluminium foil in Working electrolyte
It is middle to corrode, so that oxidation film be made to deteriorate；2) the outermost loose porous aqua oxidation nitride layer of oxidation film；3) it is cracked,
Volume contraction when unformed oxidation film is changed into crystal form oxidation film causes to be cracked.
Therefore, it is necessary to develop a kind of chemical synthesizing method that can overcome drawbacks described above.
Summary of the invention
For the etched foil and lamination foil that mesohigh condition uses in the prior art, in chemical conversion, existing leakage current is larger
The problems such as, the present invention provides a kind of method for reducing medium-high pressure chemical foil leakage current, by the etched foil after hydration-treated
Or lamination foil carries out solution impregnation, goes the outermost loose porous aqua oxidation nitride layer of oxide film dissolving, and improve oxidation film
Property increase the service life of electrolytic capacitor to reduce leakage current.
Specifically, the present invention adopts the following technical scheme that:
The present invention provides a kind of method for reducing medium-high pressure chemical foil leakage current, comprising the following steps:
1) pre-treatment: etched foil or lamination foil are successively subjected to hydration-treated and solution impregnates；
2) level Four is melted into: the foil after pre-treatment is placed in progress level Four chemical conversion in forming liquid；
3) be heat-treated for the first time: the foil after level Four is melted into carries out first time heat treatment；
4) impregnate for the first time: the foil after first time is heat-treated is placed in progress first time dipping in acid solution；
5) mend formation processing for the first time: the foil after first time is impregnated, which is placed in forming liquid, mend at formation for the first time
Reason；
6) second impregnates: will mend the foil that forms that treated for the first time and be placed in acid solution and carry out second and impregnate；
7) second of benefit formation processing: the foil after second is impregnated, which is placed in forming liquid, mend at formation for the second time
Reason；
8) it second is heat-treated: the foil that forms that treated will be mended for second carries out second and be heat-treated；
9) third time is mended formation and handled: the foil after second is heat-treated, which is placed in forming liquid, to carry out at third time benefit formation
Reason；
10) third time impregnates: third time being mended and forms that treated foil is placed in progress third time dipping in phosphate solution；
11) post-process: the foil after third time is impregnated is washed, is dried, and Waste Acid From Hua Cheng Foil is obtained.
Further, the solution dipping in pre-treatment described in step 1) is that organic acid soln or alkalescent are inorganic with solution
Salting liquid.
Further, the concentration of the organic acid soln is 0.6-2.0wt%；The concentration of the alkalescent inorganic salt solution
For 0.1-2.0wt%.
Further, the organic acid in the organic acid soln is selected from fumaric acid, adipic acid, citric acid, tartaric acid, bigcatkin willow
Acid, one of benzoic acid or at least two combination；Inorganic salts in the alkalescent inorganic salt solution are selected from phosphate, boron
One of hydrochlorate, carbonate, silicate or at least two combination.
Further, the temperature of the solution dipping in pre-treatment described in step 1) is 50-90 DEG C, the time of solution dipping
It is 1-30 minutes.
Further, the forming liquid of level Four chemical conversion described in step 2) is to contain 2-10wt% boric acid and 0.01-1wt% boron
The aqueous solution of sour ammonium；The level Four chemical conversion temperature is 75-90 DEG C, and the level Four chemical conversion time is to reach the constant 5-20 of ceiling voltage
Minute；In the level Four chemical conversion highest formation voltage of chemical conversion at different levels be followed successively by final voltage 30 ± 2%, 60 ± 2%, 90 ±
2%, 100%, current density 10-60mA/cm2。
Further, the temperature being heat-treated for the first time described in step 3) is 450-550 DEG C, and the time is 1-4 minutes；Step
8) temperature of second of heat treatment described in is 550-580 DEG C, and the time is 0.5-2 minutes.
Further, dipping with acid solution is that the ortho phosphorous acid that concentration is 0.2-1wt% is molten for the first time described in step 4)
Liquid, dipping temperature are 50-80 DEG C, and dip time is 3-12 minutes；Second of dipping described in step 6) is concentration with acid solution
For the phosphoric acid solution of 4-15wt%, dipping temperature is 50-75 DEG C, and dip time is 3-12 minutes；Third time described in step 10)
The dipping ammonium dihydrogen phosphate that phosphate solution is that concentration is 1-8wt%, dipping temperature are 40-75 DEG C, and dip time is
1-5 minutes.
Further, it is to contain 2-10wt% that benefit described in step 5), step 7) and step 9), which forms processing forming liquid,
The aqueous solution of boric acid and 0.01-1wt% ammonium borate, mending formation temperature is 75-90 DEG C, and benefit forms the time to reach highest chemical conversion electricity
It presses 5-10 minutes constant.
Further, temperature dry described in step 11) is 100-400 DEG C.
Invention is detailed
1, pre-treatment
In chemical synthesizing method provided by the invention, the pre-treatment includes that etched foil or lamination foil are carried out hydration-treated and molten
Liquid impregnates two steps.
The temperature of the hydration-treated is 95-100 DEG C, and the time is 8-15 minutes.
The non-limiting example of the hydration-treated temperature includes: 95 DEG C, 96 DEG C, 97 DEG C, 98 DEG C, 99 DEG C or 100 DEG C, etc.
Deng.
The non-limiting example of the hydration-treated time includes: 8 minutes, 9 minutes, 10 minutes, 11 minutes, 12 minutes,
13 minutes, 14 minutes or 15 minutes, etc..
The etched foil or lamination foil by after hydration-treated, the oxidation film of formation it is outermost have it is loose porous
Oxidation film exists, and is a kind of defect film, is to cause the biggish one of the main reasons of Waste Acid From Hua Cheng Foil leakage current.At the solution dipping
Reason can eliminate the loose porous oxidation film generated in hydration-treated, and improve the property of oxidation film, to reach reduction electric leakage
The purpose of stream.
The solution dipping is organic acid soln or alkalescent inorganic salt solution with solution.
The concentration of the organic acid soln be 0.6-2.0wt%, preferably 0.6-1.5wt%, such as: 0.6wt%,
0.7wt%, 0.8wt%, 0.9wt%, 1.0wt%, 1.2wt% or 1.5wt%, etc..
The concentration of the alkalescent inorganic salt solution be 0.1-2.0wt%, preferred 0.4-1wt%, such as: 0.4wt%,
0.5wt%, 0.6wt%, 0.7wt%, 0.8wt%, 0.9wt% or 1wt%, etc..
Organic acid in the organic acid soln is selected from fumaric acid, adipic acid, citric acid, tartaric acid, salicylic acid, benzoic acid
One of or at least two combination.
Inorganic salts in the alkalescent inorganic salt solution are selected from one of phosphate, borate, carbonate, silicate
Or at least two combination.
In some embodiments, the alkalescent inorganic salt solution is in ammonium pentaborate solution and sodium bicarbonate solution
One kind.
" alkalescent " refers to that the size of pH value is 8-13.
The temperature of solution dipping is not easy more than 90 DEG C, if it exceeds 90 DEG C, then the oxygen of soluble endothecium structure densification
Change film layer, energy consumption is caused to increase.Preferably, the temperature of the solution dipping is 50-90 DEG C, more preferably 60-90 DEG C.
The non-limiting example of the temperature of solution dipping include: 60 DEG C, 65 DEG C, 70 DEG C, 75 DEG C, 80 DEG C, 85 DEG C or
90 DEG C, etc..
The time of the solution dipping is 1-30 minutes.
When dipping is organic acid soln with solution, it is preferred that the time of the solution dipping is 2-10 minutes, such as: 2
Minute, 3 minutes, 4 minutes, 5 minutes, 6 minutes, 7 minutes, 8 minutes or 10 minutes, etc..
When dipping is alkalescent inorganic salt solution with solution, it is preferred that the time of the solution dipping is 4-20 minutes,
Such as: 4 minutes, 5 minutes, 6 minutes, 7 minutes, 8 minutes, 10 minutes, 12 minutes, 16 minutes, 18 minutes or 20 minutes, etc..
2, level Four is melted into
The level Four chemical conversion as successively carries out level-one chemical conversion, second level chemical conversion, three-level chemical conversion and level Four chemical conversion, can be used and appoints
What chemical synthesizing method known in the art carries out.
Preferably, the condition control of the level Four chemical conversion is as follows:
The level Four chemical conversion forming liquid is the aqueous solution containing 2-10wt% boric acid and 0.01-1wt% ammonium borate.
Preferably, in the forming liquid boric acid concentration be 4-7wt%, such as: 4wt%, 4.5wt%, 5wt%,
5.5wt%, 6.0wt%, 6.5wt% or 7wt%, etc..
Preferably, the concentration of ammonium borate is 0.1-1.0wt% in the forming liquid, such as: 0.1wt%, 0.2wt%,
0.3wt%, 0.4wt%, 0.5wt%, 0.6wt%, 0.7wt%, 0.8wt%, 0.9wt% or 1.0wt%, etc..
The level Four chemical conversion temperature is 75-90 DEG C, such as: 75 DEG C, 80 DEG C, 85 DEG C or 90 DEG C, etc..
The level Four chemical conversion time is to reach ceiling voltage constant pressure holding 5-20 minutes, preferably 10-20 minutes, example
Such as: 10 minutes, 12 minutes, 14 minutes, 15 minutes, 16 minutes, 18 minutes or 20 minutes, etc..
In the level Four chemical conversion highest formation voltage of chemical conversion at different levels be followed successively by final voltage 30 ± 2%, 60 ± 2%,
90 ± 2%, 100%, current density 10-60mA/cm2。
Such as: if final voltage is 520V, the highest formation voltage of the level-one chemical conversion is 160V, the second level
At highest formation voltage be 320V, the highest formation voltage of three-level chemical conversion is 470V, the maximum of the level Four chemical conversion
It is 520V at voltage.
Preferably, the current density is 20-40mA/cm2, such as: 20mA/cm2、25mA/cm2、30mA/cm2、35mA/
cm2Or 40mA/cm2, etc..
3, it is heat-treated
In chemical synthesizing method provided by the invention, comprising being heat-treated twice.
First time heat treatment in the step 3), i.e. heat treatment after level Four chemical conversion, actual conditions are as follows: the heat treatment
Temperature is 450-550 DEG C, and the heat treatment time is 1-4 minutes.
The non-limiting example of the first time heat treatment temperature includes: 450 DEG C, 580 DEG C, 500 DEG C, 520 DEG C or 550
DEG C, etc..
The non-limiting example of the first time heat treatment time includes: 1 minute, 2 minutes, 3 minutes or 4 minutes, etc..
Form that treated heat treatment, actual conditions are as follows: institute are mended in second in the step 8) heat treatment for that is, second
Stating heat treatment temperature is 550-580 DEG C, and the heat treatment time is 0.5-2 minutes.
Second of heat treatment temperature is increased, removes gas and exposure defect therein in oxide film dissolving as far as possible, favorably
In the reparation for mending formation processing.
The non-limiting example of second of heat treatment temperature includes: 550 DEG C, 560 DEG C, 570 DEG C or 580 DEG C, etc..
The non-limiting example of second of heat treatment time includes: 0.5 minute, 1 minute, 1.5 minutes or 2 minutes,
Etc..
4, impregnation
It include acid solution impregnation three times in chemical synthesizing method provided by the invention.
First time dipping in the step 4), i.e., the dipping after being heat-treated for the first time, actual conditions are as follows:
The first time dipping is ortho phosphorous acid solution with acid solution, and the concentration of the ortho phosphorous acid solution is 0.2-
1wt%, such as: 0.2wt%, 0.3wt%, 0.4wt%, 0.5wt%, 0.6wt%, 0.7wt%, 0.8wt%, 0.9wt% or
1.0wt%, etc..
The temperature of the first time dipping is 50-80 DEG C, such as: 50 DEG C, 55 DEG C, 60 DEG C, 65 DEG C, 70 DEG C, 75 DEG C or 80
DEG C, etc..
The time of the first time dipping is 3-12 minutes, such as: 3 minutes, 5 minutes, 6 minutes, 7 minutes, 8 minutes, 10
Minute or 12 minutes, etc..
Second in the step 6) dipping mends form that treated dipping, actual conditions for the first time are as follows:
Second of dipping is phosphoric acid solution with acid solution, and the concentration of the phosphoric acid solution is 4-15wt%, such as:
4wt%, 6wt%, 8wt%, 10wt%, 12wt% or 15wt%, etc..
The temperature of second of dipping is 50-75 DEG C, such as: 50 DEG C, 55 DEG C, 60 DEG C, 65 DEG C, 70 DEG C or 75 DEG C, etc.
Deng.
The time of second of dipping is 3-12 minutes, such as: 3 minutes, 5 minutes, 8 minutes, 10 minutes or 12 minutes,
Etc..
In the step 10) third time dipping, i.e., third time mend formed treated dipping, actual conditions are as follows:
The third time dipping is ammonium dihydrogen phosphate with phosphate solution, and the ammonium dihydrogen phosphate concentration is 1-
8wt%, such as: 1wt%, 2wt%, 3wt%, 4wt%, 5wt%, 6wt%, 7wt% or 8wt%, etc..
The temperature of the third time dipping is 40-75 DEG C, such as: 40 DEG C, 50 DEG C, 60 DEG C, 70 DEG C or 75 DEG C, etc..
The time of the third time dipping is 1-5 minutes, such as: 1 minute, 2 minutes, 3 minutes, 4 minutes or 5 minutes, etc.
Deng.
5, formation processing is mended
In chemical synthesizing method provided by the invention, comprising mending formation processing three times.
The formation forming liquid of mending three times is the aqueous solution containing 2-10wt% boric acid and 0.01-1wt% ammonium borate.
Preferably, in the forming liquid boric acid concentration be 4-7wt%, such as: 4wt%, 4.5wt%, 5wt%,
5.5wt%, 6.0wt%, 6.5wt% or 7wt%, etc..
Preferably, the concentration of ammonium borate is 0.1-1.0wt% in the forming liquid, such as: 0.1wt%, 0.2wt%,
0.3wt%, 0.4wt%, 0.5wt%, 0.6wt%, 0.7wt%, 0.8wt%, 0.9wt% or 1.0wt%, etc..
The formation temperature of mending three times is 75-90 DEG C, such as: 75 DEG C, 80 DEG C, 85 DEG C or 90 DEG C, etc..
Described mend three times forms the time to reach highest formation voltage constant pressure and being kept for 5-10 minutes, such as: 5 minutes, 6 points
Clock, 7 minutes, 8 minutes, 9 minutes or 10 minutes, etc..
The formation voltage mended when forming processing is final formation voltage, current density 10-60mA/cm2。
Preferably, the current density is 20-40mA/cm2, such as: 20mA/cm2、25mA/cm2、30mA/cm2、35mA/
cm2Or 40mA/cm2, etc..
6, it post-processes
The post-processing includes the steps that washing and drying.
The drying carries out at high temperature, as far as possible the reduction outermost water content of oxidation film, advantageously reduces electric leakage
Stream.
Specifically, the drying temperature be 100-400 DEG C, preferably 250-300 DEG C, such as: 250 DEG C, 260 DEG C, 270
DEG C, 280 DEG C, 290 DEG C or 300 DEG C, etc..
The time of the drying is 1-4 minutes, such as: 1 minute, 2 minutes, 3 minutes or 4 minutes, etc..
The invention has the benefit that
(1) in the present invention after etched foil or lamination foil hydration-treated by organic acid soln or alkalescent inorganic salt solution
Middle carry out impregnation, can effectively eliminate loose porous oxidation film layer present in hydration-treated, improves the property of oxidation film,
Leakage current purpose is reduced to reach；
(2) second of depolarising heat treatment temperature is increased in the present invention, exposes the discharge of the defects of oxidation film as far as possible
Gas therein is conducive to the subsequent reparation mended and form processing, to be also beneficial to the reduction of leakage current；
(3) the outermost water content of oxidation film can be effectively removed by improving drying temperature in the present invention in last handling process,
Leakage current can further be reduced.
Detailed description of the invention
Fig. 1 is the flow chart of the method provided by the invention for reducing medium-high pressure chemical foil leakage current.
Specific embodiment
To keep the technical problems solved, the adopted technical scheme and the technical effect achieved by the invention clearer, below
It will the technical scheme of the embodiment of the invention will be described in further detail in conjunction with attached drawing, it is clear that described embodiment is only
It is a part of the embodiment of the present invention, instead of all the embodiments.
Embodiment 1
1) pre-treatment: using thick 120 μm of mesohigh etched foil, boiling 12 minutes, are then immersed in 100 DEG C of pure water
In concentration 0.6wt%, the citric acid solution that temperature is 70 DEG C, kept for 10 minutes；
2) level Four be melted into: by the foil after pre-treatment in the aqueous solution of 5wt% boric acid+0.6wt% ammonium borate in 85 DEG C into
Row anodized, current density 30mA/cm2, constant current boost arrival 180V, constant pressure holding 10 minutes；Then in 5wt%
In 85 DEG C of progress anodizeds, current density 30mA/cm in the aqueous solution of boric acid+0.4wt% ammonium borate2, constant current liter
It is pressed onto up to 360V, constant pressure is kept for 10 minutes；Then in 85 DEG C of progress sun in the aqueous solution of 5wt% boric acid+0.2wt% ammonium borate
Pole oxidation processes, current density 30mA/cm2, constant current boost arrival 520V, constant pressure holding 12 minutes；Then in 5wt% boric acid
In 85 DEG C of progress anodizeds, current density 30mA/cm in the aqueous solution of+0.1wt% ammonium borate2, constant current boost arrives
Up to 580V, constant pressure is kept for 15 minutes；
3) be heat-treated for the first time: the foil after level Four is melted into is washed, and is then heat-treated 2 under 550 DEG C of air atmospheres
Minute；
4) impregnate for the first time: the foil after first time is heat-treated is molten for 60 DEG C of ortho phosphorous acid in concentration 0.5wt%, temperature
It is impregnated 8 minutes in liquid；
5) mend formation processing for the first time: the foil after first time is impregnated is in the water-soluble of 5wt% boric acid+0.1wt% ammonium borate
It mends to form processing in 85 DEG C of progress anodic oxidations in liquid, current density 30mA/cm2, constant current boost arrival 580V, constant pressure holding
8 minutes；
6) second impregnates: first time is mended to the phosphoric acid solution that the foil that forms that treated is 60 DEG C in concentration 8wt% temperature
Middle dipping 8 minutes；
7) mend formation processing second: the foil after second is impregnated is in the water-soluble of 5wt% boric acid+0.1wt% ammonium borate
It mends to form processing in 85 DEG C of progress anodic oxidations in liquid, current density 30mA/cm2, constant current boost arrival 580V, constant pressure holding
8 minutes；
8) it second is heat-treated: will mend for second and form that treated foil is washed, then under 580 DEG C of air atmospheres
Heat treatment 1 minute；
9) third time mends formation processing: the foil after second is heat-treated is at 85 DEG C of ammonium borate of 5wt% boric acid+0.1wt%
It carries out anodic oxidation in aqueous solution to mend to form processing, current density 30mA/cm2, constant current boost arrival 580V, constant pressure holding 8
Minute；
10) third time impregnates: third time being mended and forms that treated that foil is washed, then in concentration 5wt%, temperature 60
DEG C ammonium dihydrogen phosphate in impregnate 2 minutes；
11) post-process: the foil after third time is impregnated wash in the air atmosphere for be placed on 300 DEG C and is dried 2 minutes
Obtain Waste Acid From Hua Cheng Foil.
Embodiment 2
1) pre-treatment: using thick 120 μm of mesohigh etched foil, boiling 12 minutes in 100 DEG C of pure water；It is then immersed in
In concentration 0.9wt%, the fumaric acid solution that temperature is 80 DEG C, kept for 10 minutes；
Step 2) -11) it is same as Example 1.
Embodiment 3
1) pre-treatment: using thick 120 μm of mesohigh etched foil, boiling 12 minutes in 100 DEG C of pure water；It is then immersed in
In concentration 0.4wt%, the ammonium pentaborate solution that temperature is 80 DEG C, kept for 8 minutes；
Step 2) -11) it is same as Example 1.
Embodiment 4
1) pre-treatment: using thick 130 μm of lamination foil, boiling 8 minutes in 100 DEG C of pure water；It is then immersed in concentration
In 0.4wt%, the sodium bicarbonate solution that temperature is 80 DEG C, kept for 4 minutes；
2) level Four be melted into: by the foil after pre-treatment in the aqueous solution of 5wt% boric acid+0.6wt% ammonium borate in 85 DEG C into
Row anodized, current density 30mA/cm2, constant current boost arrival 160V, constant pressure holding 10 minutes；Then in 5wt%
In 85 DEG C of progress anodizeds, current density 30mA/cm in the aqueous solution of boric acid+0.4wt% ammonium borate2, constant current liter
It is pressed onto up to 320V, constant pressure is kept for 10 minutes；Then in 85 DEG C of progress sun in the aqueous solution of 5wt% boric acid+0.2wt% ammonium borate
Pole oxidation processes, current density 30mA/cm2, constant current boost arrival 480V, constant pressure holding 12 minutes；Then in 5wt% boric acid
In 85 DEG C of progress anodizeds, current density 30mA/cm in the aqueous solution of+0.1wt% ammonium borate2, constant current boost arrives
Up to 520V, constant pressure is kept for 15 minutes；
3) be heat-treated for the first time: the foil after level Four is melted into is washed, and is then heat-treated 2 under 550 DEG C of air atmospheres
Minute；
4) impregnate for the first time: the foil after first time is heat-treated is molten for 60 DEG C of ortho phosphorous acid in concentration 0.5wt%, temperature
It is impregnated 8 minutes in liquid；
5) mend formation processing for the first time: the foil after first time is impregnated is in the water-soluble of 5wt% boric acid+0.1wt% ammonium borate
It mends to form processing in 85 DEG C of progress anodic oxidations in liquid, current density 30mA/cm2, constant current boost arrival 520V, constant pressure holding
8 minutes；
6) second impregnates: will mend the foil that forms that treated for the first time in concentration 8wt%, the phosphoric acid solution that temperature is 60 DEG C
Middle dipping 8 minutes；
7) mend formation processing second: the foil after second is impregnated is in the water-soluble of 5wt% boric acid+0.1wt% ammonium borate
It mends to form processing in 85 DEG C of progress anodic oxidations in liquid, current density 30mA/cm2, constant current boost arrival 520V, constant pressure holding
8 minutes；
8) it second is heat-treated: mending for second and to form that treated foil is washed, it is then hot under 580 DEG C of air atmospheres
Processing 1 minute；
9) third time mends formation processing: the water of foil after second is heat-treated in 5wt% boric acid+0.1wt% ammonium borate
It mends to form processing in 85 DEG C of progress anodic oxidations in solution, current density 30mA/cm2, constant current boost arrival 520V, constant pressure guarantor
It holds 8 minutes；
10) third time impregnates: third time being mended and forms treated foil in concentration 5wt%, the di(2-ethylhexyl)phosphate that temperature is 60 DEG C
It is impregnated 2 minutes in hydrogen ammonium salt solution；
11) post-process: the foil after third time is impregnated wash in the air atmosphere for be placed on 300 DEG C and is dried 2 minutes
Obtain Waste Acid From Hua Cheng Foil.
Embodiment 5
1) pre-treatment: using thick 130 μm of lamination foil, boiling 8 minutes in 100 DEG C of pure water；It is then immersed in concentration
In 0.4wt%, ammonium pentaborate solution at a temperature of 90 °C, kept for 8 minutes；
Step 2) -11) it is same as Example 4.
Embodiment 6
1) pre-treatment: using thick 130 μm of lamination foil, boiling 8 minutes in 100 DEG C of pure water；It is then immersed in concentration
In 0.4wt%, ammonium pentaborate solution at a temperature of 90 °C, kept for 16 minutes；
Step 2) -11) it is same as Example 4.
Embodiment 7
1) pre-treatment: using thick 130 μm of lamination foil, boiling 8 minutes in 100 DEG C of pure water；It is then immersed in concentration
In 1.2wt%, the solution of adipic acid that temperature is 60 DEG C, kept for 6 minutes；
Step 2) -11) it is same as Example 4.
Embodiment 8
1) pre-treatment: using thick 130 μm of lamination foil, boiling 8 minutes in 100 DEG C of pure water；It is then immersed in concentration
In 0.93wt%, the fumaric acid solution that temperature is 70 DEG C, kept for 6 minutes；
Step 2) -11) it is same as Example 4.
Comparative example 1
1) pre-treatment: using thick 120 μm of mesohigh etched foil, boiling 12 minutes in 100 DEG C of pure water；
Step 2) -11) it is same as Example 1.
Comparative example 2
1) pre-treatment: using thick 130 μm of lamination foil, boiling 8 minutes in 100 DEG C of pure water；
Step 2) -11) it is same as Example 4.
Performance test
The Waste Acid From Hua Cheng Foil that embodiment 1-8 and comparative example 1-2 are obtained is water-soluble in the boric acid that concentration is 7wt%, temperature is 65 DEG C
In liquid, permanent charging voltage is to reach voltage/1.07, is 0.4mA/cm in charging current2Lower test 900 minutes.Test result column
In table 1.
The leakage current test result of 1 Waste Acid From Hua Cheng Foil of table
By the test result of table 1 it is found that compared with comparative example 1 and 2, for etched foil, the case where specific volume slightly reduces
Under, the leakage current for the Waste Acid From Hua Cheng Foil that 1-3 of the embodiment of the present invention is provided reduces obviously, and the range of decrease is greater than 11%, especially 0-5h minimum and leaks
Current value, minimum can be reduced to 8.7 μ A/cm2, 36% is decreased by compared with comparative example 1；For lamination foil, the present invention is real
The leakage current for applying the Waste Acid From Hua Cheng Foil that a 4-8 is provided also reduces obviously, and especially 0-5h minimum leakage flow valuve, minimum can be reduced to
9.7μA/cm2, 41.9% is decreased by compared with comparative example 2.Show oxidation film in Waste Acid From Hua Cheng Foil provided in an embodiment of the present invention
Defect is greatly decreased, and leakage current is greatly reduced.
The technical principle of the invention is described above in combination with a specific embodiment.These descriptions are intended merely to explain of the invention
Principle, and shall not be construed in any way as a limitation of the scope of protection of the invention.Based on the explanation herein, the technology of this field
Personnel can associate with other specific embodiments of the invention without creative labor, these modes are fallen within
Within protection scope of the present invention.
Claims (10)
1. a kind of method for reducing medium-high pressure chemical foil leakage current, which comprises the following steps:
1) pre-treatment: etched foil or lamination foil are successively subjected to hydration-treated and solution impregnates；
2) level Four is melted into: the foil after pre-treatment is placed in progress level Four chemical conversion in forming liquid；
3) be heat-treated for the first time: the foil after level Four is melted into carries out first time heat treatment；
4) impregnate for the first time: the foil after first time is heat-treated is placed in progress first time dipping in acid solution；
5) mend formation processing for the first time: the foil after first time is impregnated, which is placed in forming liquid, to carry out mending formation processing for the first time；
6) second impregnates: will mend the foil that forms that treated for the first time and be placed in acid solution and carry out second and impregnate；
7) second of benefit formation processing: the foil after second is impregnated, which is placed in forming liquid, to carry out mending formation processing for the second time；
8) it second is heat-treated: the foil that forms that treated will be mended for second carries out second and be heat-treated；
9) third time is mended formation and handled: the foil after second is heat-treated, which is placed in forming liquid, carries out third time benefit formation processing；
10) third time impregnates: third time being mended and forms that treated foil is placed in progress third time dipping in phosphate solution；
11) post-process: the foil after third time is impregnated is washed, is dried, and Waste Acid From Hua Cheng Foil is obtained.
2. a kind of method for reducing medium-high pressure chemical foil leakage current according to claim 1, which is characterized in that in step 1)
Solution dipping in the pre-treatment is organic acid soln or alkalescent inorganic salt solution with solution.
3. a kind of method for reducing medium-high pressure chemical foil leakage current according to claim 2, which is characterized in that described organic
The concentration of acid solution is 0.6-2.0wt%, and the concentration of the alkalescent inorganic salt solution is 0.1-2.0wt%.
4. a kind of method for reducing medium-high pressure chemical foil leakage current according to claim 2 or 3, which is characterized in that described
Organic acid in organic acid soln is selected from one of fumaric acid, adipic acid, citric acid, tartaric acid, salicylic acid, benzoic acid or extremely
Few two kinds of combination；Inorganic salts in the alkalescent inorganic salt solution are in phosphate, borate, carbonate, silicate
One kind or at least two combination.
5. a kind of method for reducing medium-high pressure chemical foil leakage current according to claim 1, which is characterized in that in step 1)
The temperature of solution dipping in the pre-treatment is 50-90 DEG C, and the time of solution dipping is 1-30 minutes.
6. a kind of method for reducing medium-high pressure chemical foil leakage current according to claim 1, which is characterized in that in step 2)
The level Four chemical conversion forming liquid is the aqueous solution containing 2-10wt% boric acid and 0.01-1wt% ammonium borate；The level Four chemical conversion
Temperature is 75-90 DEG C, and the level Four chemical conversion time is to reach ceiling voltage constant pressure to be kept for 5-20 minutes；It is each in the level Four chemical conversion
The highest formation voltage of grade chemical conversion is followed successively by 30 ± 2%, 60 ± 2%, 90 ± 2%, the 100% of final voltage, and current density is
10~60mA/cm2。
7. a kind of method for reducing medium-high pressure chemical foil leakage current according to claim 1, which is characterized in that in step 3)
The temperature of the first time heat treatment is 450-550 DEG C, and the time is 1-4 minutes；The temperature of second of heat treatment described in step 8)
Degree is 550-580 DEG C, and the time is 0.5-2 minutes.
8. a kind of method for reducing medium-high pressure chemical foil leakage current according to claim 1, which is characterized in that in step 4)
The first time dipping ortho phosphorous acid solution that acid solution is that concentration is 0.2-1wt%, dipping temperature are 50-80 DEG C, dipping
Time is 3-12 minutes；The phosphoric acid solution that acid solution is that concentration is 4-15wt% of second of dipping described in step 6), dipping
Temperature is 50-75 DEG C, and dip time is 3-12 minutes；It is 1- that dipping, which is concentration with phosphate, for the third time described in step 10)
The ammonium dihydrogen phosphate of 8wt%, dipping temperature are 40-75 DEG C, and dip time is 1-5 minutes.
9. a kind of method for reducing medium-high pressure chemical foil leakage current according to claim 1, which is characterized in that step 5),
Mending described in step 7) and step 9) and forming processing forming liquid is containing 2-10wt% boric acid and 0.01-1wt% ammonium borate
Aqueous solution；Mending formation temperature is 75-90 DEG C, and benefit forms the time to reach highest formation voltage constant pressure and being kept for 5-10 minutes；
The formation voltage mended when forming processing is final formation voltage, and current density is 10~60mA/cm2。
10. a kind of method for reducing medium-high pressure chemical foil leakage current according to claim 1, which is characterized in that step 11)
Described in dry temperature be 100-400 DEG C.
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