CN116752198A - Novel formation method of anode foil of aluminum electrolytic capacitor - Google Patents
Novel formation method of anode foil of aluminum electrolytic capacitor Download PDFInfo
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- CN116752198A CN116752198A CN202310919107.5A CN202310919107A CN116752198A CN 116752198 A CN116752198 A CN 116752198A CN 202310919107 A CN202310919107 A CN 202310919107A CN 116752198 A CN116752198 A CN 116752198A
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- aluminum foil
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- 239000011888 foil Substances 0.000 title claims abstract description 99
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 title claims abstract description 88
- 229910052782 aluminium Inorganic materials 0.000 title claims abstract description 88
- 230000015572 biosynthetic process Effects 0.000 title claims abstract description 68
- 238000000034 method Methods 0.000 title claims abstract description 21
- 239000003990 capacitor Substances 0.000 title claims abstract description 16
- 239000007864 aqueous solution Substances 0.000 claims abstract description 49
- WNLRTRBMVRJNCN-UHFFFAOYSA-N adipic acid Chemical compound OC(=O)CCCCC(O)=O WNLRTRBMVRJNCN-UHFFFAOYSA-N 0.000 claims abstract description 40
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 claims abstract description 32
- 239000004327 boric acid Substances 0.000 claims abstract description 32
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 23
- FLDCSPABIQBYKP-UHFFFAOYSA-N 5-chloro-1,2-dimethylbenzimidazole Chemical compound ClC1=CC=C2N(C)C(C)=NC2=C1 FLDCSPABIQBYKP-UHFFFAOYSA-N 0.000 claims abstract description 20
- 239000001741 Ammonium adipate Substances 0.000 claims abstract description 20
- 239000001361 adipic acid Substances 0.000 claims abstract description 20
- 235000011037 adipic acid Nutrition 0.000 claims abstract description 20
- 235000019293 ammonium adipate Nutrition 0.000 claims abstract description 20
- 230000000737 periodic effect Effects 0.000 claims abstract description 17
- 238000002791 soaking Methods 0.000 claims abstract description 12
- KWSLGOVYXMQPPX-UHFFFAOYSA-N 5-[3-(trifluoromethyl)phenyl]-2h-tetrazole Chemical compound FC(F)(F)C1=CC=CC(C2=NNN=N2)=C1 KWSLGOVYXMQPPX-UHFFFAOYSA-N 0.000 claims abstract description 7
- 229910001379 sodium hypophosphite Inorganic materials 0.000 claims abstract description 7
- 230000007797 corrosion Effects 0.000 claims abstract description 4
- 238000005260 corrosion Methods 0.000 claims abstract description 4
- 235000010338 boric acid Nutrition 0.000 claims description 23
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 21
- 238000004140 cleaning Methods 0.000 claims description 18
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 14
- OTRAYOBSWCVTIN-UHFFFAOYSA-N OB(O)O.OB(O)O.OB(O)O.OB(O)O.OB(O)O.N.N.N.N.N.N.N.N.N.N.N.N.N.N.N Chemical compound OB(O)O.OB(O)O.OB(O)O.OB(O)O.OB(O)O.N.N.N.N.N.N.N.N.N.N.N.N.N.N.N OTRAYOBSWCVTIN-UHFFFAOYSA-N 0.000 claims description 12
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 7
- 239000000243 solution Substances 0.000 claims description 7
- YWYZEGXAUVWDED-UHFFFAOYSA-N triammonium citrate Chemical compound [NH4+].[NH4+].[NH4+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O YWYZEGXAUVWDED-UHFFFAOYSA-N 0.000 claims description 7
- 235000015165 citric acid Nutrition 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 6
- 239000011259 mixed solution Substances 0.000 claims description 4
- LFVGISIMTYGQHF-UHFFFAOYSA-N ammonium dihydrogen phosphate Chemical compound [NH4+].OP(O)([O-])=O LFVGISIMTYGQHF-UHFFFAOYSA-N 0.000 claims description 3
- 229910000387 ammonium dihydrogen phosphate Inorganic materials 0.000 claims description 3
- 235000019837 monoammonium phosphate Nutrition 0.000 claims description 3
- 238000004381 surface treatment Methods 0.000 claims description 3
- 239000006185 dispersion Substances 0.000 abstract description 6
- 238000004519 manufacturing process Methods 0.000 abstract description 6
- 230000000052 comparative effect Effects 0.000 description 6
- 239000001393 triammonium citrate Substances 0.000 description 4
- 235000011046 triammonium citrate Nutrition 0.000 description 4
- 238000010586 diagram Methods 0.000 description 3
- 238000004891 communication Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000007547 defect Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000011218 segmentation Effects 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25C—PROCESSES FOR THE ELECTROLYTIC PRODUCTION, RECOVERY OR REFINING OF METALS; APPARATUS THEREFOR
- C25C3/00—Electrolytic production, recovery or refining of metals by electrolysis of melts
- C25C3/06—Electrolytic production, recovery or refining of metals by electrolysis of melts of aluminium
- C25C3/08—Cell construction, e.g. bottoms, walls, cathodes
- C25C3/12—Anodes
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25C—PROCESSES FOR THE ELECTROLYTIC PRODUCTION, RECOVERY OR REFINING OF METALS; APPARATUS THEREFOR
- C25C3/00—Electrolytic production, recovery or refining of metals by electrolysis of melts
- C25C3/06—Electrolytic production, recovery or refining of metals by electrolysis of melts of aluminium
Abstract
The application discloses a novel formation method of an anode foil of an aluminum electrolytic capacitor, which comprises the following steps: firstly, putting the aluminum foil subjected to corrosion treatment into pure water with the temperature of 95 ℃ and above, and soaking for 5-12 min; putting into a first aqueous solution consisting of ammonium adipate, adipic acid, sodium hypophosphite and boric acid for formation, wherein the voltage output waveform is an asymmetric waveform, the amplitude of the formed voltage is controlled to be 0-1000V, the current is controlled to be 0-3000A, the time is controlled to be 1-999S, and the periodic cycle times are controlled to be 1-1000 times; the pH value of the first aqueous solution is 4-5, the conductivity is 4000-5000 mu S/cm, the formation temperature is 85-90 ℃, and the primary formation aluminum foil is obtained. The formation method can improve the production efficiency by more than 30%, save the production cost by more than 10%, and reduce the voltage-resistant dispersion by 30% compared with the traditional process.
Description
Technical Field
The application relates to the field of forming and processing of polar foils, in particular to a novel forming method of an anode foil of an aluminum electrolytic capacitor.
Background
The traditional formation method of the anode foil of the aluminum electrolytic capacitor has the defects that the dispersion of the withstand voltage of the formation foil is large, so that the anode foil with higher voltage level is required to be used for designing a product, and the product cost is increased. In addition, the traditional anode foil formation method adopts a staged constant voltage and constant current scheme, and has low energy utilization rate. Accordingly, a new formation method of anode foil for aluminum electrolytic capacitor is provided by those skilled in the art to solve the above-mentioned problems in the prior art.
Disclosure of Invention
The application aims to provide a novel formation method of an anode foil of an aluminum electrolytic capacitor, which aims to solve the problems in the background technology.
In order to achieve the above purpose, the present application provides the following technical solutions:
a novel formation method of an anode foil of an aluminum electrolytic capacitor comprises the following steps:
firstly, putting the aluminum foil subjected to corrosion treatment into pure water with the temperature of 95 ℃ and above, and soaking for 5-12 min; putting into a first aqueous solution consisting of ammonium adipate, adipic acid, sodium hypophosphite and boric acid for formation, wherein the voltage output waveform is an asymmetric waveform, the amplitude of the formed voltage is controlled to be 0-1000V, the current is controlled to be 0-3000A, the time is controlled to be 1-999S, and the periodic cycle times are controlled to be 1-1000 times; the PH value of the first aqueous solution is 4-5, the conductivity is 4000-5000 mu S/cm, the formation temperature is 85-90 ℃, and the primary formation aluminum foil is obtained;
step two, cleaning the primary formed aluminum foil obtained in the step one by pure water, placing the aluminum foil into a second aqueous solution of ammonium adipate, adipic acid and boric acid for forming, controlling the voltage output waveform to be an asymmetric waveform, and controlling the formation voltage amplitude to be 0-1000V, the current to be 0-3000A and the time to be 1-999S, wherein the periodic cycle number to be 1-1000 times; the pH value of the second aqueous solution is 4-5, the conductivity is 1500-2000 mu S/cm, the formation temperature is 85-90 ℃, and the secondary formation aluminum foil is obtained;
step three, cleaning the secondary formed aluminum foil obtained in the step two by pure water, soaking the aluminum foil in a triammonium citrate solution with the pH value of 4.5-5.5 and the conductivity of 20000-30000 mu S/cm, then placing the aluminum foil into a third aqueous solution of ammonium adipate, citric acid, adipic acid and boric acid for forming, wherein a voltage output waveform is an asymmetric waveform, and controlling the formed voltage amplitude to be 0-1000V, the current to be 0-3000A and the time to be 1-999S, and the periodic cycle number to be 1-1000; the PH value of the third aqueous solution is 4.5-5.5, the conductivity is 500-700 mu S/cm, the formation temperature is 85-90 ℃, and the three-stage formation aluminum foil is obtained;
step four, cleaning the three-stage formed aluminum foil obtained in the step three by pure water, then placing the aluminum foil into a fourth aqueous solution of boric acid and ammonium pentaborate for forming, controlling the voltage output waveform to be an asymmetric waveform, and controlling the formed voltage amplitude to be 0-1000V, the current to be 0-3000A and the time to be 1-999S, wherein the periodic cycle number to be 1-1000 times; the pH value of the fourth aqueous solution is 4.2-5.2, the conductivity is 400-500 mu S/cm, the formation temperature is 85-90 ℃, and the four-stage formation aluminum foil is obtained;
step five, cleaning the four-stage formed aluminum foil obtained in the step four by pure water, soaking the aluminum foil in the citric acid tri-ammonium with the pH value of 7-9 and the conductivity of 20000-30000 mu S/cm, then placing the aluminum foil into a mixed solution of a fifth aqueous solution of boric acid and ammonium pentaborate and phosphoric acid for forming, controlling the voltage output waveform to be an asymmetric waveform, and controlling the formed voltage amplitude to be 0-1000V, the current to be 0-3000A and the time to be 1-999S, wherein the periodic cycle number to be 1-1000; the pH value of the fifth aqueous solution is 3.8-5.2, the conductivity is 130-400, the conductivity of phosphoric acid is 25000-35000 mu S/cm, the formation temperature is 85-90 ℃, and the five-stage formation aluminum foil is obtained;
step six, taking out the aluminum foil obtained in the step five, cleaning the aluminum foil with pure water, and performing heat treatment for 1-5 minutes in an environment with the temperature of 450-600 ℃;
and seventhly, placing the formed aluminum foil after heat treatment into an ammonium dihydrogen phosphate solution with the pH value of 4.5-6.0 and the conductivity of 4000-6000 mu S/cm for surface treatment for 1-10min, taking out the aluminum foil, cleaning the aluminum foil with pure water, and drying the aluminum foil at the drying temperature of 230 ℃ to obtain the medium-high voltage aluminum electrolytic capacitor anode foil.
As a further scheme of the application: the positive and negative voltage amplitude values in the first to fifth steps are adjustable, and the positive or negative wave patterns are independently set.
As a further scheme of the application: in the first aqueous solution, the weight percentage of ammonium adipate is 1-20%, the weight percentage of adipic acid is 1-20%, the weight percentage of sodium hypophosphite is 1-20%, and the weight percentage of boric acid is 1-20%;
in the second aqueous solution, the weight percentage of ammonium adipate is 1-20%, the weight percentage of adipic acid is 1-20% + boric acid is 1-20%;
in the third aqueous solution, the weight percentage of ammonium adipate is 1-20%, the weight percentage of citric acid is 1-20%, the weight percentage of adipic acid is 1-20%, and the weight percentage of boric acid is 1-20%;
in the fourth aqueous solution, the weight percentage of boric acid is 1-20%, and the weight percentage of ammonium pentaborate is 1-20%;
in the fifth step, in the fifth aqueous solution, the weight percentage of boric acid is 1-25%, and the weight percentage of ammonium pentaborate is 1-25%.
The application can improve the production efficiency by more than 30%, save the production cost by more than 10%, reduce the voltage dispersion by 30% compared with the traditional process, and the prepared formed foil has small voltage dispersion, low product cost and high energy utilization rate.
Drawings
FIG. 1 is a waveform diagram of a programmable high frequency DC power supply according to the present application;
FIG. 2 is a schematic diagram of superposition of formation waveforms in the present application;
FIG. 3 is a diagram of a data record formed in the present application.
Description of the embodiments
Referring to fig. 1-3, in an embodiment of the present application, a novel formation method of an anode foil of an aluminum electrolytic capacitor includes the following steps:
a novel formation method of an anode foil of an aluminum electrolytic capacitor comprises the following steps:
firstly, putting the aluminum foil subjected to corrosion treatment into pure water with the temperature of 95 ℃ and above, and soaking for 5-12 min; putting into a first aqueous solution consisting of ammonium adipate, adipic acid, sodium hypophosphite and boric acid for formation, wherein the voltage output waveform is an asymmetric waveform, the amplitude of the formed voltage is controlled to be 0-1000V, the current is controlled to be 0-3000A, the time is controlled to be 1-999S, and the periodic cycle times are controlled to be 1-1000 times; the PH value of the first aqueous solution is 4-5, the conductivity is 4000-5000 mu S/cm, the formation temperature is 85-90 ℃, and the primary formation aluminum foil is obtained;
step two, cleaning the primary formed aluminum foil obtained in the step one by pure water, placing the aluminum foil into a second aqueous solution of ammonium adipate, adipic acid and boric acid for forming, controlling the voltage output waveform to be an asymmetric waveform, and controlling the formation voltage amplitude to be 0-1000V, the current to be 0-3000A and the time to be 1-999S, wherein the periodic cycle number to be 1-1000 times; the pH value of the second aqueous solution is 4-5, the conductivity is 1500-2000 mu S/cm, the formation temperature is 85-90 ℃, and the secondary formation aluminum foil is obtained;
step three, cleaning the secondary formed aluminum foil obtained in the step two by pure water, soaking the aluminum foil in a triammonium citrate solution with the pH value of 4.5-5.5 and the conductivity of 20000-30000 mu S/cm, then placing the aluminum foil into a third aqueous solution of ammonium adipate, citric acid, adipic acid and boric acid for forming, wherein a voltage output waveform is an asymmetric waveform, and controlling the formed voltage amplitude to be 0-1000V, the current to be 0-3000A and the time to be 1-999S, and the periodic cycle number to be 1-1000; the PH value of the third aqueous solution is 4.5-5.5, the conductivity is 500-700 mu S/cm, the formation temperature is 85-90 ℃, and the three-stage formation aluminum foil is obtained;
step four, cleaning the three-stage formed aluminum foil obtained in the step three by pure water, then placing the aluminum foil into a fourth aqueous solution of boric acid and ammonium pentaborate for forming, controlling the voltage output waveform to be an asymmetric waveform, and controlling the formed voltage amplitude to be 0-1000V, the current to be 0-3000A and the time to be 1-999S, wherein the periodic cycle number to be 1-1000 times; the pH value of the fourth aqueous solution is 4.2-5.2, the conductivity is 400-500 mu S/cm, the formation temperature is 85-90 ℃, and the four-stage formation aluminum foil is obtained;
step five, cleaning the four-stage formed aluminum foil obtained in the step four by pure water, soaking the aluminum foil in the citric acid tri-ammonium with the pH value of 7-9 and the conductivity of 20000-30000 mu S/cm, then placing the aluminum foil into a mixed solution of a fifth aqueous solution of boric acid and ammonium pentaborate and phosphoric acid for forming, controlling the voltage output waveform to be an asymmetric waveform, and controlling the formed voltage amplitude to be 0-1000V, the current to be 0-3000A and the time to be 1-999S, wherein the periodic cycle number to be 1-1000; the pH value of the fifth aqueous solution is 3.8-5.2, the conductivity is 130-400 mu S/cm, the conductivity of phosphoric acid is 25000-35000 mu S/cm, the formation temperature is 85-90 ℃, and the five-stage formation aluminum foil is obtained;
step six, taking out the aluminum foil obtained in the step five, cleaning the aluminum foil with pure water, and performing heat treatment for 1-5 minutes in an environment with the temperature of 450-600 ℃;
and seventhly, placing the formed aluminum foil after heat treatment into an ammonium dihydrogen phosphate solution with the pH value of 4.5-6.0 and the conductivity of 4000-6000 mu S/cm for surface treatment for 1-10min, taking out the aluminum foil, cleaning the aluminum foil with pure water, and drying the aluminum foil at the drying temperature of 230 ℃ to obtain the medium-high voltage aluminum electrolytic capacitor anode foil.
In the third step, the secondary aluminum foil is soaked by the tri-ammonium citrate, so that the secondary aluminum foil is well transited and placed into the third water solution, and a better formation effect is realized; and fifthly, soaking the four-stage formed aluminum foil in the tri-ammonium citrate to ensure that the four-stage formed aluminum foil is well transited and placed into the mixed solution of the fifth aqueous solution and the phosphoric acid, thereby realizing better formation effect.
The asymmetric waveform includes asymmetric square wave, asymmetric sine wave, asymmetric triangular wave, and asymmetric sawtooth wave as shown in fig. 1.
As a further scheme of the application: the positive and negative voltage amplitude values in the first to fifth steps are adjustable, and the positive or negative wave patterns are independently set.
The method comprises the steps of setting an asymmetric waveform of voltage amplitude, current, time and voltage output by adopting a programmable high-frequency direct-current power supply device; the asymmetric voltage output waveform is set, the magnitude of positive and negative amplitude values are adjusted, the positive or negative waveform is independently set, the periodic cycle times are set, and all the settings of equipment integration industrial communication (such as RS-485 communication) and the like can be completed on an upper computer (a computer, an industrial personal computer).
In the first step, in the first aqueous solution, the weight percentage of ammonium adipate is 1-20%, the weight percentage of adipic acid is 1-20%, the weight percentage of sodium hypophosphite is 1-20%, and the weight percentage of boric acid is 1-20%;
in the second aqueous solution, the weight percentage of ammonium adipate is 1-20%, the weight percentage of adipic acid is 1-20% + boric acid is 1-20%;
in the third aqueous solution, the weight percentage of ammonium adipate is 1-20%, the weight percentage of citric acid is 1-20%, the weight percentage of adipic acid is 1-20%, and the weight percentage of boric acid is 1-20%;
in the fourth aqueous solution, the weight percentage of boric acid is 1-20%, and the weight percentage of ammonium pentaborate is 1-20%;
in the fifth step, in the fifth aqueous solution, the weight percentage of boric acid is 1-25%, and the weight percentage of ammonium pentaborate is 1-25%.
The 650V graded formation foil is selected, the conventional DC segmentation formation scheme is adopted for formation in the comparative example, the vehicle speed is 0.7m/min, and the extreme difference is 13; the scheme of the application has the vehicle speed of 1m/min and the extremely poor of 5, and can obtain the following table
| 650V graded foil (comparative example) | 650V graded foil (present scheme) | |
| Formation scheme | Current traditional DC sectionalization scheme | The superimposed asymmetric waveform scheme of the application |
| Vehicle speed | 0.7m/min | 1m/min |
| Extremely poor | 13 | 5 |
The obtained formation voltage values are as follows:
| comparison set | 1 | 2 | 3 | 4 | 5 | 6 | 7 | 8 | 9 | 10 | 11 | 12 | 13 | 14 | 15 |
| Comparative example | 650 | 655. | 654 | 652 | 655 | 654 | 657 | 660 | 658 | 652 | 654 | 657 | 657 | 652 | 653 |
| The proposal is that | 655 | 658 | 654 | 656 | 655 | 654 | 658 | 654 | 656 | 654 | 654 | 656 | 658 | 653 | 655 |
| Comparison set | 16 | 17 | 18 | 19 | 20 | 21 | 22 | 23 | 24 | 25 | 26 | 27 | 28 | 29 | 30 |
| Comparative example | 655 | 658 | 655 | 654 | 657 | 661 | 656 | 653 | 656 | 657 | 654 | 663 | 655 | 656 | 657 |
| The proposal is that | 655 | 658 | 654 | 655 | 656 | 656 | 655 | 654 | 656 | 658 | 656 | 657 | 655 | 655 | 658 |
| Comparison set | 31 | 32 | 33 | 34 | 35 | 36 | 37 | 38 | 39 | 40 | 41 | 42 | 43 | 44 | 45 |
| Comparative example | 657 | 654 | 658 | 657 | 650 | 654 | 657 | 657 | 659 | 659 | 655 | 655 | 652 | 652 | 651 |
| The proposal is that | 656 | 656 | 656 | 657 | 654 | 655 | 656 | 656 | 655 | 654 | 655 | 656 | 654 | 655 | 655 |
| Comparison set | 46 | 47 | 48 | 49 | 50 | 51 | 52 | 53 | 54 | ||||||
| Comparative example | 654 | 650 | 655 | 655 | 661 | 659 | 657 | 658 | 657 | ||||||
| The proposal is that | 654 | 654 | 655 | 656 | 657 | 655 | 657 | 656 | 654 |
Fig. 3 is an image of formation voltage data in the above table, and it can be seen from the above table that, on the premise that formation voltages are close, the vehicle speed of the formation method in the scheme is increased from 0.7m/min to 1m/min, the production efficiency is improved by more than 30%, the extremely poor is reduced from 13 to 5, and the voltage-withstand dispersion is reduced by 30% compared with that in the conventional scheme. The same amount of formation foil is produced, the required time of the scheme is shorter, the power cost can be saved, meanwhile, the depreciation rate of equipment is lower, thereby realizing the production cost saving by more than 10 percent, and the anode foil prepared by the formation foil obtained by adopting the scheme has small voltage dispersion difference, low product cost and high energy utilization rate.
The foregoing is only a preferred embodiment of the present application, but the scope of the present application is not limited thereto, and any person skilled in the art, who is within the scope of the present application, should make equivalent substitutions or modifications according to the technical scheme of the present application and the inventive concept thereof, and should be covered by the scope of the present application.
Claims (3)
1. The novel formation method of the anode foil of the aluminum electrolytic capacitor is characterized by comprising the following steps of:
firstly, putting the aluminum foil subjected to corrosion treatment into pure water with the temperature of 95 ℃ and above, and soaking for 5-12 min; putting into a first aqueous solution consisting of ammonium adipate, adipic acid, sodium hypophosphite and boric acid for formation, wherein the voltage output waveform is an asymmetric waveform, the amplitude of the formed voltage is controlled to be 0-1000V, the current is controlled to be 0-3000A, the time is controlled to be 1-999S, and the periodic cycle times are controlled to be 1-1000 times; the PH value of the first aqueous solution is 4-5, the conductivity is 4000-5000 mu S/cm, the formation temperature is 85-90 ℃, and the primary formation aluminum foil is obtained;
step two, cleaning the primary formed aluminum foil obtained in the step one by pure water, placing the aluminum foil into a second aqueous solution of ammonium adipate, adipic acid and boric acid for forming, controlling the voltage output waveform to be an asymmetric waveform, and controlling the formation voltage amplitude to be 0-1000V, the current to be 0-3000A and the time to be 1-999S, wherein the periodic cycle number to be 1-1000 times; the pH value of the second aqueous solution is 4-5, the conductivity is 1500-2000 mu S/cm, the formation temperature is 85-90 ℃, and the secondary formation aluminum foil is obtained;
step three, cleaning the secondary formed aluminum foil obtained in the step two by pure water, soaking the aluminum foil in the third aqueous solution of ammonium adipate, citric acid and adipic acid and boric acid with the pH value of 4.5-5.5 and the conductivity of 20000-30000, and then placing the aluminum foil into the third aqueous solution of ammonium adipate, citric acid and adipic acid and boric acid for forming, wherein the voltage output waveform is an asymmetric waveform, and the formed voltage amplitude is controlled to be 0-1000V, the current is controlled to be 0-3000A and the time is controlled to be 1-999S, and the periodic cycle times are controlled to be 1-1000 times; the PH value of the third aqueous solution is 4.5-5.5, the conductivity is 500-700 mu S/cm, the formation temperature is 85-90 ℃, and the three-stage formation aluminum foil is obtained;
step four, cleaning the three-stage formed aluminum foil obtained in the step three by pure water, then placing the aluminum foil into a fourth aqueous solution of boric acid and ammonium pentaborate for forming, controlling the voltage output waveform to be an asymmetric waveform, and controlling the formed voltage amplitude to be 0-1000V, the current to be 0-3000A and the time to be 1-999S, wherein the periodic cycle number to be 1-1000 times; the pH value of the fourth aqueous solution is 4.2-5.2, the conductivity is 400-500 mu S/cm, the formation temperature is 85-90 ℃, and the four-stage formation aluminum foil is obtained;
step five, cleaning the four-stage formed aluminum foil obtained in the step four by pure water, soaking the aluminum foil in the mixed solution of the phosphoric acid and a fifth aqueous solution of boric acid and ammonium pentaborate after soaking the aluminum foil in the ammonium citrate with the pH value of 7-9 and the conductivity of 20000-30000, controlling the voltage output waveform to be an asymmetric waveform, and controlling the formation voltage amplitude to be 0-1000V, the current to be 0-3000A and the time to be 1-999S, wherein the periodic cycle number to be 1-1000 times; the pH value of the fifth aqueous solution is 3.8-5.2, the conductivity is 130-400 mu S/cm, the conductivity of phosphoric acid is 25000-35000 mu S/cm, the formation temperature is 85-90 ℃, and the five-stage formation aluminum foil is obtained;
step six, taking out the aluminum foil obtained in the step five, cleaning the aluminum foil with pure water, and performing heat treatment for 1-5 minutes in an environment with the temperature of 450-600 ℃;
and seventhly, placing the formed aluminum foil after heat treatment into an ammonium dihydrogen phosphate solution with the pH value of 4.5-6.0 and the conductivity of 4000-6000 mu S/cm for surface treatment for 1-10min, taking out the aluminum foil, cleaning the aluminum foil with pure water, and drying the aluminum foil at the drying temperature of 230 ℃ to obtain the medium-high voltage aluminum electrolytic capacitor anode foil.
2. The novel formation method of the anode foil of the aluminum electrolytic capacitor as claimed in claim 1, wherein the method comprises the following steps: the positive and negative voltage amplitude values in the first to fifth steps are adjustable, and the positive or negative wave patterns are independently set.
3. The novel formation method of the anode foil of the aluminum electrolytic capacitor as claimed in claim 1, wherein the method comprises the following steps: in the first aqueous solution, the weight percentage of ammonium adipate is 1-20%, the weight percentage of adipic acid is 1-20%, the weight percentage of sodium hypophosphite is 1-20%, and the weight percentage of boric acid is 1-20%;
in the second aqueous solution, the weight percentage of ammonium adipate is 1-20%, the weight percentage of adipic acid is 1-20% + boric acid is 1-20%;
in the third aqueous solution, the weight percentage of ammonium adipate is 1-20%, the weight percentage of citric acid is 1-20%, the weight percentage of adipic acid is 1-20%, and the weight percentage of boric acid is 1-20%;
in the fourth aqueous solution, the weight percentage of boric acid is 1-20%, and the weight percentage of ammonium pentaborate is 1-20%;
in the fifth step, in the fifth aqueous solution, the weight percentage of boric acid is 2-25%, and the weight percentage of ammonium pentaborate is 1-25%.
Priority Applications (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310919107.5A CN116752198A (en) | 2023-07-26 | 2023-07-26 | Novel formation method of anode foil of aluminum electrolytic capacitor |
| CN202311582879.0A CN117535759A (en) | 2023-07-26 | 2023-11-24 | Formation method of anode foil of aluminum electrolytic capacitor |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310919107.5A CN116752198A (en) | 2023-07-26 | 2023-07-26 | Novel formation method of anode foil of aluminum electrolytic capacitor |
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| CN116752198A true CN116752198A (en) | 2023-09-15 |
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| CN202310919107.5A Pending CN116752198A (en) | 2023-07-26 | 2023-07-26 | Novel formation method of anode foil of aluminum electrolytic capacitor |
| CN202311582879.0A Pending CN117535759A (en) | 2023-07-26 | 2023-11-24 | Formation method of anode foil of aluminum electrolytic capacitor |
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| CN112530708A (en) * | 2020-10-30 | 2021-03-19 | 东莞东阳光科研发有限公司 | Method for preparing formed foil by using asymmetric intermittent positive and negative combined pulses |
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| JPH07235456A (en) * | 1993-12-28 | 1995-09-05 | Nippon Chikudenki Kogyo Kk | Etching method of aluminum foil for electrolytic capacitor |
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| CN102610390A (en) * | 2011-01-20 | 2012-07-25 | 严民 | Method for forming ultrahigh-voltage anode foil for aluminum electrolytic capacitors |
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| CN117535759A (en) | 2024-02-09 |
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