CN107254707B - Method for manufacturing multi-stage pore-forming rapid medium-high voltage electrode foil - Google Patents
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- 239000011888 foil Substances 0.000 title claims abstract description 42
- 238000000034 method Methods 0.000 title claims abstract description 18
- 238000004519 manufacturing process Methods 0.000 title abstract description 6
- 230000007797 corrosion Effects 0.000 claims abstract description 63
- 238000005260 corrosion Methods 0.000 claims abstract description 63
- 239000011148 porous material Substances 0.000 claims abstract description 13
- 238000005406 washing Methods 0.000 claims description 21
- 239000000126 substance Substances 0.000 claims description 18
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 17
- 229910052782 aluminium Inorganic materials 0.000 claims description 17
- 239000007788 liquid Substances 0.000 claims description 17
- 238000011282 treatment Methods 0.000 claims description 17
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 17
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 10
- 229910017604 nitric acid Inorganic materials 0.000 claims description 10
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 8
- 238000001035 drying Methods 0.000 claims description 8
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 6
- 239000000654 additive Substances 0.000 claims description 6
- 230000000996 additive effect Effects 0.000 claims description 6
- 238000005868 electrolysis reaction Methods 0.000 claims description 6
- 239000003792 electrolyte Substances 0.000 claims description 5
- 239000011259 mixed solution Substances 0.000 claims description 4
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 3
- 238000002791 soaking Methods 0.000 claims description 3
- 239000000243 solution Substances 0.000 claims description 3
- 239000004793 Polystyrene Substances 0.000 claims description 2
- 239000013543 active substance Substances 0.000 claims description 2
- 150000001450 anions Chemical class 0.000 claims description 2
- 239000000203 mixture Substances 0.000 claims description 2
- 229920002223 polystyrene Polymers 0.000 claims description 2
- 238000012545 processing Methods 0.000 abstract description 6
- 230000009286 beneficial effect Effects 0.000 abstract description 4
- 238000005516 engineering process Methods 0.000 abstract description 3
- 230000008859 change Effects 0.000 abstract description 2
- 230000008569 process Effects 0.000 description 8
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 6
- 230000015572 biosynthetic process Effects 0.000 description 4
- 239000003990 capacitor Substances 0.000 description 3
- 239000006185 dispersion Substances 0.000 description 3
- 230000003287 optical effect Effects 0.000 description 3
- 238000002360 preparation method Methods 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 2
- 230000010354 integration Effects 0.000 description 2
- 238000004891 communication Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000002848 electrochemical method Methods 0.000 description 1
- 238000006056 electrooxidation reaction Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25F—PROCESSES FOR THE ELECTROLYTIC REMOVAL OF MATERIALS FROM OBJECTS; APPARATUS THEREFOR
- C25F3/00—Electrolytic etching or polishing
- C25F3/02—Etching
- C25F3/04—Etching of light metals
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23F—NON-MECHANICAL REMOVAL OF METALLIC MATERIAL FROM SURFACE; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL; MULTI-STEP PROCESSES FOR SURFACE TREATMENT OF METALLIC MATERIAL INVOLVING AT LEAST ONE PROCESS PROVIDED FOR IN CLASS C23 AND AT LEAST ONE PROCESS COVERED BY SUBCLASS C21D OR C22F OR CLASS C25
- C23F1/00—Etching metallic material by chemical means
- C23F1/02—Local etching
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23F—NON-MECHANICAL REMOVAL OF METALLIC MATERIAL FROM SURFACE; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL; MULTI-STEP PROCESSES FOR SURFACE TREATMENT OF METALLIC MATERIAL INVOLVING AT LEAST ONE PROCESS PROVIDED FOR IN CLASS C23 AND AT LEAST ONE PROCESS COVERED BY SUBCLASS C21D OR C22F OR CLASS C25
- C23F1/00—Etching metallic material by chemical means
- C23F1/10—Etching compositions
- C23F1/14—Aqueous compositions
- C23F1/16—Acidic compositions
- C23F1/20—Acidic compositions for etching aluminium or alloys thereof
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25F—PROCESSES FOR THE ELECTROLYTIC REMOVAL OF MATERIALS FROM OBJECTS; APPARATUS THEREFOR
- C25F3/00—Electrolytic etching or polishing
- C25F3/02—Etching
- C25F3/14—Etching locally
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G9/00—Electrolytic capacitors, rectifiers, detectors, switching devices, light-sensitive or temperature-sensitive devices; Processes of their manufacture
- H01G9/004—Details
- H01G9/04—Electrodes or formation of dielectric layers thereon
- H01G9/048—Electrodes or formation of dielectric layers thereon characterised by their structure
- H01G9/055—Etched foil electrodes
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Abstract
The invention relates to a method for manufacturing a multi-stage pore-forming rapid medium-high voltage electrode foil, which improves the conventional single-stage constant-current pore-forming technology into the method adopting special waveform direct current multi-stage pore-forming, wherein each stage divides the total processing time into a plurality of different processing time periods, the connection point between the adjacent time periods is a time node, the current density is gradually changed along with the change of the processing node, the multi-stage pore-forming is beneficial to re-pore-forming of an un-pore-forming area, and simultaneously has the advantages of large pore-forming current density and small current density in a pore growth stage, and the extracorporeal circulation is added to pore-forming and pore-expanding, so that large pores are favorably formed, the capacity of corrosion foil is improved, and the.
Description
Technical Field
The invention relates to a corrosion manufacturing method of a multistage-pore-forming rapid medium-high voltage electrode foil for an aluminum electrolytic capacitor, belonging to the field of preparation of electrode foil corrosion technology.
Background
With the development of the electronic industry, the demand for electrode foils in the fields of communication products, aerospace, home appliances, and the like has sharply increased. Meanwhile, the requirements of the aluminum electrolytic capacitor for volume miniaturization, high performance and chip type are more and more obvious, and in order to realize the requirements, higher technical and quality requirements are provided for an electrode foil, and the specific volume of the anode aluminum foil used as the anode of the capacitor needs to be improved.
The electrode foil is prepared by a special corrosion formation process, the corrosion process takes the electronic optical foil as a raw material, and the electronic optical foil is etched by a chemical or electrochemical method to form holes on the surface, so that the specific surface area of the anode optical foil is increased, and the capacity of the corrosion foil is increased. The corrosion step is crucial and is the key step for determining whether the aluminum foil can be prepared into a high-performance electrode foil.
In the existing method for manufacturing the corrosion foil in China, a hole forming procedure is generally single-stage constant-current hole forming, under the condition of single-stage hole forming, a larger area of the surface of the corrosion foil still does not form an initial corrosion hole, in order to improve the corrosion specific volume, the corrosion electric quantity needs to be increased to improve the initial corrosion hole density, and after the corrosion current density is improved under the constant-current condition, the current density is too large in the hole growth stage to cause the surface of the aluminum foil to be dissolved, and the improvement of the specific volume of the aluminum foil is not facilitated. And pure electrochemical corrosion is basically adopted in the reaming stage, and the holes formed in the mode are smaller, so that the preparation of high-voltage formed foil is not facilitated. Meanwhile, at present, the hair holes and the reaming grooves adopt internal circulation of the groove body, and the temperature and the concentration of the groove liquid can form local unevenness, so that the transverse dispersion of the aluminum foil is large.
Disclosure of Invention
The invention aims to overcome the defects and provide a method for manufacturing a multi-stage pore-forming rapid medium-high voltage electrode foil. The hole-forming mode is changed by changing the current application method, a chemical and electrochemical mixed type hole-expanding corrosion process is adopted, and extracorporeal circulation is added to the hole-forming and hole-expanding simultaneously, so that the corrosion foil with high specific volume, high foil-reducing rate, high yield and low dispersion difference is obtained.
In order to realize the purpose of the invention, the invention adopts the following technical scheme:
the preparation method of the multistage perforation rapid medium-voltage electrode foil corrosion comprises the following steps:
1) pretreatment: taking a high-purity aluminum foil, soaking in a grade I tank liquor at the temperature of 50-90 ℃ for 1-3 minutes, and washing with water;
2) and (3) corrosion of grade I pores: the grade I pore formation is I-1 to I-5 common pentapole pore formation corrosion, the electrolyte is a mixed solution of 25-35% of sulfuric acid and 1-5% of hydrochloric acid, the temperature is 60-80 ℃, a special waveform direct current is adopted, and the electric quantity applied to each grade is 3.5-6.5C/cm2The electrolysis time is 15-25 seconds, and the water washing: the special waveform direct current is a gradual current which is constant current and then gradually reduced according to the size of a conductive negative electrode plate, the distance between an anode aluminum foil and the negative electrode plate and the conductive resistance of the electrolyte;
3) chemical and electrochemical pore-enlarging corrosion: the chemical reaming corrosion and the electrochemical reaming corrosion are respectively divided into 8 grades, wherein the chemical reaming corrosion 1 and the electrochemical reaming corrosion 1 are carried out till the chemical reaming corrosion 8 and the electrochemical reaming corrosion 8;
chemical reaming corrosion: the corrosive liquid is 1-5% of nitric acid and 1-10% of phosphoric acid, the temperature is 50-75 ℃, and the treatment time is 1-3 minutes;
electrochemical reaming corrosion: the corrosive liquid is a mixed liquid of 0.01-0.1 g/L of additive and 1-10% of nitric acid, II-1 of the corrosive liquid overflows to II-8 in sequence, the temperature is 60-80 ℃, conventional waveform direct current is adopted, and the applied electric quantity of each stage is 2-8C/cm2Electrolyzing for 60-90 seconds, and washing with water; the additive is 20000-100000 polystyrene anion active agent;
4) and (3) post-treatment: washing with 1-10% nitric acid as a treatment solution at 50-80 ℃ for 1-5 minutes;
5) and (3) drying treatment: and drying the mixture for 2 to 3 minutes at the temperature of between 150 and 250 ℃.
The water washing temperature among the steps is normal temperature, the water washing time is 1-3 minutes, and deionized water is adopted for water washing after the II-level reaming corrosion.
The invention has the following beneficial effects:
(1) the multi-stage special waveform direct current hair hole is added on the basis of the traditional single-stage constant current hair hole technology (the current applying mode used in the industry at present is only constant current), the total processing time of each stage is divided into a plurality of different processing time periods, the connecting point between the adjacent time periods is a time node, the current density changes gradually along with the change of the processing node, the multi-stage hair hole is beneficial to secondary hair hole of an un-hair hole area, and meanwhile, the multi-stage hair hole has the advantages of large hair hole current density and small current density in a hole growth stage, so that the hole density and the hole uniformity are increased, the product strength is high, the specific volume performance is high, the product strength and the specific volume performance are improved by 5% -10%, the market demand is met, the product quality of an electrode foil is ensured. And the corrosion amount is large, the thickness is thinner than that of the traditional corrosion foil, and the specific volume is high, so that the method conforms to the trend that the current electronic products develop towards volume miniaturization and integration.
(2) If the hole expanding process is a pure electrochemical process, the formed holes are small; the invention adopts a chemical and electrochemical mixed type hole expanding process, which is beneficial to forming large holes, thereby improving the capacity of the corrosion foil and being more suitable for high-voltage formation foil.
The properties of the electrode foils manufactured according to the present invention and the prior art are compared and shown in table 1.
TABLE 1
Drawings
FIG. 1 is a process flow diagram of the present invention.
Detailed Description
The technical solution of the present invention will be described with reference to the following specific examples:
example 1
(1) Pretreatment: taking an aluminum foil with the purity of 99.99 percent, and soaking in I-grade tank liquor at 60 ℃ for 3 minutes;
(2) first water washing, namely washing the pretreated aluminum foil with water at normal temperature for 2 minutes;
(3) and (3) corrosion of grade I pores: the grade I pore generation is divided into five-electrode pore generation corrosion of I-1 to I-5, the electrolyte is a mixed solution of 25 percent of sulfuric acid and 5 percent of hydrochloric acid, the temperature is 80 ℃, special waveform direct current is adopted, and the electric quantity is applied to each grade by 3.5C/cm2The electrolysis time is 25 seconds;
(4) and (3) second water washing: washing the aluminum foil subjected to the corrosion of the grade I pores at normal temperature for 2 minutes;
(5) reaming and corroding: the reaming corrosion is divided into chemical reaming corrosion and electrochemical reaming corrosion: the chemical reaming corrosion and the electrochemical reaming corrosion are respectively divided into 8 grades, namely chemical reaming corrosion 1 and electrochemical reaming corrosion 1 to chemical reaming corrosion 8 and electrochemical reaming corrosion 8;
chemical reaming corrosion: the corrosive liquid is 2.0 percent of nitric acid and 1.5 percent of phosphoric acid, the temperature is 75 ℃, and the treatment time is 2 minutes;
electrochemical reaming corrosion: the corrosive liquid is a mixed liquid of 0.01-0.1 g/L additive and 2.8% nitric acid, the temperature is 60 ℃, the conventional waveform direct current is adopted, and the applied electric quantity of each stage is 3C/cm2The electrolysis time is 80 seconds;
(6) and (3) third water washing: washing the aluminum foil subjected to the II-stage reaming corrosion at normal temperature for 2 minutes;
(7) the post-treatment liquid is 3.5 percent nitric acid, the temperature is 60 ℃, and the treatment time is 2 minutes;
(8) fourth water washing: washing the aluminum foil subjected to the II-stage reaming corrosion at normal temperature for 2 minutes;
(9) and (3) drying treatment: and drying the aluminum foil subjected to fourth washing at the temperature of 200 ℃ for 2-3 minutes.
The comparison of the main parameters of the processes used in examples 1-3 is shown in Table 2, wherein the first to fourth water washing, post-treatment and drying treatments of examples 2-3 are the same as those of example 1.
TABLE 2
Comparative example
The pretreatment, the first to fourth water washing, the post-treatment and the drying steps are the same as those of the example 1, and the difference from the example 1 is that: and (3) corrosion of grade I pores: the corrosive liquid is a mixed solution of 30% sulfuric acid and 4% hydrochloric acid, the temperature is 70 ℃, a constant current is adopted, and the electric quantity is applied to 20C/cm2The electrolysis time is 55 seconds;
and (3) stage II reaming corrosion: the corrosive liquid is a mixed liquid of 0.01-0.1 g/L additive and 2.8% nitric acid, the temperature is 60 ℃, and the applied electric quantity is 40C/cm2The electrolysis time was 540 seconds.
The test results of examples 1 to 3 of the present invention and comparative examples are shown in Table 3:
TABLE 3
The invention increases the hole density and the hole uniformity due to the special corrosion step, improves the product strength and specific volume performance, reduces the transverse dispersion difference, increases the foil reduction rate, and conforms to the trend of the electronic products developing towards volume miniaturization and integration at present.
Claims (1)
1. A method for preparing a multistage pore-forming rapid medium-voltage electrode foil through corrosion is characterized by comprising the following steps:
1) pretreatment: taking a high-purity aluminum foil, soaking in I-5 grade tank liquor at 50-90 ℃ for 1-3 minutes, and washing with water;
2) and (3) corrosion of grade I pores: the grade I pores are divided into grade I-1 to grade I-5 and five pore corrosion, and the electrolyte is 25-35% of sulfuric acidAnd 1-5% hydrochloric acid mixed solution at 60-80 deg.C, applying special waveform direct current, and applying electric quantity of 3.5-6.5C/cm2The electrolysis time is 15-25 seconds, and the water washing:
3) chemical and electrochemical pore-enlarging corrosion: the chemical reaming corrosion and the electrochemical reaming corrosion are respectively divided into 8 grades, wherein the chemical reaming corrosion 1 and the electrochemical reaming corrosion 1 are carried out to the chemical reaming corrosion 8 and the electrochemical reaming corrosion 8;
chemical reaming corrosion: the corrosive liquid is a mixed liquid of 1-5% of nitric acid and 1-10% of phosphoric acid, the temperature is 50-75 ℃, and the treatment time is 1-3 minutes;
electrochemical reaming corrosion: the corrosive liquid is a mixed liquid of 0.01-0.1 g/L of additive and 1-10% of nitric acid, the corrosive liquid overflows from II-1 to II-8 in sequence, the temperature is 60-80 ℃, direct current is adopted, and the applied electric quantity of each stage is 2-8C/cm2Electrolyzing for 60-90 seconds, and washing with water;
4) and (3) post-treatment: 1-10% of nitric acid is used as a treatment solution, the temperature is 50-80 ℃, the treatment time is 1-5 minutes, and the mixture is washed and dried; the additive is 20000-100000 polystyrene anion active agent;
the drying treatment is drying treatment for 2-3 minutes at the temperature of 150-250 ℃;
the special waveform direct current is a gradual current which is constant current firstly and then gradually reduced according to the size of a conductive negative electrode plate, the distance between an anode aluminum foil and the negative electrode plate and the conductive resistance of the electrolyte.
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| CN110923779B (en) * | 2019-11-27 | 2021-09-14 | 东莞东阳光科研发有限公司 | Ultrahigh pressure etched foil and etching method thereof |
| CN112038100B (en) * | 2020-07-15 | 2021-12-07 | 新疆众和股份有限公司 | Corrosion process of anode foil for high-voltage aluminum electrolytic capacitor |
| CN113279046A (en) * | 2021-05-20 | 2021-08-20 | 浙江丰川电子环保科技股份有限公司 | Rapid chemical corrosion process for anode aluminum foil for electrolytic capacitor |
| CN114164481B (en) * | 2021-11-12 | 2023-04-28 | 乳源瑶族自治县东阳光化成箔有限公司 | Hole forming corrosion method, medium-high pressure corrosion foil and preparation method thereof |
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