CN110164696B - Electrochemical corrosion process for producing medium-high voltage anode foil - Google Patents
Electrochemical corrosion process for producing medium-high voltage anode foil Download PDFInfo
- Publication number
- CN110164696B CN110164696B CN201910293767.0A CN201910293767A CN110164696B CN 110164696 B CN110164696 B CN 110164696B CN 201910293767 A CN201910293767 A CN 201910293767A CN 110164696 B CN110164696 B CN 110164696B
- Authority
- CN
- China
- Prior art keywords
- mass
- aluminum foil
- high voltage
- voltage anode
- foil
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
- 239000011888 foil Substances 0.000 title claims abstract description 137
- 238000000034 method Methods 0.000 title claims abstract description 58
- 238000006056 electrooxidation reaction Methods 0.000 title claims abstract description 29
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims abstract description 78
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 78
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 72
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 72
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 46
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 46
- 239000011259 mixed solution Substances 0.000 claims abstract description 40
- 239000000243 solution Substances 0.000 claims abstract description 30
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims abstract description 29
- 239000008367 deionised water Substances 0.000 claims abstract description 29
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 29
- 229910017604 nitric acid Inorganic materials 0.000 claims abstract description 29
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 29
- 238000005260 corrosion Methods 0.000 claims abstract description 26
- 230000007797 corrosion Effects 0.000 claims abstract description 26
- 238000001035 drying Methods 0.000 claims abstract description 24
- 238000005406 washing Methods 0.000 claims abstract description 17
- 238000002791 soaking Methods 0.000 claims abstract description 15
- 238000004080 punching Methods 0.000 claims abstract description 6
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 19
- HHIMNFJHTNVXBJ-UHFFFAOYSA-L zinc;dinitrite Chemical compound [Zn+2].[O-]N=O.[O-]N=O HHIMNFJHTNVXBJ-UHFFFAOYSA-L 0.000 claims description 16
- 238000004519 manufacturing process Methods 0.000 claims description 15
- 238000004140 cleaning Methods 0.000 claims description 12
- 239000003990 capacitor Substances 0.000 claims description 10
- LBLYYCQCTBFVLH-UHFFFAOYSA-N 2-Methylbenzenesulfonic acid Chemical compound CC1=CC=CC=C1S(O)(=O)=O LBLYYCQCTBFVLH-UHFFFAOYSA-N 0.000 claims description 8
- 238000005452 bending Methods 0.000 description 18
- 239000003112 inhibitor Substances 0.000 description 4
- 238000012360 testing method Methods 0.000 description 3
- 230000006978 adaptation Effects 0.000 description 2
- 239000000654 additive Substances 0.000 description 2
- 230000000996 additive effect Effects 0.000 description 2
- 238000007796 conventional method Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000010998 test method Methods 0.000 description 2
- 239000002253 acid Substances 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000005530 etching Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
Classifications
-
- 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
-
- 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
Landscapes
- Engineering & Computer Science (AREA)
- Power Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Electric Double-Layer Capacitors Or The Like (AREA)
- Cleaning And De-Greasing Of Metallic Materials By Chemical Methods (AREA)
Abstract
The invention discloses an electrochemical corrosion process for producing medium-high voltage anode foil, which comprises the following steps: A. pretreatment: putting the aluminum foil into a mixed solution of sodium hydroxide and potassium hydroxide at the temperature of 35-45 ℃, and soaking for 40-60 s; B. and (3) punching: placing the pretreated aluminum foil into a mixed solution containing 10-15% by mass of hydrochloric acid and 35-45% by mass of sulfuric acid at the temperature of 65-75 ℃, controlling the corrosion current density to be 250-400 mA/cm2, and performing perforation corrosion for 100-120 s; C. reaming: washing the aluminum foil subjected to hole forming with deionized water, putting the aluminum foil into a nitric acid solution with the temperature of 80-90 ℃ and the mass percent of 11-15%, controlling the hole expanding current to be 50-150 mA/cm2, and expanding the hole for 9-12 min; D. post-treatment; E. and (5) drying. The electrochemical corrosion process disclosed by the invention is simple in process, easy to control in process, capable of effectively ensuring the stable foil surface quality of the prepared medium-high voltage anode foil, and high in specific volume and strength.
Description
Technical Field
The invention relates to the technical field of production of medium and high voltage anode foils for aluminum electrolytic capacitors, in particular to an electrochemical corrosion process for producing the medium and high voltage anode foils.
Background
Because of simple manufacture, low price, superior performance and reliable quality, the aluminum electrolytic capacitor is widely applied to electric products. Moreover, with the rapid an ancient type of spoon development of the electrical and electronic industry, the production scale and market demand of aluminum electrolytic capacitors are still increasing. In order to meet the trend of miniaturization and high performance of electric products, capacitors with high specific capacitance need to be developed. The specific capacitance of an aluminum electrolytic capacitor is proportional to the effective surface area and dielectric constant of the dielectric layer thereof and inversely proportional to the thickness of the dielectric layer. Therefore, the high specific volume electrode foil manufacturing technology is mainly realized by three aspects: the improved etching process can increase the area expansion ratio, reduce the average dielectric layer thickness under a certain formation voltage and modify the dielectric layer to increase the dielectric constant. The thickness of the dielectric layer depends on the working voltage, the dielectric constant of the aluminum oxide film is a constant value, and therefore, enlarging the surface area of the aluminum foil through corrosion is a key technology for improving the specific capacitance of the corrosion foil.
However, the current electrochemical corrosion process for the production of medium and high voltage anode foils still has the following problems: the foil surface quality of the medium-high voltage anode foil is easy to be unstable due to improper control of the process; and the real corrosion coefficient of the medium-high voltage anode foil has a larger promotion space than the practical limit corrosion coefficient, so that the medium-high voltage anode foil with high specific volume and high strength (high bending times) is difficult to obtain.
Based on the situation, the invention provides an electrochemical corrosion process for producing medium-high voltage anode foils, which can effectively solve the problems.
Disclosure of Invention
The invention aims to provide an electrochemical corrosion process for producing medium-high voltage anode foils. The electrochemical corrosion process for producing the medium-high voltage anode foil is simple in process and easy to control in process, can effectively ensure stable foil surface quality of the prepared medium-high voltage anode foil, and has the performance of high specific volume and high strength (high bending times).
In order to solve the technical problems, the technical scheme provided by the invention is as follows:
an electrochemical corrosion process for the production of medium and high voltage anode foils comprising the steps of:
A. pretreatment:
putting the aluminum foil into a mixed solution of sodium hydroxide and potassium hydroxide at the temperature of 35-45 ℃, soaking for 40-60 s, and then washing for 2-5 times by using deionized water; the molar concentrations of the sodium hydroxide and the potassium hydroxide in the mixed solution of the sodium hydroxide and the potassium hydroxide are 0.06-0.08 mol/L and 0.02-0.03 mol/L respectively;
compared with the traditional pretreatment by acid, the pretreatment process steps have the advantages of higher treatment speed, higher efficiency, lower temperature during treatment, energy consumption saving, good treatment effect, capability of effectively ensuring the stable quality of the foil surface of the prepared medium-high voltage anode foil, and high specific volume and high strength (high bending times). In addition, compared with the single alkali such as sodium hydroxide or potassium hydroxide, the processing speed is higher, and the foil surface quality stability and high strength (high bending times) of the prepared medium-high voltage anode foil can be improved.
B. And (3) punching:
placing the pretreated aluminum foil into a mixed solution containing 10-15% by mass of hydrochloric acid and 35-45% by mass of sulfuric acid at the temperature of 65-75 ℃, controlling the corrosion current density to be 250-400 mA/cm2, and performing perforation corrosion for 100-120 s;
compared with the traditional perforation process steps, the pretreatment process steps better aim at the process system of the invention, optimize the process conditions, enable the process to be more easily and accurately controlled, ensure the foil surface quality of the prepared middle-high voltage anode foil to be stable, and have the performance of high specific volume and high strength (high bending times).
C. Reaming:
washing the aluminum foil subjected to hole forming with deionized water, putting the aluminum foil into a nitric acid solution with the temperature of 80-90 ℃ and the mass percent of 11-15%, controlling the hole expanding current to be 50-150 mA/cm2, and expanding the hole for 9-12 min;
compared with the traditional reaming process steps, the pretreatment process steps better aim at the process system of the invention, optimize the process conditions, enable the process to be more easily and accurately controlled, ensure the foil surface quality of the prepared medium-high voltage anode foil to be stable, and have the performance of high specific volume and high strength (high bending times).
D. And (3) post-treatment:
cleaning the aluminum foil after hole expansion by using deionized water, and soaking the aluminum foil in a nitric acid solution with the temperature of 70-80 ℃ and the mass percent of 3-5% for 2-3 min;
E. and (3) drying:
and (3) cleaning the post-treated aluminum foil with deionized water, putting the aluminum foil into drying equipment, controlling the temperature to be 70-90 ℃, and drying for 2-5 hours to obtain the medium-high voltage anode foil.
The electrochemical corrosion process for producing the medium-high voltage anode foil is simple in process and easy to control in process, can effectively ensure stable foil surface quality of the prepared medium-high voltage anode foil, and has the performance of high specific volume and high strength (high bending times).
Preferably, in the step A, the aluminum foil is an aluminum foil for an electrolytic capacitor anode with the aluminum content of more than or equal to 99.99% and the thickness of 120 um.
Preferably, in the step B, the mixed solution containing 10 to 15 mass% of hydrochloric acid and 35 to 45 mass% of sulfuric acid further contains 0.35 to 0.45 mass% of zinc nitrite.
In the pretreatment process steps, 0.35-0.45% of zinc nitrite is added as a corrosion inhibitor, so that the corrosion inhibitor is better adapted (matched) with the process system, the foil surface quality stability and the strength (bending times are high) of the prepared medium-high voltage anode foil can be improved, and the specific volume is also improved to a certain extent.
Preferably, in the step B, the mixed solution containing 10 to 15 mass% of hydrochloric acid and 35 to 45 mass% of sulfuric acid further contains 0.5 to 0.7 mass% of isopropyl alcohol.
In the pretreatment process steps, 0.5-0.7% of isopropanol is added as an additive, so that the process system is better adapted (matched), the specific volume and the foil surface quality stability of the prepared medium-high voltage anode foil are improved, and the strength (high bending times) is also improved to a certain extent.
Preferably, in the step C, the 11-15% by mass nitric acid solution further contains 0.65-0.85% by mass zinc nitrite.
In the pretreatment process steps, 0.65-0.85% of zinc nitrite is added as a corrosion inhibitor, so that the corrosion inhibitor is better adapted (matched) with the process system, the foil surface quality stability and the strength (bending times are high) of the prepared medium-high voltage anode foil can be improved, and the specific volume is also improved to a certain extent.
Preferably, in the step C, the nitric acid solution with the mass percentage of 11-15% further contains 0.15-0.25% of toluenesulfonic acid.
In the pretreatment process steps, 0.15-0.25% of toluenesulfonic acid is added as an additive, so that the process system is better adapted (matched), the specific volume and the foil surface quality stability of the prepared medium-high voltage anode foil are improved, and the strength (high bending frequency) is also improved to a certain extent.
Preferably, in step a, the pretreatment: putting the aluminum foil into a mixed solution of sodium hydroxide and potassium hydroxide at the temperature of 40 ℃, soaking for 55s, and then washing for 3 times by using deionized water; the molar concentrations of the sodium hydroxide and the potassium hydroxide in the mixed solution of the sodium hydroxide and the potassium hydroxide are 0.07mol/L and 0.024mol/L respectively;
preferably, in step B, the pore: placing the pretreated aluminum foil into a mixed solution containing 12.5 mass percent of hydrochloric acid and 42 mass percent of sulfuric acid at the temperature of 68 ℃, controlling the corrosion current density to be 280mA/cm2, and performing perforation corrosion for 110 s; the mixed solution containing 12.5 percent by mass of hydrochloric acid and 42 percent by mass of sulfuric acid also contains 0.41 percent by mass of zinc nitrite; the mixed solution containing 12.5% by mass of hydrochloric acid and 42% by mass of sulfuric acid also contains 0.65% by mass of isopropanol.
Preferably, in step C, reaming: washing the aluminum foil subjected to hole forming with deionized water, putting into a nitric acid solution with the temperature of 82 ℃ and the mass percent of 13%, controlling the hole-expanding current to be 75mA/cm2, and expanding the hole for 11 min; the nitric acid solution with the mass percentage of 13 percent also contains zinc nitrite with the mass percentage of 0.75 percent; the nitric acid solution with the mass percent of 13% also contains 0.18% of toluenesulfonic acid with the mass percent.
Preferably, in step E, the drying device is an oven.
Compared with the prior art, the invention has the following advantages and beneficial effects:
the electrochemical corrosion process for producing the medium-high voltage anode foil is simple in process and easy to control in process, can effectively ensure stable foil surface quality of the prepared medium-high voltage anode foil, and has the performance of high specific volume and high strength (high bending times).
Detailed Description
In order that those skilled in the art will better understand the technical solutions of the present invention, the following description of the preferred embodiments of the present invention is provided in connection with specific examples, which should not be construed as limiting the present patent.
The test methods or test methods described in the following examples are conventional methods unless otherwise specified; the reagents and materials, unless otherwise indicated, are conventionally obtained commercially or prepared by conventional methods.
Example 1:
an electrochemical corrosion process for the production of medium and high voltage anode foils comprising the steps of:
A. pretreatment:
putting the aluminum foil into a mixed solution of sodium hydroxide and potassium hydroxide at the temperature of 35-45 ℃, soaking for 40-60 s, and then washing for 2-5 times by using deionized water; the molar concentrations of the sodium hydroxide and the potassium hydroxide in the mixed solution of the sodium hydroxide and the potassium hydroxide are 0.06-0.08 mol/L and 0.02-0.03 mol/L respectively;
B. and (3) punching:
placing the pretreated aluminum foil into a mixed solution containing 10-15% by mass of hydrochloric acid and 35-45% by mass of sulfuric acid at the temperature of 65-75 ℃, controlling the corrosion current density to be 250-400 mA/cm2, and performing perforation corrosion for 100-120 s;
C. reaming:
washing the aluminum foil subjected to hole forming with deionized water, putting the aluminum foil into a nitric acid solution with the temperature of 80-90 ℃ and the mass percent of 11-15%, controlling the hole expanding current to be 50-150 mA/cm2, and expanding the hole for 9-12 min;
D. and (3) post-treatment:
cleaning the aluminum foil after hole expansion by using deionized water, and soaking the aluminum foil in a nitric acid solution with the temperature of 70-80 ℃ and the mass percent of 3-5% for 2-3 min;
E. and (3) drying:
and (3) cleaning the post-treated aluminum foil with deionized water, putting the aluminum foil into drying equipment, controlling the temperature to be 70-90 ℃, and drying for 2-5 hours to obtain the medium-high voltage anode foil.
Example 2:
an electrochemical corrosion process for the production of medium and high voltage anode foils comprising the steps of:
A. pretreatment:
putting the aluminum foil into a mixed solution of sodium hydroxide and potassium hydroxide at the temperature of 35 ℃, soaking for 60s, and then washing for 2 times by using deionized water; the molar concentrations of the sodium hydroxide and the potassium hydroxide in the mixed solution of the sodium hydroxide and the potassium hydroxide are 0.08mol/L and 0.02mol/L respectively;
B. and (3) punching:
placing the pretreated aluminum foil into a mixed solution containing 15% by mass of hydrochloric acid and 35% by mass of sulfuric acid at the temperature of 65 ℃, controlling the corrosion current density to be 400mA/cm2, and performing perforation corrosion for 120 s;
C. reaming:
washing the aluminum foil subjected to hole forming with deionized water, putting into a nitric acid solution with the temperature of 80 ℃ and the mass percent of 15%, controlling the hole-expanding current to be 150mA/cm2, and expanding the hole for 12 min;
D. and (3) post-treatment:
cleaning the aluminum foil after hole expansion with deionized water, and soaking in a nitric acid solution with the temperature of 70 ℃ and the mass percent of 5% for 3 min;
E. and (3) drying:
and (3) cleaning the post-treated aluminum foil with deionized water, putting the aluminum foil into drying equipment, controlling the temperature to be 70 ℃, and drying for 5 hours to obtain the medium-high voltage anode foil.
In this embodiment, in the step a, the aluminum foil is an aluminum foil for an electrolytic capacitor anode with an aluminum content of not less than 99.99% and a thickness of 120 um.
In this embodiment, in step B, the mixed solution containing 15% by mass of hydrochloric acid and 35% by mass of sulfuric acid further contains 0.35% by mass of zinc nitrite.
In this embodiment, in the step B, the mixed solution containing 15% by mass of hydrochloric acid and 35% by mass of sulfuric acid further contains 0.5% by mass of isopropyl alcohol.
In this embodiment, in step C, the nitric acid solution with a mass percentage of 15% further contains zinc nitrite with a mass percentage of 0.65%.
In this embodiment, in step C, the nitric acid solution with a mass percentage of 15% further contains 0.15% by mass of toluenesulfonic acid.
In this embodiment, in step E, the drying device is an oven.
Through tests, the 520Vt specific volume of the medium-high voltage anode foil prepared by the electrochemical corrosion process for producing the medium-high voltage anode foil is 0.62uF/cm2, the strength (bending times are 134 times), the foil surface quality is stable, and the high-voltage anode foil has the performance of both high specific volume and high strength (bending times are high).
Example 3:
an electrochemical corrosion process for the production of medium and high voltage anode foils comprising the steps of:
A. pretreatment:
putting the aluminum foil into a mixed solution of sodium hydroxide and potassium hydroxide at the temperature of 45 ℃, soaking for 40s, and then washing for 5 times by using deionized water; the molar concentrations of the sodium hydroxide and the potassium hydroxide in the mixed solution of the sodium hydroxide and the potassium hydroxide are 0.06mol/L and 0.03mol/L respectively;
B. and (3) punching:
placing the pretreated aluminum foil into a mixed solution containing 10 mass percent of hydrochloric acid and 45 mass percent of sulfuric acid at the temperature of 75 ℃, controlling the corrosion current density to be 250mA/cm2, and carrying out perforation corrosion for 100 s;
C. reaming:
washing the aluminum foil subjected to hole forming with deionized water, putting into a nitric acid solution with the temperature of 90 ℃ and the mass percent of 11%, controlling the hole-expanding current to be 50mA/cm2, and expanding the hole for 9 min;
D. and (3) post-treatment:
cleaning the aluminum foil after hole expansion with deionized water, and soaking in a nitric acid solution with the temperature of 80 ℃ and the mass percent of 3% for 2 min;
E. and (3) drying:
and (3) cleaning the post-treated aluminum foil with deionized water, putting the aluminum foil into drying equipment, controlling the temperature to be 90 ℃, and drying for 2h to obtain the medium-high voltage anode foil.
In this embodiment, in the step a, the aluminum foil is an aluminum foil for an electrolytic capacitor anode with an aluminum content of not less than 99.99% and a thickness of 120 um.
In this embodiment, in step B, the mixed solution containing 10% by mass of hydrochloric acid and 45% by mass of sulfuric acid further contains 0.45% by mass of zinc nitrite.
In this embodiment, in the step B, the mixed solution containing 10% by mass of hydrochloric acid and 45% by mass of sulfuric acid further contains 0.7% by mass of isopropyl alcohol.
In this embodiment, in step C, the 11% by mass nitric acid solution further contains 0.85% by mass zinc nitrite.
In this embodiment, in step C, the 11% by mass nitric acid solution further contains 0.25% by mass toluenesulfonic acid.
In this embodiment, in step E, the drying device is an oven.
Through tests, the 520Vt specific volume of the medium-high voltage anode foil prepared by the electrochemical corrosion process for producing the medium-high voltage anode foil is 0.65uF/cm2, the strength (bending times of 136 times) is high, the foil surface quality is stable, and the high-voltage anode foil has the performance of both high specific volume and high strength (bending times of high).
Example 4:
an electrochemical corrosion process for the production of medium and high voltage anode foils comprising the steps of:
A. pre-treating;
B. hair holes;
C. reaming;
D. and (3) post-treatment:
cleaning the aluminum foil after hole expansion with deionized water, and soaking in a nitric acid solution with the temperature of 75 ℃ and the mass percent of 4.5% for 2.5 min;
E. and (3) drying:
and (3) cleaning the post-treated aluminum foil with deionized water, putting the aluminum foil into drying equipment, controlling the temperature to be 80 ℃, and drying for 3 hours to obtain the medium-high voltage anode foil.
In this embodiment, in the step a, the aluminum foil is an aluminum foil for an electrolytic capacitor anode with an aluminum content of not less than 99.99% and a thickness of 120 um.
In this embodiment, in step a, the pretreatment: putting the aluminum foil into a mixed solution of sodium hydroxide and potassium hydroxide at the temperature of 40 ℃, soaking for 55s, and then washing for 3 times by using deionized water; the molar concentrations of the sodium hydroxide and the potassium hydroxide in the mixed solution of the sodium hydroxide and the potassium hydroxide are 0.07mol/L and 0.024mol/L respectively;
in this embodiment, in step B, the perforation: placing the pretreated aluminum foil into a mixed solution containing 12.5 mass percent of hydrochloric acid and 42 mass percent of sulfuric acid at the temperature of 68 ℃, controlling the corrosion current density to be 280mA/cm2, and performing perforation corrosion for 110 s; the mixed solution containing 12.5 percent by mass of hydrochloric acid and 42 percent by mass of sulfuric acid also contains 0.41 percent by mass of zinc nitrite; the mixed solution containing 12.5% by mass of hydrochloric acid and 42% by mass of sulfuric acid also contains 0.65% by mass of isopropanol.
In this embodiment, in step C, hole expansion: washing the aluminum foil subjected to hole forming with deionized water, putting into a nitric acid solution with the temperature of 82 ℃ and the mass percent of 13%, controlling the hole-expanding current to be 75mA/cm2, and expanding the hole for 11 min; the nitric acid solution with the mass percentage of 13 percent also contains zinc nitrite with the mass percentage of 0.75 percent; the nitric acid solution with the mass percent of 13% also contains 0.18% of toluenesulfonic acid with the mass percent.
In this embodiment, in step E, the drying device is an oven.
Through tests, the 520Vt specific volume of the medium-high voltage anode foil prepared by the electrochemical corrosion process for producing the medium-high voltage anode foil is 0.68uF/cm2, the strength (bending times are 145 times), the foil surface quality is stable, and the high-voltage anode foil has the performance of both high specific volume and high strength (bending times are high).
The above is only a preferred embodiment of the present invention, and it should be noted that the above preferred embodiment should not be considered as limiting the present invention, and the protection scope of the present invention should be subject to the scope defined by the claims. It will be apparent to those skilled in the art that various modifications and adaptations can be made without departing from the spirit and scope of the invention, and these modifications and adaptations should be considered within the scope of the invention.
Claims (10)
1. An electrochemical corrosion process for the production of medium and high voltage anode foils, characterized by comprising the following steps:
A. pretreatment:
putting the aluminum foil into a mixed solution of sodium hydroxide and potassium hydroxide at the temperature of 35-45 ℃, soaking for 40-60 s, and then washing for 2-5 times by using deionized water; the molar concentrations of the sodium hydroxide and the potassium hydroxide in the mixed solution of the sodium hydroxide and the potassium hydroxide are 0.06-0.08 mol/L and 0.02-0.03 mol/L respectively;
B. and (3) punching:
placing the pretreated aluminum foil into a mixed solution containing 10-15% by mass of hydrochloric acid and 35-45% by mass of sulfuric acid at the temperature of 65-75 ℃, controlling the corrosion current density to be 250-400 mA/cm2, and performing perforation corrosion for 100-120 s;
C. reaming:
washing the aluminum foil subjected to hole forming with deionized water, putting the aluminum foil into a nitric acid solution with the temperature of 80-90 ℃ and the mass percent of 11-15%, controlling the hole expanding current to be 50-150 mA/cm2, and expanding the hole for 9-12 min;
D. and (3) post-treatment:
cleaning the aluminum foil after hole expansion by using deionized water, and soaking the aluminum foil in a nitric acid solution with the temperature of 70-80 ℃ and the mass percent of 3-5% for 2-3 min;
E. and (3) drying:
and (3) cleaning the post-treated aluminum foil with deionized water, putting the aluminum foil into drying equipment, controlling the temperature to be 70-90 ℃, and drying for 2-5 hours to obtain the medium-high voltage anode foil.
2. The electrochemical corrosion process for producing the medium-high voltage anode foil according to claim 1, wherein in the step A, the aluminum foil is an aluminum foil for an electrolytic capacitor anode with an aluminum content of not less than 99.99% and a thickness of 120 um.
3. The electrochemical corrosion process for producing the medium-high voltage anode foil according to claim 1, wherein in the step B, the mixed solution containing 10-15% by mass of hydrochloric acid and 35-45% by mass of sulfuric acid further contains 0.35-0.45% by mass of zinc nitrite.
4. The electrochemical corrosion process for producing the medium-high voltage anode foil as claimed in claim 1, wherein in the step B, the mixed solution containing 10-15% by mass of hydrochloric acid and 35-45% by mass of sulfuric acid further contains 0.5-0.7% by mass of isopropanol.
5. The electrochemical corrosion process for producing the medium-high voltage anode foil according to claim 1, wherein in the step C, the nitric acid solution with the mass percentage of 11-15% further contains 0.65-0.85% of zinc nitrite.
6. The electrochemical corrosion process for producing the medium-high voltage anode foil according to claim 1, wherein in the step C, the nitric acid solution with the mass percentage of 11-15% further contains 0.15-0.25% of toluenesulfonic acid with mass percentage.
7. The electrochemical corrosion process for the production of medium-high voltage anode foils according to claim 1, characterized in that in step a, the pretreatment: putting the aluminum foil into a mixed solution of sodium hydroxide and potassium hydroxide at the temperature of 40 ℃, soaking for 55s, and then washing for 3 times by using deionized water; the molar concentrations of the sodium hydroxide and the potassium hydroxide in the mixed solution of the sodium hydroxide and the potassium hydroxide are 0.07mol/L and 0.024mol/L respectively.
8. Electrochemical corrosion process for the production of medium-high voltage anode foils according to claim 1, characterized in that in step B, the ratio of open porosity: placing the pretreated aluminum foil into a mixed solution containing 12.5 mass percent of hydrochloric acid and 42 mass percent of sulfuric acid at the temperature of 68 ℃, controlling the corrosion current density to be 280mA/cm2, and performing perforation corrosion for 110 s; the mixed solution containing 12.5 percent by mass of hydrochloric acid and 42 percent by mass of sulfuric acid also contains 0.41 percent by mass of zinc nitrite; the mixed solution containing 12.5% by mass of hydrochloric acid and 42% by mass of sulfuric acid also contains 0.65% by mass of isopropanol.
9. Electrochemical corrosion process for the production of medium and high voltage anode foils according to claim 1, characterized in that in step C, the hole expansion: washing the aluminum foil subjected to hole forming with deionized water, putting into a nitric acid solution with the temperature of 82 ℃ and the mass percent of 13%, controlling the hole-expanding current to be 75mA/cm2, and expanding the hole for 11 min; the nitric acid solution with the mass percentage of 13 percent also contains zinc nitrite with the mass percentage of 0.75 percent; the nitric acid solution with the mass percent of 13% also contains 0.18% of toluenesulfonic acid with the mass percent.
10. The electrochemical corrosion process for the production of middle and high voltage anode foils according to claim 1, characterized in that in step E, the drying apparatus is an oven.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910293767.0A CN110164696B (en) | 2019-04-12 | 2019-04-12 | Electrochemical corrosion process for producing medium-high voltage anode foil |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910293767.0A CN110164696B (en) | 2019-04-12 | 2019-04-12 | Electrochemical corrosion process for producing medium-high voltage anode foil |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN110164696A CN110164696A (en) | 2019-08-23 |
| CN110164696B true CN110164696B (en) | 2021-06-22 |
Family
ID=67639115
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201910293767.0A Active CN110164696B (en) | 2019-04-12 | 2019-04-12 | Electrochemical corrosion process for producing medium-high voltage anode foil |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN110164696B (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111472039A (en) * | 2020-03-27 | 2020-07-31 | 东莞东阳光科研发有限公司 | Preparation method of middle-high voltage electrode foil for aluminum electrolytic capacitor |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1458658A (en) * | 2003-05-26 | 2003-11-26 | 深圳市东阳光化成箔股份有限公司乳源分公司 | Anode aluminium foil etching process for electrolytic capacitor |
| CN101425392A (en) * | 2008-07-29 | 2009-05-06 | 东莞市东阳光电容器有限公司 | Pre-treating process for high-voltage aluminum foil corrosion |
| CN102094231A (en) * | 2011-01-11 | 2011-06-15 | 江苏立富电极箔有限公司 | Process for corroding anode foil for intermediate and high voltage aluminum electrolytic capacitor |
| CN105420803A (en) * | 2015-11-27 | 2016-03-23 | 广西贺州市桂东电子科技有限责任公司 | Method for ultrasonic-assisted corrosion of middle-high voltage anode aluminum foil |
| CN108538600A (en) * | 2018-05-10 | 2018-09-14 | 广西贺州市桂东电子科技有限责任公司 | A kind of aluminium electroloysis mesohigh anode foils nitration mixture reaming caustic solution |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US10718059B2 (en) * | 2017-07-10 | 2020-07-21 | Rohm And Haas Electronic Materials Llc | Nickel electroplating compositions with cationic polymers and methods of electroplating nickel |
-
2019
- 2019-04-12 CN CN201910293767.0A patent/CN110164696B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1458658A (en) * | 2003-05-26 | 2003-11-26 | 深圳市东阳光化成箔股份有限公司乳源分公司 | Anode aluminium foil etching process for electrolytic capacitor |
| CN101425392A (en) * | 2008-07-29 | 2009-05-06 | 东莞市东阳光电容器有限公司 | Pre-treating process for high-voltage aluminum foil corrosion |
| CN102094231A (en) * | 2011-01-11 | 2011-06-15 | 江苏立富电极箔有限公司 | Process for corroding anode foil for intermediate and high voltage aluminum electrolytic capacitor |
| CN105420803A (en) * | 2015-11-27 | 2016-03-23 | 广西贺州市桂东电子科技有限责任公司 | Method for ultrasonic-assisted corrosion of middle-high voltage anode aluminum foil |
| CN108538600A (en) * | 2018-05-10 | 2018-09-14 | 广西贺州市桂东电子科技有限责任公司 | A kind of aluminium electroloysis mesohigh anode foils nitration mixture reaming caustic solution |
Also Published As
| Publication number | Publication date |
|---|---|
| CN110164696A (en) | 2019-08-23 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN111146005B (en) | Sintered low-voltage anode foil of aluminum electrolytic capacitor and preparation method thereof | |
| CN110993347B (en) | High-voltage anode foil of sintered aluminum electrolytic capacitor and preparation method thereof | |
| CN105097286B (en) | A kind of caustic solution of super-pressure energy storage material | |
| CN100587126C (en) | Method for erosion of supervoltage high specific volume anode foil | |
| CN110993348B (en) | Sintered aluminum electrolytic capacitor ultrahigh-voltage anode foil and preparation method thereof | |
| WO2019166034A1 (en) | Anode foil etching process for aluminium electrolytic capacitor | |
| CN103366964B (en) | Be applicable to the manufacture method of the low pressure formed aluminum foil of low impedance at high frequency electrolytic capacitor aqueous electrolyte | |
| CN112117128B (en) | High-specific-volume and high-strength medium-high voltage corrosion electrode foil and preparation method and application thereof | |
| CN113628888B (en) | Preparation method of corrosion aluminum foil with high consistency of hole length | |
| CN107313108A (en) | A kind of aluminium electrolutic capacitor high voltage ultra-thin electrode foil and preparation method thereof | |
| CN110164696B (en) | Electrochemical corrosion process for producing medium-high voltage anode foil | |
| CN112899766A (en) | Manufacturing method of medium-pressure corrosion foil | |
| CN112853456B (en) | Method for manufacturing high-pressure high-specific-volume corrosion foil | |
| CN1117182C (en) | Three-stage manufacturing method of electrode foil for medium-high voltage aluminum electrolytic capacitor | |
| CN115172054B (en) | Medium-high voltage anodic oxidation pretreatment method, aluminum foil and aluminum electrolytic capacitor | |
| CN103151174B (en) | The manufacture method of electrode foil of high-pressure aluminum electrolytic capacitor | |
| CN104630871B (en) | A kind of etching process method of low pressure hard Fabrication of High Specific Capacitance aluminum electric pole foil | |
| CN101154508B (en) | Four-stage manufacturing method for electrode foil of high-pressure aluminum electrolytic capacitor | |
| JP2009146984A (en) | Method of manufacturing electrode foil for electrolytic capacitor | |
| CN114808076A (en) | Preparation method of electrode foil with good bending performance | |
| CN103714974A (en) | Method for preparing aluminum electrolytic capacitor anode material | |
| CN103489657A (en) | Preparation method of high-conductivity polymer electrolytic capacitor | |
| CN112941592A (en) | Low-voltage formed foil production process for aluminum electrolytic capacitor | |
| JP4690171B2 (en) | Method for producing aluminum electrode foil for electrolytic capacitor | |
| CN103500657A (en) | Method for reducing volume of tantalum capacitor |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| CB02 | Change of applicant information | ||
| CB02 | Change of applicant information |
Address after: 314000 south head of FENGCHUAN Road, Xinfeng Town, Nanhu District, Jiaxing City, Zhejiang Province Applicant after: Zhejiang FengChuan electronic environmental protection technology Co.,Ltd. Address before: 314000 south head of FENGCHUAN Road, Xinfeng Town, Nanhu District, Jiaxing City, Zhejiang Province Applicant before: ZHEJIANG FENGCHUAN ELECTRONIC TECHNOLOGY Co.,Ltd. |
|
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| PE01 | Entry into force of the registration of the contract for pledge of patent right | ||
| PE01 | Entry into force of the registration of the contract for pledge of patent right |
Denomination of invention: An electrochemical corrosion process for the production of medium and high voltage anode foils Granted publication date: 20210622 Pledgee: Zhejiang Hecheng Rural Commercial Bank Co.,Ltd. Pledgor: Zhejiang FengChuan electronic environmental protection technology Co.,Ltd. Registration number: Y2024990000007 |