CN112863880A - Process method for medium-high voltage anode aluminum foil corrosion reaming - Google Patents

Process method for medium-high voltage anode aluminum foil corrosion reaming Download PDF

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CN112863880A
CN112863880A CN202110087548.4A CN202110087548A CN112863880A CN 112863880 A CN112863880 A CN 112863880A CN 202110087548 A CN202110087548 A CN 202110087548A CN 112863880 A CN112863880 A CN 112863880A
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aluminum foil
corrosion
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reaming
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CN112863880B (en
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杨小飞
蒋碧君
梁力勃
蔡小宇
熊传勇
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GUANGXI HEZHOU GUIDONG ELECTRONIC TECHNOLOGY CO LTD
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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
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    • H01G9/04—Electrodes or formation of dielectric layers thereon
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Abstract

The invention discloses a process method for medium-high voltage anode aluminum foil corrosion reaming, which comprises the steps of pretreatment, first-level pore-forming corrosion, second-level pore-forming corrosion, third-level pore-forming corrosion, post-treatment and the like. The method has simple process, not only can effectively improve the efficiency of corrosion reaming, but also can reduce the generation of wastewater containing ammonia, nitrogen and phosphorus.

Description

Process method for medium-high voltage anode aluminum foil corrosion reaming
Technical Field
The invention belongs to the technical field of electrode foil production, and particularly relates to a process method for medium-high voltage anode aluminum foil corrosion reaming.
Background
The aluminum electrolytic capacitor is an energy storage component widely applied in the electronic and electrical industry, and the anode foil for the aluminum electrolytic capacitor is an energy storage raw material. With the rapid development of electronic information technology, the trend of miniaturization and large-capacity capacitors is more and more obvious, and the attention to green and environmental protection of products is more and more paid, so that the requirement of higher environmental protection is put forward in the pursuit of improving the capacity of the high-voltage anode aluminum foil.
At present, the electrolytic corrosion process of the medium-high voltage anode aluminum foil generally comprises four main steps of pretreatment, holing corrosion, reaming corrosion, post-treatment and the like. The key for obtaining high specific capacitance is that tunnel holes with high density, proper pore size distribution and regular hole length are uniformly distributed on the surface of the medium and high anode pressure aluminum foil. The pretreatment has the effects of removing oil stains, impurities and oxidation films on the surface of the plain foil, improving the surface state and promoting the formation of ordered initial tunnel holes when the aluminum foil is subjected to hole corrosion in the next step. The function of the pitting corrosion is to form initial tunnel holes with a certain number, length and aperture on the surface of the aluminum foil by applying direct current. The reaming corrosion has the effect of further electrifying corrosion or chemical corrosion on the basis of the initial tunnel hole, so that the hole diameter of the tunnel hole is further enlarged and reaches the designed size. The post-treatment is used for eliminating residual metal impurities and aluminum powder on the surface of the aluminum foil and chloride ions in the tunnel holes.
With the development of society, the industry pursues high-performance electrode aluminum foil and simultaneously increases the protection to the environment. The existing nitric acid reaming system has the treatment problems of ammonia nitrogen and phosphorus in the wastewater treatment process. Compared with a nitric acid reaming process, the hydrochloric acid reaming process has the problem of low performance and efficiency although the ammonia nitrogen treatment problem does not exist; the pure chemical reaming process has significant advantages in terms of cost, but has the disadvantages of low performance and efficiency, deviation in stability and the like.
Disclosure of Invention
Aiming at the defects, the invention discloses a medium-high voltage anodic aluminum foil corrosion reaming process method, which not only improves the corrosion reaming efficiency, but also reduces the generation of wastewater containing ammonia nitrogen and phosphorus.
The invention is realized by adopting the following technical scheme:
a process method for medium-high voltage anode aluminum foil corrosion reaming comprises the following steps:
(1) pretreatment: soaking an aluminum foil in a solution A, wherein the solution A contains the following components in percentage by mass: 1-10% hydrochloric acid and 10-40% sulfuric acid; in the pretreatment, the soaking time is 50-200 s;
(2) primary pitting corrosion: washing the aluminum foil treated in the step (1) with water, and then putting the aluminum foil into a solution B for primary direct-current pore-forming corrosion, wherein the solution B comprises the following components in percentage by mass: 1-10% hydrochloric acid and 10-40% sulfuric acid; in the primary direct current perforation corrosion, the applied current density is 200-800 mA/cm2The time for applying the current is 50-120 s;
(3) secondary reaming corrosion: washing the aluminum foil treated in the step (2) with water, and then putting the aluminum foil into a solution C for secondary pure chemical reaming corrosion, wherein the solution C is a hydrochloric acid solution with the mass percent of 1-10%; in the secondary reaming corrosion, the soaking time is 200-500 s, and the reaming corrosion weight loss control range is 8-15%;
(4) and (3) three-stage reaming corrosion: washing the aluminum foil treated in the step (3) with water, and then carrying out three-stage direct current electric reaming corrosion in a nitric acid solution or a hydrochloric acid solution, wherein the reaming corrosion weight loss control range is 8-15%; the three-stage DC electric reaming corrosion in the nitric acid solution is carried out by putting the aluminum foil in the nitric acid solution with the mass percent of 1-10% and the temperature of 60-90 ℃, and the density of applied current is 50-200 mA/cm2The time for applying the current is 200-500 s; the three-stage DC electric reaming corrosion in the hydrochloric acid solution is carried out by putting the aluminum foil in the hydrochloric acid solution with the mass percent of 1-10% and the temperature of 60-90 ℃, and the density of the applied current is 7-45 mA/cm2The time for applying the current is 200-500 s;
(5) and (3) post-treatment: washing the aluminum foil treated in the step (4) with water, and then soaking the aluminum foil in a nitric acid solution with the temperature of 50-70 ℃ and the mass percent of 1-10% for 50-200 s;
(6) and (4) cleaning the aluminum foil treated in the step (5) by using tap water, then cleaning the aluminum foil by using pure water, drying and winding to obtain the etched foil.
Further, the temperature of the solution A in the step (1) is 50-90 ℃.
Further, the temperature of the solution B in the step (2) is 65-85 ℃.
Further, the temperature of the solution C in the step (3) is 70-90 ℃.
Further, in the step (4), the nitric acid solution or hydrochloric acid solution contains a corrosion inhibitor with a mass percentage of 0.1-0.3%, and the corrosion inhibitor is a tannic acid microcapsule and is prepared according to the following steps:
s1, mixing fatty acid methyl ester and span 80 uniformly, adding tannic acid solution with the mass fraction of 60%, and stirring uniformly to obtain emulsion;
s2, mixing furfuryl alcohol and fatty acid methyl ester uniformly, adding the emulsion obtained in the step S1, stirring and reacting for 60min to obtain a microcapsule suspension, and then performing centrifugal separation, washing and drying on the microcapsule suspension to obtain the powdery tannin microcapsule.
According to the invention, the tannic acid microcapsule is added as a corrosion inhibitor in the three-stage reaming corrosion, the tannic acid is slowly released in the three-stage reaming corrosion process, and the tannic acid is utilized to improve the corrosion and pore cluster merging phenomenon on the surface of the aluminum foil, so that the effective specific surface area of the corroded foil is increased, and the specific capacitance is improved; meanwhile, the pore density of the expanded pore foil is increased along with the increase of the concentration of the corrosion inhibitor, so that the average pore diameter is reduced, if the diameter of the expanded pore foil is too small, a small tunnel pore is easy to block in the high-pressure formation process, the specific surface area of the formed foil cannot be effectively improved, the tannin microcapsules are slowly dissolved to release tannin, so that the tannin concentration is gradually increased, the tannin concentration is controlled at the early stage of expansion, the condition that the pore diameter of the expanded pore foil is too small is avoided, then the tannin concentration is gradually increased at the middle and later stages of expansion, the corrosion inhibition effect of the tannin is improved, the corrosion of the corrosion liquid and the current to the aluminum foil surface and the tunnel pore diameter part is weakened, the corrosion to the bottom of the tunnel pore is strengthened, and the pore cluster phenomenon is weakened.
Further, in step S1, the fatty acid methyl ester and span 80 are mixed according to the mass ratio of 100:1, and the ratio of the addition volume of the tannic acid solution to the volume of the fatty acid methyl ester is 1: 6.
Further, in step S2, the furfuryl alcohol and the fatty acid methyl ester are mixed in a mass ratio of 2:100, and the ratio of the added volume of the emulsion to the volume of the mixed solution of the furfuryl alcohol and the fatty acid methyl ester is 2: 1.
Compared with the prior art, the technical scheme has the following beneficial effects:
1. the method has simple process and strong controllability, and the method combines pure chemical reaming and power-on reaming, namely, hydrochloric acid is firstly used for pure chemical reaming, then nitric acid or hydrochloric acid is used for power-on reaming, and the corrosion weight loss ratio is controlled by adjusting the process parameters of the solution temperature, the density and time of applied current, the soaking treatment time and the like of each step, so that not only can high-performance and high-quality corrosion foil be obtained, but also the raw material cost, the equipment investment and the maintenance cost are greatly reduced.
2. The invention adopts the tannic acid microcapsule as the corrosion inhibitor, which not only can improve the corrosion and the pore cluster combination phenomenon on the surface of the aluminum foil, increase the effective specific surface area of the corroded foil and improve the specific capacitance, but also has low toxicity and little environmental pollution compared with other chemical corrosion inhibitors.
Detailed Description
The invention is further illustrated by the following examples, which are not to be construed as limiting the invention thereto. The specific experimental conditions and methods not indicated in the following examples are generally conventional means well known to those skilled in the art.
Example 1:
a process method for medium-high voltage anode aluminum foil corrosion reaming comprises the following steps:
(1) pretreatment: soaking an aluminum foil in a solution A, wherein the solution A contains the following components in percentage by mass: 2% hydrochloric acid and 30% sulfuric acid; in the pretreatment, the soaking time is 150s, and the temperature of the solution A is 60 ℃;
(2) first-class hairAnd (3) hole corrosion: washing the aluminum foil treated in the step (1) with water, and then putting the aluminum foil into a solution B for primary direct-current pore-forming corrosion, wherein the solution B comprises the following components in percentage by mass: 3% hydrochloric acid, 35% sulfuric acid; in the first-stage direct-current hair hole corrosion, the applied current density is 300mA/cm2The time for applying the current is 80s, and the temperature of the solution B is 70 ℃;
(3) secondary reaming corrosion: washing the aluminum foil treated in the step (2) with water, and then putting the aluminum foil into a solution C for secondary pure chemical reaming corrosion, wherein the solution C is a hydrochloric acid solution with the mass percent of 2.5%; in the secondary reaming corrosion, the soaking time is 300s, the reaming corrosion weight loss control range is 8%, and the temperature of the solution C is 85 ℃;
(4) and (3) three-stage reaming corrosion: washing the aluminum foil treated in the step (3) with water, and then carrying out three-stage direct current electric reaming corrosion in a hydrochloric acid solution, wherein the reaming corrosion weight loss control range is 12%; the three-stage DC electric reaming corrosion in hydrochloric acid solution is carried out by putting the aluminum foil in 2.5% by mass of hydrochloric acid solution at 80 ℃ and applying electric current with the density of 20mA/cm2The time for applying the current is 400 s;
the corrosion inhibitor in the hydrochloric acid solution is 0.2% in mass percentage, is a tannic acid microcapsule and is prepared according to the following steps:
s1, uniformly mixing fatty acid methyl ester and span 80 according to the mass ratio of 100:1, adding a tannic acid solution with the mass fraction of 60%, and uniformly stirring to obtain an emulsion, wherein the ratio of the addition volume of the tannic acid solution to the volume of the fatty acid methyl ester is 1: 6;
s2, mixing furfuryl alcohol and fatty acid methyl ester uniformly according to the mass ratio of 2:100, adding the emulsion obtained in the step S1, stirring and reacting for 60min to obtain microcapsule suspension, and performing centrifugal separation, washing and drying on the microcapsule suspension to obtain powdery tannin microcapsules, wherein the ratio of the adding volume of the emulsion to the volume of the mixed solution of the furfuryl alcohol and the fatty acid methyl ester is 2: 1;
(5) and (3) post-treatment: washing the aluminum foil treated in the step (4) with water, and then soaking the aluminum foil in a nitric acid solution with the temperature of 60 ℃ and the mass percent of 2.5%, wherein the soaking time is 100 s;
(6) and (4) cleaning the aluminum foil treated in the step (5) by using tap water, then cleaning the aluminum foil by using pure water, drying and winding to obtain the etched foil.
Example 2:
a process method for medium-high voltage anode aluminum foil corrosion reaming comprises the following steps:
(1) pretreatment: soaking an aluminum foil in a solution A, wherein the solution A contains the following components in percentage by mass: 2.5% hydrochloric acid, 15% sulfuric acid; in the pretreatment, the soaking time is 150s, and the temperature of the solution A is 60 ℃;
(2) primary pitting corrosion: washing the aluminum foil treated in the step (1) with water, and then putting the aluminum foil into a solution B for primary direct-current pore-forming corrosion, wherein the solution B comprises the following components in percentage by mass: 4% hydrochloric acid, 25% sulfuric acid; in the first-stage direct-current hair hole corrosion, the applied current density is 300mA/cm2The time for applying the current is 80s, and the temperature of the solution B is 70 ℃;
(3) secondary reaming corrosion: washing the aluminum foil treated in the step (2) with water, and then putting the aluminum foil into a solution C for secondary pure chemical reaming corrosion, wherein the solution C is a hydrochloric acid solution with the mass percent of 2.5%; in the secondary reaming corrosion, the soaking time is 400s, the reaming corrosion weight loss control range is 10%, and the temperature of the solution C is 85 ℃;
(4) and (3) three-stage reaming corrosion: washing the aluminum foil treated in the step (3) with water, and then carrying out three-stage direct current electric reaming corrosion in a nitric acid solution, wherein the reaming corrosion weight loss control range is 12%; the three-stage DC electric reaming corrosion in the nitric acid solution is carried out by putting the aluminum foil in the nitric acid solution with the mass percentage of 3% and the temperature of 70 ℃, and the density of the applied electric current is 100mA/cm2The time for applying the current is 350 s;
the corrosion inhibitor with the mass percentage of 0.1% in the nitric acid solution is a tannic acid microcapsule and is prepared by the following steps:
s1, uniformly mixing fatty acid methyl ester and span 80 according to the mass ratio of 100:1, adding a tannic acid solution with the mass fraction of 60%, and uniformly stirring to obtain an emulsion, wherein the ratio of the addition volume of the tannic acid solution to the volume of the fatty acid methyl ester is 1: 6;
s2, mixing furfuryl alcohol and fatty acid methyl ester uniformly according to the mass ratio of 2:100, adding the emulsion obtained in the step S1, stirring and reacting for 60min to obtain microcapsule suspension, and performing centrifugal separation, washing and drying on the microcapsule suspension to obtain powdery tannin microcapsules, wherein the ratio of the adding volume of the emulsion to the volume of the mixed solution of the furfuryl alcohol and the fatty acid methyl ester is 2: 1;
(5) and (3) post-treatment: washing the aluminum foil treated in the step (4) with water, and then soaking the aluminum foil in a nitric acid solution with the temperature of 60 ℃ and the mass percent of 2.5%, wherein the soaking time is 100 s;
(6) and (4) cleaning the aluminum foil treated in the step (5) by using tap water, then cleaning the aluminum foil by using pure water, drying and winding to obtain the etched foil.
Example 3:
a process method for medium-high voltage anode aluminum foil corrosion reaming comprises the following steps:
(1) pretreatment: soaking an aluminum foil in a solution A, wherein the solution A contains the following components in percentage by mass: 2.5% hydrochloric acid, 25% sulfuric acid; in the pretreatment, the soaking time is 100s, and the temperature of the solution A is 55 ℃;
(2) primary pitting corrosion: washing the aluminum foil treated in the step (1) with water, and then putting the aluminum foil into a solution B for primary direct-current pore-forming corrosion, wherein the solution B comprises the following components in percentage by mass: 5% hydrochloric acid, 25% sulfuric acid; in the first-stage direct-current hair hole corrosion, the applied current density is 400mA/cm2The time of applying the current is 100s, and the temperature of the solution B is 75 ℃;
(3) secondary reaming corrosion: washing the aluminum foil treated in the step (2) with water, and then putting the aluminum foil into a solution C for secondary pure chemical reaming corrosion, wherein the solution C is a hydrochloric acid solution with the mass percent of 2.5%; in the secondary reaming corrosion, the soaking time is 500s, the reaming corrosion weight loss control range is 12%, and the temperature of the solution C is 85 ℃;
(4) and (3) three-stage reaming corrosion: washing the aluminum foil treated in the step (3) with water, and then carrying out three-stage direct current electric reaming corrosion in a hydrochloric acid solution, wherein the reaming corrosion weight loss control range is 12%; the three-stage DC electric reaming corrosion in hydrochloric acid solution is carried out by putting the aluminum foil in 2.5% by mass of hydrochloric acid solution at 80 ℃ and applying electric current with the density of 20mA/cm2The time for applying the current is 400 s;
the corrosion inhibitor in the hydrochloric acid solution is 0.3% by mass, is a tannic acid microcapsule and is prepared by the following steps:
s1, uniformly mixing fatty acid methyl ester and span 80 according to the mass ratio of 100:1, adding a tannic acid solution with the mass fraction of 60%, and uniformly stirring to obtain an emulsion, wherein the ratio of the addition volume of the tannic acid solution to the volume of the fatty acid methyl ester is 1: 6;
s2, mixing furfuryl alcohol and fatty acid methyl ester uniformly according to the mass ratio of 2:100, adding the emulsion obtained in the step S1, stirring and reacting for 60min to obtain microcapsule suspension, and performing centrifugal separation, washing and drying on the microcapsule suspension to obtain powdery tannin microcapsules, wherein the ratio of the adding volume of the emulsion to the volume of the mixed solution of the furfuryl alcohol and the fatty acid methyl ester is 2: 1;
(5) and (3) post-treatment: washing the aluminum foil treated in the step (4) with water, and then soaking the aluminum foil in a nitric acid solution with the temperature of 65 ℃ and the mass percent of 4% for 150 s;
(6) and (4) cleaning the aluminum foil treated in the step (5) by using tap water, then cleaning the aluminum foil by using pure water, drying and winding to obtain the etched foil.
Example 4:
a process method for medium-high voltage anode aluminum foil corrosion reaming comprises the following steps:
(1) pretreatment: soaking an aluminum foil in a solution A, wherein the solution A contains the following components in percentage by mass: 3% hydrochloric acid, 25% sulfuric acid; in the pretreatment, the soaking time is 120s, and the temperature of the solution A is 55 ℃;
(2) primary pitting corrosion: washing the aluminum foil treated in the step (1) with water, and then putting the aluminum foil into a solution B for primary direct-current pore-forming corrosion, wherein the solution B comprises the following components in percentage by mass: 6% hydrochloric acid, 20% sulfuric acid; in the first-stage direct-current hair hole corrosion, the applied current density is 400mA/cm2The time of applying the current is 100s, and the temperature of the solution B is 75 ℃;
(3) secondary reaming corrosion: washing the aluminum foil treated in the step (2) with water, and then putting the aluminum foil into a solution C for secondary pure chemical reaming corrosion, wherein the solution C is a hydrochloric acid solution with the mass percent of 2.5%; in the secondary reaming corrosion, the soaking time is 400s, the reaming corrosion weight loss control range is 9%, and the temperature of the solution C is 70 ℃;
(4) and (3) three-stage reaming corrosion: washing the aluminum foil treated in the step (3) with water, and then carrying out three-stage direct current electric reaming corrosion in a nitric acid solution, wherein the reaming corrosion weight loss control range is 10%; the three-stage DC electric reaming corrosion in the nitric acid solution is carried out by putting the aluminum foil in the nitric acid solution with the mass percentage of 3% and the temperature of 65 ℃, and the density of the applied electric current is 80mA/cm2The time for applying the current was 250 s;
the corrosion inhibitor with the mass percentage of 0.3% in the nitric acid solution is a tannic acid microcapsule and is prepared by the following steps:
s1, uniformly mixing fatty acid methyl ester and span 80 according to the mass ratio of 100:1, adding a tannic acid solution with the mass fraction of 60%, and uniformly stirring to obtain an emulsion, wherein the ratio of the addition volume of the tannic acid solution to the volume of the fatty acid methyl ester is 1: 6;
s2, mixing furfuryl alcohol and fatty acid methyl ester uniformly according to the mass ratio of 2:100, adding the emulsion obtained in the step S1, stirring and reacting for 60min to obtain microcapsule suspension, and performing centrifugal separation, washing and drying on the microcapsule suspension to obtain powdery tannin microcapsules, wherein the ratio of the adding volume of the emulsion to the volume of the mixed solution of the furfuryl alcohol and the fatty acid methyl ester is 2: 1;
(5) and (3) post-treatment: washing the aluminum foil treated in the step (4) with water, and then soaking the aluminum foil in a nitric acid solution with the temperature of 65 ℃ and the mass percent of 4% for 150 s;
(6) and (4) cleaning the aluminum foil treated in the step (5) by using tap water, then cleaning the aluminum foil by using pure water, drying and winding to obtain the etched foil.
Example 5:
a process method for medium-high voltage anode aluminum foil corrosion reaming comprises the following steps:
(1) pretreatment: soaking an aluminum foil in a solution A, wherein the solution A contains the following components in percentage by mass: 4% hydrochloric acid and 30% sulfuric acid; in the pretreatment, the soaking time is 150s, and the temperature of the solution A is 75 ℃;
(2) primary pitting corrosion: washing the aluminum foil treated in the step (1) with water, and then putting the aluminum foil into a solution B for primary direct-current pore-forming corrosion, wherein the solution B comprises the following components in percentage by mass: 7.5% hydrochloric acid, 20% sulfuric acid; in the first-stage direct-current hair hole corrosion, the applied current density is 450mA/cm2The time of applying the current is 60s, and the temperature of the solution B is 80 ℃;
(3) secondary reaming corrosion: washing the aluminum foil treated in the step (2) with water, and then putting the aluminum foil into a solution C for secondary pure chemical reaming corrosion, wherein the solution C is a hydrochloric acid solution with the mass percent of 2.5%; in the secondary reaming corrosion, the soaking time is 400s, the reaming corrosion weight loss control range is 11%, and the temperature of the solution C is 80 ℃;
(4) and (3) three-stage reaming corrosion: washing the aluminum foil treated in the step (3) with water, and then carrying out three-stage direct current electric reaming corrosion in a hydrochloric acid solution, wherein the reaming corrosion weight loss control range is 11%;the three-stage DC electric reaming corrosion in hydrochloric acid solution is carried out by putting aluminum foil in 3.5% by mass hydrochloric acid solution at 75 ℃ and applying electric current with density of 40mA/cm2The time for applying the current is 350 s;
the corrosion inhibitor in the hydrochloric acid solution is 0.1% by mass, is a tannic acid microcapsule and is prepared by the following steps:
s1, uniformly mixing fatty acid methyl ester and span 80 according to the mass ratio of 100:1, adding a tannic acid solution with the mass fraction of 60%, and uniformly stirring to obtain an emulsion, wherein the ratio of the addition volume of the tannic acid solution to the volume of the fatty acid methyl ester is 1: 6;
s2, mixing furfuryl alcohol and fatty acid methyl ester uniformly according to the mass ratio of 2:100, adding the emulsion obtained in the step S1, stirring and reacting for 60min to obtain microcapsule suspension, and performing centrifugal separation, washing and drying on the microcapsule suspension to obtain powdery tannin microcapsules, wherein the ratio of the adding volume of the emulsion to the volume of the mixed solution of the furfuryl alcohol and the fatty acid methyl ester is 2: 1;
(5) and (3) post-treatment: washing the aluminum foil treated in the step (4) with water, and then soaking in a nitric acid solution with the temperature of 55 ℃ and the mass percent of 7.5%, wherein the soaking time is 80 s;
(6) and (4) cleaning the aluminum foil treated in the step (5) by using tap water, then cleaning the aluminum foil by using pure water, drying and winding to obtain the etched foil.
Example 6:
a process method for medium-high voltage anode aluminum foil corrosion reaming comprises the following steps:
(1) pretreatment: soaking an aluminum foil in a solution A, wherein the solution A contains the following components in percentage by mass: 5% hydrochloric acid and 35% sulfuric acid; in the pretreatment, the soaking time is 80s, and the temperature of the solution A is 75 ℃;
(2) primary pitting corrosion: washing the aluminum foil treated in the step (1) with water, and then putting the aluminum foil into a solution B to perform primary direct-current pore-forming corrosion, wherein the solution B containsThe components by mass percent are as follows: 8% hydrochloric acid, 15% sulfuric acid; in the first-stage direct-current hair hole corrosion, the applied current density is 350mA/cm2The time of applying the current is 60s, and the temperature of the solution B is 805 ℃;
(3) secondary reaming corrosion: washing the aluminum foil treated in the step (2) with water, and then putting the aluminum foil into a solution C for secondary pure chemical reaming corrosion, wherein the solution C is a hydrochloric acid solution with the mass percent of 4%; in the secondary reaming corrosion, the soaking time is 400s, the reaming corrosion weight loss control range is 13%, and the temperature of the solution C is 90 ℃;
(4) and (3) three-stage reaming corrosion: washing the aluminum foil treated in the step (3) with water, and then carrying out three-stage direct current electric reaming corrosion in a nitric acid solution, wherein the reaming corrosion weight loss control range is 11%; the three-stage DC electric reaming corrosion in the nitric acid solution is carried out by putting the aluminum foil in the nitric acid solution with the mass percent of 2.5% and the temperature of 80 ℃, and the density of the applied current is 150mA/cm2The time for applying the current is 300 s;
the corrosion inhibitor with the mass percentage of 0.2% in the nitric acid solution is a tannic acid microcapsule and is prepared by the following steps:
s1, uniformly mixing fatty acid methyl ester and span 80 according to the mass ratio of 100:1, adding a tannic acid solution with the mass fraction of 60%, and uniformly stirring to obtain an emulsion, wherein the ratio of the addition volume of the tannic acid solution to the volume of the fatty acid methyl ester is 1: 6;
s2, mixing furfuryl alcohol and fatty acid methyl ester uniformly according to the mass ratio of 2:100, adding the emulsion obtained in the step S1, stirring and reacting for 60min to obtain microcapsule suspension, and performing centrifugal separation, washing and drying on the microcapsule suspension to obtain powdery tannin microcapsules, wherein the ratio of the adding volume of the emulsion to the volume of the mixed solution of the furfuryl alcohol and the fatty acid methyl ester is 2: 1;
(5) and (3) post-treatment: washing the aluminum foil treated in the step (4) with water, and then soaking in a nitric acid solution with the temperature of 55 ℃ and the mass percent of 7.5%, wherein the soaking time is 80 s;
(6) and (4) cleaning the aluminum foil treated in the step (5) by using tap water, then cleaning the aluminum foil by using pure water, drying and winding to obtain the etched foil.
Example 7:
a process method for medium-high voltage anode aluminum foil corrosion reaming comprises the following steps:
(1) pretreatment: soaking an aluminum foil in a solution A, wherein the solution A contains the following components in percentage by mass: 6% hydrochloric acid and 20% sulfuric acid; in the pretreatment, the soaking time is 100s, and the temperature of the solution A is 80 ℃;
(2) primary pitting corrosion: washing the aluminum foil treated in the step (1) with water, and then putting the aluminum foil into a solution B for primary direct-current pore-forming corrosion, wherein the solution B comprises the following components in percentage by mass: 8% hydrochloric acid, 15% sulfuric acid; in the first-stage direct-current hair hole corrosion, the applied current density is 600mA/cm2The time of applying the current is 65s, and the temperature of the solution B is 78 ℃;
(3) secondary reaming corrosion: washing the aluminum foil treated in the step (2) with water, and then putting the aluminum foil into a solution C for secondary pure chemical reaming corrosion, wherein the solution C is a hydrochloric acid solution with the mass percent of 6%; in the secondary reaming corrosion, the soaking time is 350s, the reaming corrosion weight loss control range is 10%, and the temperature of the solution C is 80 ℃;
(4) and (3) three-stage reaming corrosion: washing the aluminum foil treated in the step (3) with water, and then carrying out three-stage direct current electric reaming corrosion in a hydrochloric acid solution, wherein the reaming corrosion weight loss control range is 9%; the three-stage DC electric reaming corrosion in hydrochloric acid solution is carried out by putting aluminum foil in 3% by mass hydrochloric acid solution at 85 ℃, and applying electric current with density of 30mA/cm2The time for applying the current is 350 s;
the corrosion inhibitor in the hydrochloric acid solution is 0.2% in mass percentage, is a tannic acid microcapsule and is prepared according to the following steps:
s1, uniformly mixing fatty acid methyl ester and span 80 according to the mass ratio of 100:1, adding a tannic acid solution with the mass fraction of 60%, and uniformly stirring to obtain an emulsion, wherein the ratio of the addition volume of the tannic acid solution to the volume of the fatty acid methyl ester is 1: 6;
s2, mixing furfuryl alcohol and fatty acid methyl ester uniformly according to the mass ratio of 2:100, adding the emulsion obtained in the step S1, stirring and reacting for 60min to obtain microcapsule suspension, and performing centrifugal separation, washing and drying on the microcapsule suspension to obtain powdery tannin microcapsules, wherein the ratio of the adding volume of the emulsion to the volume of the mixed solution of the furfuryl alcohol and the fatty acid methyl ester is 2: 1;
(5) and (3) post-treatment: washing the aluminum foil treated in the step (4) with water, and then soaking the aluminum foil in a nitric acid solution with the temperature of 60 ℃ and the mass percent of 8% for 180 s;
(6) and (4) cleaning the aluminum foil treated in the step (5) by using tap water, then cleaning the aluminum foil by using pure water, drying and winding to obtain the etched foil.
Example 8:
a process method for medium-high voltage anode aluminum foil corrosion reaming comprises the following steps:
(1) pretreatment: soaking an aluminum foil in a solution A, wherein the solution A contains the following components in percentage by mass: 7.5% hydrochloric acid, 20% sulfuric acid; in the pretreatment, the soaking time is 100s, and the temperature of the solution A is 890 ℃;
(2) primary pitting corrosion: washing the aluminum foil treated in the step (1) with water, and then putting the aluminum foil into a solution B for primary direct-current pore-forming corrosion, wherein the solution B comprises the following components in percentage by mass: 2.5% hydrochloric acid, 30% sulfuric acid; in the primary direct current hair hole corrosion, the applied current density is 500mA/cm2The time of applying the current is 75s, and the temperature of the solution B is 76 ℃;
(3) secondary reaming corrosion: washing the aluminum foil treated in the step (2) with water, and then putting the aluminum foil into a solution C for secondary pure chemical reaming corrosion, wherein the solution C is a hydrochloric acid solution with the mass percent of 8%; in the secondary reaming corrosion, the soaking time is 250s, the reaming corrosion weight loss control range is 10%, and the temperature of the solution C is 85 ℃;
(4) and (3) three-stage reaming corrosion: washing the aluminum foil treated in the step (3) with water, and then carrying out three-stage direct current electric reaming corrosion in a nitric acid solution, wherein the reaming corrosion weight loss control range is 15%; the three-stage DC electric reaming corrosion in the nitric acid solution is carried out by putting the aluminum foil in the nitric acid solution with the mass percent of 7.5% and the temperature of 85 ℃, and the density of the applied current is 120mA/cm2The time for applying the current was 450 s;
the corrosion inhibitor with the mass percentage of 0.1% in the nitric acid solution is a tannic acid microcapsule and is prepared by the following steps:
s1, uniformly mixing fatty acid methyl ester and span 80 according to the mass ratio of 100:1, adding a tannic acid solution with the mass fraction of 60%, and uniformly stirring to obtain an emulsion, wherein the ratio of the addition volume of the tannic acid solution to the volume of the fatty acid methyl ester is 1: 6;
s2, mixing furfuryl alcohol and fatty acid methyl ester uniformly according to the mass ratio of 2:100, adding the emulsion obtained in the step S1, stirring and reacting for 60min to obtain microcapsule suspension, and performing centrifugal separation, washing and drying on the microcapsule suspension to obtain powdery tannin microcapsules, wherein the ratio of the adding volume of the emulsion to the volume of the mixed solution of the furfuryl alcohol and the fatty acid methyl ester is 2: 1;
(5) and (3) post-treatment: washing the aluminum foil treated in the step (4) with water, and then soaking the aluminum foil in a nitric acid solution with the temperature of 60 ℃ and the mass percent of 8% for 180 s;
(6) and (4) cleaning the aluminum foil treated in the step (5) by using tap water, then cleaning the aluminum foil by using pure water, drying and winding to obtain the etched foil.
Example 9:
a process method for medium-high voltage anode aluminum foil corrosion reaming comprises the following steps:
(1) pretreatment: soaking an aluminum foil in a solution A, wherein the solution A contains the following components in percentage by mass: 8% hydrochloric acid and 15% sulfuric acid; in the pretreatment, the soaking time is 180s, and the temperature of the solution A is 85 ℃;
(2) primary pitting corrosion: washing the aluminum foil treated in the step (1) with water, and then putting the aluminum foil into a solution B for primary direct-current pore-forming corrosion, wherein the solution B comprises the following components in percentage by mass: 2.5% hydrochloric acid, 30% sulfuric acid; in the first-stage direct-current hair hole corrosion, the applied current density is 550mA/cm2The time of applying the current is 90s, and the temperature of the solution B is 68 ℃;
(3) secondary reaming corrosion: washing the aluminum foil treated in the step (2) with water, and then putting the aluminum foil into a solution C for secondary pure chemical reaming corrosion, wherein the solution C is a hydrochloric acid solution with the mass percent of 7.5%; in the secondary reaming corrosion, the soaking time is 200s, the reaming corrosion weight loss control range is 9%, and the temperature of the solution C is 75 ℃;
(4) and (3) three-stage reaming corrosion: washing the aluminum foil treated in the step (3) with water, and then carrying out three-stage direct current electric reaming corrosion in a hydrochloric acid solution, wherein the reaming corrosion weight loss control range is 8%; the three-stage DC electric reaming corrosion in hydrochloric acid solution is carried out by putting the aluminum foil in 7.5% by mass of hydrochloric acid solution at 65 ℃ and applying electric current with the density of 10mA/cm2The time for applying the current was 450 s;
(5) and (3) post-treatment: washing the aluminum foil treated in the step (4) with water, and then soaking the aluminum foil in a nitric acid solution with the temperature of 70 ℃ and the mass percent of 3% for 50 s;
(6) and (4) cleaning the aluminum foil treated in the step (5) by using tap water, then cleaning the aluminum foil by using pure water, drying and winding to obtain the etched foil.
Example 10:
a process method for medium-high voltage anode aluminum foil corrosion reaming comprises the following steps:
(1) pretreatment: soaking an aluminum foil in a solution A, wherein the solution A contains the following components in percentage by mass: 8% hydrochloric acid and 15% sulfuric acid; in the pretreatment, the soaking time is 100s, and the temperature of the solution A is 85 ℃;
(2) primary pitting corrosion: washing the aluminum foil treated in the step (1) with water, and then putting the aluminum foil into a solution B for primary direct-current pore-forming corrosion, wherein the solution B comprises the following components in percentage by mass: 2% hydrochloric acid, 20% sulfuric acid; in the primary direct current hair hole corrosion, the applied current density is 700mA/cm2The time of applying the current is 95s, and the temperature of the solution B is 80 ℃;
(3) secondary reaming corrosion: washing the aluminum foil treated in the step (2) with water, and then putting the aluminum foil into a solution C for secondary pure chemical reaming corrosion, wherein the solution C is a hydrochloric acid solution with the mass percent of 1.5%; in the secondary reaming corrosion, the soaking time is 200s, the reaming corrosion weight loss control range is 9%, and the temperature of the solution C is 90 ℃;
(4) and (3) three-stage reaming corrosion: washing the aluminum foil treated in the step (3) with water, and then carrying out three-stage direct current electric reaming corrosion in a nitric acid solution, wherein the reaming corrosion weight loss control range is 8%; the three-stage DC electric reaming corrosion in the nitric acid solution is carried out by putting the aluminum foil in the nitric acid solution with the mass percent of 8% and the temperature of 90 ℃, and the density of the applied electric current is 180mA/cm2The time for applying the current was 450 s;
(5) and (3) post-treatment: washing the aluminum foil treated in the step (4) with water, and then soaking the aluminum foil in a nitric acid solution with the temperature of 50 ℃ and the mass percent of 3% for 200 s;
(6) and (4) cleaning the aluminum foil treated in the step (5) by using tap water, then cleaning the aluminum foil by using pure water, drying and winding to obtain the etched foil.
Example 11:
a process method for medium-high voltage anode aluminum foil corrosion reaming comprises the following steps:
(1) pretreatment: soaking an aluminum foil in a solution A, wherein the solution A contains the following components in percentage by mass: 10% hydrochloric acid and 40% sulfuric acid; in the pretreatment, the soaking time is 50s, and the temperature of the solution A is 50 ℃;
(2) primary pitting corrosion: washing the aluminum foil treated in the step (1) with water, and then putting the aluminum foil into a solution B for primary direct-current pore-forming corrosion, wherein the solution B comprises the following components in percentage by mass: 10% hydrochloric acid, 40% sulfuric acid; in the first-stage direct-current hair hole corrosion, the applied current density is 200mA/cm2The time of applying the current is 50s, and the temperature of the solution B is 65 ℃;
(3) secondary reaming corrosion: washing the aluminum foil treated in the step (2) with water, and then putting the aluminum foil into a solution C for secondary pure chemical reaming corrosion, wherein the solution C is a hydrochloric acid solution with the mass percentage of 10%; in the secondary reaming corrosion, the soaking time is 500s, the reaming corrosion weight loss control range is 15%, and the temperature of the solution C is 70 ℃;
(4) and (3) three-stage reaming corrosion: washing the aluminum foil treated in the step (3) with water, and then carrying out three-stage direct current electric reaming corrosion in a hydrochloric acid solution, wherein the reaming corrosion weight loss control range is 15%; the three-stage DC electric reaming corrosion in the nitric acid solution is carried out by carrying out the aluminum foil in the nitric acid solution with the mass percentage of 10% and the temperature of 60 ℃, and the density of the applied electric current is 50mA/cm2The time for applying the current is 200 s;
(5) and (3) post-treatment: washing the aluminum foil treated in the step (4) with water, and then soaking the aluminum foil in a nitric acid solution with the temperature of 50 ℃ and the mass percent of 1% for 50 s;
(6) and (4) cleaning the aluminum foil treated in the step (5) by using tap water, then cleaning the aluminum foil by using pure water, drying and winding to obtain the etched foil.
Example 12:
a process method for medium-high voltage anode aluminum foil corrosion reaming comprises the following steps:
(1) pretreatment: soaking an aluminum foil in a solution A, wherein the solution A contains the following components in percentage by mass: 1% hydrochloric acid and 10% sulfuric acid; in the pretreatment, the soaking time is 200s, and the temperature of the solution A is 90 ℃;
(2) primary pitting corrosion: washing the aluminum foil treated in the step (1) with water, and then putting the aluminum foil into a solution B for primary direct-current pore-forming corrosion, wherein the solution B comprises the following components in percentage by mass: 1% hydrochloric acid, 10% sulfuric acid; in the first-stage direct-current hair hole corrosion, the applied current density is 800mA/cm2The time of applying the current is 120s, and the temperature of the solution B is 85 ℃;
(3) secondary reaming corrosion: washing the aluminum foil treated in the step (2) with water, and then putting the aluminum foil into a solution C for secondary pure chemical reaming corrosion, wherein the solution C is a hydrochloric acid solution with the mass percent of 1%; in the secondary reaming corrosion, the soaking time is 500s, the reaming corrosion weight loss control range is 8%, and the temperature of the solution C is 90 ℃;
(4) and (3) three-stage reaming corrosion: washing the aluminum foil treated in the step (3) with water, and then carrying out three-stage direct current electric reaming corrosion in a nitric acid solution, wherein the reaming corrosion weight loss control range is 8%; the three-stage DC electric reaming corrosion in the nitric acid solution is carried out by carrying out the aluminum foil in the nitric acid solution with the mass percentage of 1% and the temperature of 90 ℃, and the density of the applied current is 200mA/cm2The time for applying the current is 500 s;
(5) and (3) post-treatment: washing the aluminum foil treated in the step (4) with water, and then soaking the aluminum foil in a nitric acid solution with the temperature of 70 ℃ and the mass percent of 10% for 200 s;
(6) and (4) cleaning the aluminum foil treated in the step (5) by using tap water, then cleaning the aluminum foil by using pure water, drying and winding to obtain the etched foil.
Comparative example 1:
the pure chemical reaming process by using hydrochloric acid comprises the following steps:
(1) pretreatment: soaking the aluminum foil in a mixed solution containing 5% by mass of hydrochloric acid and 25% by mass of sulfuric acid at the temperature of 80 ℃ for 120 s;
(2) primary pitting corrosion: washing the pretreated aluminum foil with water, and introducing into a furnace at 75 ℃, wherein the aluminum foil contains 5% hydrochloric acid by massAnd 25% sulfuric acid, and applying current at a density of 600mA/cm2The time for pore corrosion treatment is 80 s;
(3) secondary reaming corrosion: washing the aluminum foil subjected to the primary pore forming corrosion, then, carrying out secondary pure chemical pore-expanding corrosion in a hydrochloric acid solution with the temperature of 85 ℃ and the mass percentage of 2.5%, and soaking for 900 s;
(4) and (3) post-treatment: and washing the aluminum foil subjected to the second-stage hole expansion, then soaking the aluminum foil in a nitric acid solution with the temperature of 70 ℃ and the mass percent of 5% for 100s, and then washing the aluminum foil clean with water, drying and storing.
Comparative example 2:
a traditional hydrochloric acid electrochemical reaming process is adopted, and the method comprises the following steps:
(1) pretreatment: soaking the aluminum foil in a mixed solution containing 5% by mass of hydrochloric acid and 25% by mass of sulfuric acid at the temperature of 80 ℃ for 120 s;
(2) primary pitting corrosion: washing the pretreated aluminum foil with water, then carrying out primary direct current perforation corrosion in a mixed solution containing 5% by mass of hydrochloric acid and 25% by mass of sulfuric acid at the temperature of 75 ℃, and applying a current with the density of 600mA/cm2The time for pore corrosion treatment is 80 s;
(3) secondary reaming corrosion: washing the aluminum foil subjected to the first-stage perforation corrosion, then, putting the aluminum foil into a hydrochloric acid solution with the temperature of 82 ℃ and the mass percent of 2.5% for second-stage direct-current electric reaming corrosion, wherein the applied current density is 20mA/cm2Reaming corrosion treatment time is 600 s;
(4) and (3) post-treatment: and washing the aluminum foil subjected to the second-stage hole expansion, then soaking the aluminum foil in a nitric acid solution with the temperature of 70 ℃ and the mass percent of 5% for 100s, and then washing the aluminum foil clean with water, drying and storing.
Comparative example 3:
the traditional nitric acid electrochemical reaming process comprises the following steps:
(1) pretreatment: soaking the aluminum foil in a mixed solution containing 5% by mass of hydrochloric acid and 25% by mass of sulfuric acid at the temperature of 80 ℃ for 120 s;
(2) primary pitting corrosion: washing the pretreated aluminum foil with water, then carrying out primary direct current perforation corrosion in a mixed solution containing 5% by mass of hydrochloric acid and 25% by mass of sulfuric acid at the temperature of 75 ℃, and applying a current with the density of 600mA/cm2The time for pore corrosion treatment is 80 s;
(3) secondary reaming corrosion: washing the aluminum foil subjected to the primary hole forming corrosion, then, putting the aluminum foil into a nitric acid solution with the temperature of 70 ℃ and the mass percentage of 3% for secondary electrochemical hole expanding corrosion, and applying a current with the density of 100mA/cm2Reaming corrosion treatment time is 600 s;
(4) and (3) post-treatment: and washing the aluminum foil subjected to the second-stage hole expansion, then soaking the aluminum foil in a nitric acid solution with the temperature of 70 ℃ and the mass percent of 5% for 100s, and then washing the aluminum foil clean with water, drying and storing.
Comparative example 4:
a process method for medium-high voltage anode aluminum foil corrosion reaming comprises the following steps:
(1) pretreatment: soaking an aluminum foil in a solution A, wherein the solution A contains the following components in percentage by mass: 2% hydrochloric acid and 30% sulfuric acid; in the pretreatment, the soaking time is 150s, and the temperature of the solution A is 60 ℃;
(2) primary pitting corrosion: washing the aluminum foil treated in the step (1) with water, and then putting the aluminum foil into a solution B for primary direct-current pore-forming corrosion, wherein the solution B comprises the following components in percentage by mass: 3% hydrochloric acid, 35% sulfuric acid; in the first-stage direct-current hair hole corrosion, the applied current density is 300mA/cm2The time for applying the current is 80s, and the temperature of the solution B is 70 ℃;
(3) secondary reaming corrosion: washing the aluminum foil treated in the step (2) with water, and then putting the aluminum foil into a solution C for secondary pure chemical reaming corrosion, wherein the solution C is a hydrochloric acid solution with the mass percent of 2.5%; in the secondary reaming corrosion, the soaking time is 600s, the reaming corrosion weight loss control range is 5%, and the temperature of the solution C is 100 ℃;
(4) and (3) three-stage reaming corrosion: the aluminum foil treated by the step (3)Washing with water, and then carrying out three-stage direct current electric reaming corrosion in a hydrochloric acid solution, wherein the reaming corrosion weight loss control range is 12%; the three-stage DC electric reaming corrosion in hydrochloric acid solution is carried out by putting the aluminum foil in 2.5% by mass of hydrochloric acid solution at 80 ℃ and applying electric current with the density of 20mA/cm2The time for applying the current is 400 s;
the corrosion inhibitor in the hydrochloric acid solution is 0.2% in mass percentage, is a tannic acid microcapsule and is prepared according to the following steps:
s1, uniformly mixing fatty acid methyl ester and span 80 according to the mass ratio of 100:1, adding a tannic acid solution with the mass fraction of 60%, and uniformly stirring to obtain an emulsion, wherein the ratio of the addition volume of the tannic acid solution to the volume of the fatty acid methyl ester is 1: 6;
s2, mixing furfuryl alcohol and fatty acid methyl ester uniformly according to the mass ratio of 2:100, adding the emulsion obtained in the step S1, stirring and reacting for 60min to obtain microcapsule suspension, and performing centrifugal separation, washing and drying on the microcapsule suspension to obtain powdery tannin microcapsules, wherein the ratio of the adding volume of the emulsion to the volume of the mixed solution of the furfuryl alcohol and the fatty acid methyl ester is 2: 1;
(5) and (3) post-treatment: washing the aluminum foil treated in the step (4) with water, and then soaking the aluminum foil in a nitric acid solution with the temperature of 60 ℃ and the mass percent of 2.5%, wherein the soaking time is 100 s;
(6) and (4) cleaning the aluminum foil treated in the step (5) by using tap water, then cleaning the aluminum foil by using pure water, drying and winding to obtain the etched foil.
Comparative example 5:
a process method for medium-high voltage anode aluminum foil corrosion reaming comprises the following steps:
(1) pretreatment: soaking an aluminum foil in a solution A, wherein the solution A contains the following components in percentage by mass: 2% hydrochloric acid and 30% sulfuric acid; in the pretreatment, the soaking time is 150s, and the temperature of the solution A is 60 ℃;
(2) primary pitting corrosion: will go through the stepWashing the aluminum foil treated in the step (1), and then putting the aluminum foil into a solution B for primary direct-current pore-forming corrosion, wherein the solution B contains the following components in percentage by mass: 3% hydrochloric acid, 35% sulfuric acid; in the first-stage direct-current hair hole corrosion, the applied current density is 300mA/cm2The time for applying the current is 80s, and the temperature of the solution B is 70 ℃;
(3) secondary reaming corrosion: washing the aluminum foil treated in the step (2) with water, and then putting the aluminum foil into a solution C for secondary pure chemical reaming corrosion, wherein the solution C is a hydrochloric acid solution with the mass percent of 2.5%; in the secondary reaming corrosion, the soaking time is 800s, the reaming corrosion weight loss control range is 5%, and the temperature of the solution C is 40 ℃;
(4) and (3) three-stage reaming corrosion: washing the aluminum foil treated in the step (3) with water, and then carrying out three-stage direct current electric reaming corrosion in a nitric acid solution, wherein the reaming corrosion weight loss control range is 12%; the three-stage DC electric reaming corrosion in the nitric acid solution is carried out by putting the aluminum foil in the nitric acid solution with the mass percentage of 3% and the temperature of 70 ℃, and the density of the applied electric current is 100mA/cm2The time for applying the current is 350 s;
the corrosion inhibitor with the mass percentage of 0.2% in the nitric acid solution is a tannic acid microcapsule and is prepared by the following steps:
s1, uniformly mixing fatty acid methyl ester and span 80 according to the mass ratio of 100:1, adding a tannic acid solution with the mass fraction of 60%, and uniformly stirring to obtain an emulsion, wherein the ratio of the addition volume of the tannic acid solution to the volume of the fatty acid methyl ester is 1: 6;
s2, mixing furfuryl alcohol and fatty acid methyl ester uniformly according to the mass ratio of 2:100, adding the emulsion obtained in the step S1, stirring and reacting for 60min to obtain microcapsule suspension, and performing centrifugal separation, washing and drying on the microcapsule suspension to obtain powdery tannin microcapsules, wherein the ratio of the adding volume of the emulsion to the volume of the mixed solution of the furfuryl alcohol and the fatty acid methyl ester is 2: 1;
(5) and (3) post-treatment: washing the aluminum foil treated in the step (4) with water, and then soaking the aluminum foil in a nitric acid solution with the temperature of 60 ℃ and the mass percent of 2.5%, wherein the soaking time is 100 s;
(6) and (4) cleaning the aluminum foil treated in the step (5) by using tap water, then cleaning the aluminum foil by using pure water, drying and winding to obtain the etched foil.
Comparative example 6:
a process method for medium-high voltage anode aluminum foil corrosion reaming comprises the following steps:
(1) pretreatment: soaking an aluminum foil in a solution A, wherein the solution A contains the following components in percentage by mass: 2.5% hydrochloric acid, 15% sulfuric acid; in the pretreatment, the soaking time is 150s, and the temperature of the solution A is 60 ℃;
(2) primary pitting corrosion: washing the aluminum foil treated in the step (1) with water, and then putting the aluminum foil into a solution B for primary direct-current pore-forming corrosion, wherein the solution B comprises the following components in percentage by mass: 4% hydrochloric acid, 25% sulfuric acid; in the first-stage direct-current hair hole corrosion, the applied current density is 300mA/cm2The time for applying the current is 80s, and the temperature of the solution B is 70 ℃;
(3) secondary reaming corrosion: washing the aluminum foil treated in the step (2) with water, and then putting the aluminum foil into a solution C for secondary pure chemical reaming corrosion, wherein the solution C is a hydrochloric acid solution with the mass percent of 8%; in the secondary reaming corrosion, the soaking time is 100s, the reaming corrosion weight loss control range is 5%, and the temperature of the solution C is 100 ℃;
(4) and (3) three-stage reaming corrosion: washing the aluminum foil treated in the step (3) with water, and then carrying out three-stage direct current electric reaming corrosion in a hydrochloric acid solution, wherein the reaming corrosion weight loss control range is 12%; the three-stage DC electric reaming corrosion in the nitric acid solution is carried out by putting the aluminum foil in the nitric acid solution with the mass percentage of 3% and the temperature of 70 ℃, and the density of the applied electric current is 100mA/cm2The time for applying the current is 350 s;
the corrosion inhibitor in the hydrochloric acid solution is 0.1% by mass, is a tannic acid microcapsule and is prepared by the following steps:
s1, uniformly mixing fatty acid methyl ester and span 80 according to the mass ratio of 100:1, adding a tannic acid solution with the mass fraction of 60%, and uniformly stirring to obtain an emulsion, wherein the ratio of the addition volume of the tannic acid solution to the volume of the fatty acid methyl ester is 1: 6;
s2, mixing furfuryl alcohol and fatty acid methyl ester uniformly according to the mass ratio of 2:100, adding the emulsion obtained in the step S1, stirring and reacting for 60min to obtain microcapsule suspension, and performing centrifugal separation, washing and drying on the microcapsule suspension to obtain powdery tannin microcapsules, wherein the ratio of the adding volume of the emulsion to the volume of the mixed solution of the furfuryl alcohol and the fatty acid methyl ester is 2: 1;
(5) and (3) post-treatment: washing the aluminum foil treated in the step (4) with water, and then soaking the aluminum foil in a nitric acid solution with the temperature of 60 ℃ and the mass percent of 2.5%, wherein the soaking time is 100 s;
(6) and (4) cleaning the aluminum foil treated in the step (5) by using tap water, then cleaning the aluminum foil by using pure water, drying and winding to obtain the etched foil.
Comparative example 7:
a process method for medium-high voltage anode aluminum foil corrosion reaming comprises the following steps:
(1) pretreatment: soaking an aluminum foil in a solution A, wherein the solution A contains the following components in percentage by mass: 2.5% hydrochloric acid, 15% sulfuric acid; in the pretreatment, the soaking time is 150s, and the temperature of the solution A is 60 ℃;
(2) primary pitting corrosion: washing the aluminum foil treated in the step (1) with water, and then putting the aluminum foil into a solution B for primary direct-current pore-forming corrosion, wherein the solution B comprises the following components in percentage by mass: 4% hydrochloric acid, 25% sulfuric acid; in the first-stage direct-current hair hole corrosion, the applied current density is 300mA/cm2The time for applying the current is 80s, and the temperature of the solution B is 70 ℃;
(3) secondary reaming corrosion: washing the aluminum foil treated in the step (2) with water, and then putting the aluminum foil into a solution C for secondary pure chemical reaming corrosion, wherein the solution C is a hydrochloric acid solution with the mass percent of 2.5%; in the secondary reaming corrosion, the soaking time is 400s, the reaming corrosion weight loss control range is 10%, and the temperature of the solution C is 85 ℃;
(4) and (3) three-stage reaming corrosion: washing the aluminum foil treated in the step (3) with water, and then carrying out three-stage direct current electric reaming corrosion in a nitric acid solution, wherein the reaming corrosion weight loss control range is 5%; the three-stage DC electric reaming corrosion in the nitric acid solution is carried out by putting the aluminum foil in the nitric acid solution with the mass percentage of 3% and the temperature of 50 ℃, and the density of the applied current is 300mA/cm2The time for applying the current is 100 s;
the corrosion inhibitor with the mass percentage of 0.1% in the nitric acid solution is a tannic acid microcapsule and is prepared by the following steps:
s1, uniformly mixing fatty acid methyl ester and span 80 according to the mass ratio of 100:1, adding a tannic acid solution with the mass fraction of 60%, and uniformly stirring to obtain an emulsion, wherein the ratio of the addition volume of the tannic acid solution to the volume of the fatty acid methyl ester is 1: 6;
s2, mixing furfuryl alcohol and fatty acid methyl ester uniformly according to the mass ratio of 2:100, adding the emulsion obtained in the step S1, stirring and reacting for 60min to obtain microcapsule suspension, and performing centrifugal separation, washing and drying on the microcapsule suspension to obtain powdery tannin microcapsules, wherein the ratio of the adding volume of the emulsion to the volume of the mixed solution of the furfuryl alcohol and the fatty acid methyl ester is 2: 1;
(5) and (3) post-treatment: washing the aluminum foil treated in the step (4) with water, and then soaking the aluminum foil in a nitric acid solution with the temperature of 60 ℃ and the mass percent of 2.5%, wherein the soaking time is 100 s;
(6) and (4) cleaning the aluminum foil treated in the step (5) by using tap water, then cleaning the aluminum foil by using pure water, drying and winding to obtain the etched foil.
Comparative example 8:
a process method for medium-high voltage anode aluminum foil corrosion reaming comprises the following steps:
(1) pretreatment: soaking an aluminum foil in a solution A, wherein the solution A contains the following components in percentage by mass: 2.5% hydrochloric acid, 15% sulfuric acid; in the pretreatment, the soaking time is 150s, and the temperature of the solution A is 60 ℃;
(2) primary pitting corrosion: washing the aluminum foil treated in the step (1) with water, and then putting the aluminum foil into a solution B for primary direct-current pore-forming corrosion, wherein the solution B comprises the following components in percentage by mass: 4% hydrochloric acid, 25% sulfuric acid; in the first-stage direct-current hair hole corrosion, the applied current density is 300mA/cm2The time for applying the current is 80s, and the temperature of the solution B is 70 ℃;
(3) secondary reaming corrosion: washing the aluminum foil treated in the step (2) with water, and then putting the aluminum foil into a solution C for secondary pure chemical reaming corrosion, wherein the solution C is a hydrochloric acid solution with the mass percent of 2.5%; in the secondary reaming corrosion, the soaking time is 400s, the reaming corrosion weight loss control range is 10%, and the temperature of the solution C is 85 ℃;
(4) and (3) three-stage reaming corrosion: washing the aluminum foil treated in the step (3) with water, and then carrying out three-stage direct current electric reaming corrosion in a hydrochloric acid solution, wherein the reaming corrosion weight loss control range is 12%; the three-stage DC electric reaming corrosion in hydrochloric acid solution is carried out by putting aluminum foil in 2.5% by mass hydrochloric acid solution at 100 ℃, and applying electric current with density of 55mA/cm2The time for applying the current is 100 s;
the corrosion inhibitor in the hydrochloric acid solution is 0.1% by mass, is a tannic acid microcapsule and is prepared by the following steps:
s1, uniformly mixing fatty acid methyl ester and span 80 according to the mass ratio of 100:1, adding a tannic acid solution with the mass fraction of 60%, and uniformly stirring to obtain an emulsion, wherein the ratio of the addition volume of the tannic acid solution to the volume of the fatty acid methyl ester is 1: 6;
s2, mixing furfuryl alcohol and fatty acid methyl ester uniformly according to the mass ratio of 2:100, adding the emulsion obtained in the step S1, stirring and reacting for 60min to obtain microcapsule suspension, and performing centrifugal separation, washing and drying on the microcapsule suspension to obtain powdery tannin microcapsules, wherein the ratio of the adding volume of the emulsion to the volume of the mixed solution of the furfuryl alcohol and the fatty acid methyl ester is 2: 1;
(5) and (3) post-treatment: washing the aluminum foil treated in the step (4) with water, and then soaking the aluminum foil in a nitric acid solution with the temperature of 60 ℃ and the mass percent of 2.5%, wherein the soaking time is 100 s;
(6) and (4) cleaning the aluminum foil treated in the step (5) by using tap water, then cleaning the aluminum foil by using pure water, drying and winding to obtain the etched foil.
Comparative example 9:
a process method for medium-high voltage anode aluminum foil corrosion reaming comprises the following steps:
(1) pretreatment: soaking an aluminum foil in a solution A, wherein the solution A contains the following components in percentage by mass: 2.5% hydrochloric acid, 15% sulfuric acid; in the pretreatment, the soaking time is 150s, and the temperature of the solution A is 60 ℃;
(2) primary pitting corrosion: washing the aluminum foil treated in the step (1) with water, and then putting the aluminum foil into a solution B for primary direct-current pore-forming corrosion, wherein the solution B comprises the following components in percentage by mass: 4% hydrochloric acid, 25% sulfuric acid; in the first-stage direct-current hair hole corrosion, the applied current density is 300mA/cm2The time for applying the current is 80s, and the temperature of the solution B is 70 ℃;
(3) secondary reaming corrosion: washing the aluminum foil treated in the step (2) with water, and then putting the aluminum foil into a solution C for secondary pure chemical reaming corrosion, wherein the solution C is a hydrochloric acid solution with the mass percent of 2.5%; in the secondary reaming corrosion, the soaking time is 400s, the reaming corrosion weight loss control range is 10%, and the temperature of the solution C is 85 ℃;
(4) and (3) three-stage reaming corrosion: washing the aluminum foil treated in the step (3) with water, and then carrying out three-stage direct current electric reaming corrosion in a nitric acid solution or a hydrochloric acid solution, wherein the reaming corrosion weight loss control range is 12%; what is needed isThe three-stage DC electric reaming corrosion in hydrochloric acid solution is carried out by putting aluminum foil in 2.5% by mass hydrochloric acid solution at 50 deg.C, and applying electric current with density of 55mA/cm2The time for applying the current is 100 s;
the corrosion inhibitor in the hydrochloric acid solution is 0.1% by mass, is a tannic acid microcapsule and is prepared by the following steps:
s1, uniformly mixing fatty acid methyl ester and span 80 according to the mass ratio of 100:1, adding a tannic acid solution with the mass fraction of 60%, and uniformly stirring to obtain an emulsion, wherein the ratio of the addition volume of the tannic acid solution to the volume of the fatty acid methyl ester is 1: 6;
s2, mixing furfuryl alcohol and fatty acid methyl ester uniformly according to the mass ratio of 2:100, adding the emulsion obtained in the step S1, stirring and reacting for 60min to obtain microcapsule suspension, and performing centrifugal separation, washing and drying on the microcapsule suspension to obtain powdery tannin microcapsules, wherein the ratio of the adding volume of the emulsion to the volume of the mixed solution of the furfuryl alcohol and the fatty acid methyl ester is 2: 1;
(5) and (3) post-treatment: washing the aluminum foil treated in the step (4) with water, and then soaking the aluminum foil in a nitric acid solution with the temperature of 60 ℃ and the mass percent of 2.5%, wherein the soaking time is 100 s;
(6) cleaning the aluminum foil treated in the step (5) with tap water, then cleaning with pure water, drying and winding to obtain the etched foil
Experimental example:
the medium-high voltage anodic corrosion aluminum foil is produced according to the methods of examples 1 to 12 and comparative examples 1 to 9, and then the obtained corrosion foil is subjected to corrosion treatment according to the electronic industry standard SJ/T1140-2012 of the people's republic of China: 520V formation of the etched foil was carried out by the method described in "electrode foil for aluminum electrolytic capacitor" to obtain an aluminum foil product, and the properties of the aluminum foil product were examined, and the specific results are shown in Table 1.
TABLE 1 aluminum foil product Performance test results
Figure 763409DEST_PATH_IMAGE001
The detection results show that the method can effectively improve the performance of the aluminum foil product, the process is very simple, the production is easy to realize, the production cost is low, chemical reagents such as nitric acid, phosphoric acid and the like can be not used or used in a small amount, the generation of ammonia nitrogen and phosphorus wastewater is greatly reduced, and the environmental protection cost is reduced.
Furthermore, it should be understood that although the present description refers to embodiments, not every embodiment may contain only a single embodiment, and such description is for clarity only, and those skilled in the art should integrate the description, and the embodiments may be combined as appropriate to form other embodiments understood by those skilled in the art.

Claims (7)

1. A middle-high voltage anode aluminum foil corrosion reaming process method is characterized in that: the method comprises the following steps:
(1) pretreatment: soaking an aluminum foil in a solution A, wherein the solution A contains the following components in percentage by mass: 1-10% hydrochloric acid and 10-40% sulfuric acid; in the pretreatment, the soaking time is 50-200 s;
(2) primary pitting corrosion: washing the aluminum foil treated in the step (1) with water, and then putting the aluminum foil into a solution B for primary direct-current pore-forming corrosion, wherein the solution B comprises the following components in percentage by mass: 1-10% hydrochloric acid and 10-40% sulfuric acid; in the primary direct current perforation corrosion, the applied current density is 200-800 mA/cm2The time for applying the current is 50-120 s;
(3) secondary reaming corrosion: washing the aluminum foil treated in the step (2) with water, and then putting the aluminum foil into a solution C for secondary pure chemical reaming corrosion, wherein the solution C is a hydrochloric acid solution with the mass percent of 1-10%; in the secondary reaming corrosion, the soaking time is 200-500 s, and the reaming corrosion weight loss control range is 8-15%;
(4) and (3) three-stage reaming corrosion: will go through the steps(3) Washing the treated aluminum foil with water, and then carrying out three-stage direct current electric reaming corrosion in a nitric acid solution or a hydrochloric acid solution, wherein the reaming corrosion weight loss control range is 8-15%; the three-stage DC electric reaming corrosion in the nitric acid solution is carried out by putting the aluminum foil in the nitric acid solution with the mass percent of 1-10% and the temperature of 60-90 ℃, and the density of applied current is 50-200 mA/cm2The time for applying the current is 200-500 s; the three-stage DC electric reaming corrosion in the hydrochloric acid solution is carried out by putting the aluminum foil in the hydrochloric acid solution with the mass percent of 1-10% and the temperature of 60-90 ℃, and the density of the applied current is 7-45 mA/cm2The time for applying the current is 200-500 s;
(5) and (3) post-treatment: washing the aluminum foil treated in the step (4) with water, and then soaking the aluminum foil in a nitric acid solution with the temperature of 50-70 ℃ and the mass percent of 1-10% for 50-200 s;
(6) and (4) cleaning the aluminum foil treated in the step (5) by using tap water, then cleaning the aluminum foil by using pure water, drying and winding to obtain the etched foil.
2. The medium-high voltage anode aluminum foil corrosion reaming process method as claimed in claim 1, characterized in that: the temperature of the solution A in the step (1) is 50-90 ℃.
3. The medium-high voltage anode aluminum foil corrosion reaming process method as claimed in claim 1, characterized in that: the temperature of the solution B in the step (2) is 65-85 ℃.
4. The medium-high voltage anode aluminum foil corrosion reaming process method as claimed in claim 1, characterized in that: the temperature of the solution C in the step (3) is 70-90 ℃.
5. The medium-high voltage anode aluminum foil corrosion reaming process method as claimed in claim 1, characterized in that: in the step (4), the nitric acid solution or the hydrochloric acid solution contains 0.1-0.3% of corrosion inhibitor by mass, and the corrosion inhibitor is a tannic acid microcapsule and is prepared according to the following steps:
s1, mixing fatty acid methyl ester and span 80 uniformly, adding tannic acid solution with the mass fraction of 60%, and stirring uniformly to obtain emulsion;
s2, mixing furfuryl alcohol and fatty acid methyl ester uniformly, adding the emulsion obtained in the step S1, stirring and reacting for 60min to obtain a microcapsule suspension, and then performing centrifugal separation, washing and drying on the microcapsule suspension to obtain the powdery tannin microcapsule.
6. The medium-high voltage anode aluminum foil corrosion reaming process method as claimed in claim 5, characterized in that: in the step S1, the fatty acid methyl ester and the span 80 are mixed according to the mass ratio of 100:1, and the ratio of the addition volume of the tannic acid solution to the volume of the fatty acid methyl ester is 1: 6.
7. The medium-high voltage anode aluminum foil corrosion reaming process method as claimed in claim 5, characterized in that: in the step S2, the furfuryl alcohol and the fatty acid methyl ester are mixed according to the mass ratio of 2:100, and the ratio of the adding volume of the emulsion to the volume of the mixed solution of the furfuryl alcohol and the fatty acid methyl ester is 2: 1.
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