CN111519239A - Etching method for ultrahigh-pressure etched foil - Google Patents
Etching method for ultrahigh-pressure etched foil Download PDFInfo
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- CN111519239A CN111519239A CN202010419733.4A CN202010419733A CN111519239A CN 111519239 A CN111519239 A CN 111519239A CN 202010419733 A CN202010419733 A CN 202010419733A CN 111519239 A CN111519239 A CN 111519239A
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- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
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Abstract
An etching method for ultrahigh pressure etching of foil, comprising: primary pretreatment: using 8-40wt% sulfuric acid and 1-10 wt% hydrochloric acid mixed solution, the temperature is 20-50 ℃, and the treatment time is controlled at 10-30 seconds; secondary pretreatment: using 8-40wt% sulfuric acid and 1-10 wt% hydrochloric acid mixed solution, adding a small amount of ferric chloride, wherein the ferric chloride content is 0.01-1g/L, the temperature is 30-60 ℃, and performing initial pitting treatment by adopting alternating current with the frequency of 50-100HZ and low power; first-stage corrosion: using 8-40wt% sulfuric acid and 1-10 wt% hydrochloric acid mixed solution, at 50-80 deg.C, performing electrolytic corrosion in intermittent pulse power-on mode, cutting off power for 6 times, each power-on time being 13-23s, and cutting off power for 8s, and using direct current; secondary corrosion: the corrosion solution is 1-10 wt% of nitric acid and corrosion inhibitor, the temperature is 30-80 ℃, direct current is adopted, and the current density is 0.05-0.2A/cm2(ii) a And (3) post-treatment: 1-10 wt% of nitric acid is adopted, the temperature is 30-70 ℃, and the cleaning time is 1-5 minutes; then cleaning with pure water, and drying in an oven at 100 ℃.
Description
Technical Field
The invention relates to the field of electrolytic corrosion processes, in particular to a corrosion method for ultrahigh-pressure corrosion foil.
Background
The ultrahigh voltage electrode foil can be used for capacitors with ultrahigh voltage requirements and large specific capacity, and is required by medium and high voltage frequency converters, inverters and communication power supplies. At present, the electrolytic corrosion process of the medium-high voltage aluminum foil generally comprises pretreatment, holing corrosion, reaming corrosion and post-treatment. The specific procedures are as follows: firstly, placing the aluminum foil in alkaline or acidic pretreatment at 30-80 ℃ for soaking for 20-90 seconds to remove oil stains, impurities and oxidation films on the surface of the aluminum foil, improve the surface state and promote the next step of pore-forming corrosion of the aluminum foil; the hole forming process is to form initial tunnel holes with certain length and hole diameter on the surface of the aluminum foil by applying direct current, the solution of the process is mixed solution of 8-40wt% of sulfuric acid and 1-10 wt% of hydrochloric acid, the temperature is 40-85 ℃, direct current constant current is used for electrification, and the current density is 0.15-1.0A/cm2The time is 60-120 seconds; the hole expanding process comprises the step of further electrifying and corroding on the basis of the initial tunnel hole to further expand the hole diameter of the tunnel hole to the required size, wherein the solution of the process is 1-10 wt% of nitric acid, the temperature is 30-80 ℃, direct current is adopted, and the electric quantity is 30-60C/cm2The current density is 0.05-0.5A/cm2(ii) a The post-treatment process is to eliminate residual metal impurities and chloride ions on the surface of the aluminum foil by using 1-10 wt% of nitric acid at 30-70 ℃ for 1-10 minutes.
The anode foil produced by the traditional corrosion process has small corrosion holes, and the corrosion holes are easy to block during high-voltage formation, so that the research on the large-aperture electrode foil is needed to meet the requirement.
Disclosure of Invention
The invention provides a corrosion method for improving the aperture of an electrode foil aiming at the defects and the defects of the prior art, which changes the traditional idea of improving the aperture by utilizing the reaming stage, innovatively provides a method for improving the density of etched holes, forming combined holes and expanding the aperture by utilizing the combined holes in the pre-treatment and the hole-forming stage.
An etching method for ultrahigh pressure etching foil comprises the following steps:
primary pretreatment: using 8-40wt% sulfuric acid and 1-10 wt% hydrochloric acid mixed solution, the temperature is 20-50 ℃, and the treatment time is controlled at 10-30 seconds;
secondary pretreatment: using 8-40wt% sulfuric acid and 1-10 wt% hydrochloric acid mixed solution, adding a small amount of ferric chloride, wherein the ferric chloride content is 0.01-1g/L, the temperature is 30-60 ℃, and performing initial pitting treatment by adopting alternating current with the frequency of 50-100HZ and low power;
first-stage corrosion: using 8-40wt% sulfuric acid and 1-10 wt% hydrochloric acid mixed solution, at 50-80 deg.C, performing electrolytic corrosion in intermittent pulse power-on mode, cutting off power for 6 times, each power-on time being 13-23s, and cutting off power for 8s, and using direct current;
secondary corrosion: the corrosion solution is 1-10 wt% of nitric acid and corrosion inhibitor, the temperature is 30-80 ℃, direct current is adopted, and the current density is 0.05-0.2A/cm 2;
and (3) post-treatment: 1-10 wt% of nitric acid is adopted, the temperature is 30-70 ℃, and the cleaning time is 1-5 minutes; then cleaning with pure water, and drying in an oven at 100 ℃.
Further, in the primary pretreatment, oil stains on the surface of the aluminum foil are removed by soaking for a short time.
Furthermore, in the secondary pretreatment, a plurality of etching pits are formed in the area which is not easy to generate holes by adding metal ions and applying high-frequency low-electricity alternating current corrosion, so that the density and the uniformity of the etching pits are improved.
Further, in the first stage corrosion, the pulse energization mode is that the first energization for 3-8s in the first stage attenuates the current density from 1.5-1A/cm2 to 0.75-0.5A/cm2, and the second energization for 10-15s in the second stage attenuates the current density from 0.75-0.5A/cm2 to 0.2-0.01A/cm 2.
Furthermore, in the pulse electrification, the high current density attenuation in the first stage promotes the surface of the aluminum foil to generate corrosion pits, so that the hole density on the surface of the aluminum foil is ensured, and the attenuation process in the second stage provides energy for the continuous growth of the holes, so that the holes are ensured to grow to a certain length; the formation of adjacent holes was promoted by 7 intermittent energization with a continuous increase in the hole density.
Furthermore, in the secondary corrosion, the corrosion inhibitor adopts a substance with a larger molecular weight, and has good adsorption performance on the surface of the aluminum foil so as to achieve the corrosion inhibition effect on the surface of the aluminum foil; the current is preferably a small current.
Compared with the prior art, the invention has the following technical effects:
(1) the traditional idea of expanding the hole first and then expanding the hole is abandoned, and the high-density expanded holes form the parallel holes, so that the effect of expanding the aperture is also achieved.
(2) In order to improve the density of the pores, the pretreatment of the invention is carried out in two steps, wherein in the first step, hydrochloric acid and sulfuric acid mixed solution is adopted to effectively remove an oxide film and impurities on the surface of the aluminum foil; and secondly, adding metal ions into the mixed solution, and applying high-frequency low-power alternating current corrosion to uniformly activate the surface of the aluminum foil and improve the pitting density of the aluminum foil.
(3) In order to improve the hole-emitting density, the hole-emitting stage of the invention adopts a seven-level pulse power-on mode, and the current density of the mode is changed from big to small: the high current density is used for improving the surface porosity; the attenuation process enables the lengths of a plurality of holes to be consistent; seven times of electrification cause the holes with too high density to be combined to increase the aperture.
(4) The reaming stage of the invention adopts small current corrosion to avoid secondary small-bore hole formation caused by overhigh current.
Drawings
Fig. 1 is a flow chart illustrating the steps of the method for etching an ultra-high pressure etched foil according to an embodiment of the present invention.
FIG. 2 is a table showing the results of the tests conducted in the comparative example and the three examples of the present invention.
Detailed Description
The technical scheme of the invention is further explained in detail by combining the drawings in the specification.
Comparative example:
pretreatment: the aluminum foil was immersed in a mixture of 28wt% sulfuric acid and 4wt% hydrochloric acid at 50 ℃ for 50 seconds.
First-stage corrosion: 35 wt% of sulfuric acid and 9 wt% of hydrochloric acid mixed solution, the temperature is 74 ℃, direct current constant current electrification is carried out, and the current density is 0.7A/cm2The time was 70 seconds.
Secondary corrosion: 8wt% nitric acid at 72 deg.C, and DC with current density of 0.2A/cm2The time period was 10 minutes.
And (3) post-treatment: 5 wt% nitric acid, 60 deg.C, and washing time controlled at 2 min.
Example 1:
primary pretreatment: a mixture of 28wt% sulfuric acid and 4wt% hydrochloric acid was used at 45 ℃ for 20 seconds.
Secondary pretreatment: using a mixture of 28wt% sulfuric acid and 4wt% hydrochloric acid, adding 0.08g/L ferric chloride at 55 deg.C, and applying AC frequency of 50HZ and 0.1A/cm2And 5s, performing initial pitting treatment.
First-stage corrosion: using 35 wt% sulfuric acid and 9 wt% hydrochloric acid mixed solution, at 70 deg.C, adopting 7 intermittent pulse power-on modes to perform electrolytic corrosion, and adopting direct current for 6 times, each power-on time is 18s, and power-off time is 8 s. Pulse energization mode: the current density was reduced from 1.4A/cm2 to 0.6A/cm2 by applying electricity for 6s, and from 0.6A/cm2 to 0.02A/cm2 by applying electricity for 12 s.
Secondary corrosion: the corrosive liquid is 9 wt% nitric acid and 0.1g/L sodium polystyrene sulfonate, the temperature is 65 ℃, direct current is adopted, and the current density is 0.08A/cm2And, 5 minutes.
And (3) post-treatment: 5 wt% nitric acid was used at 60 ℃ for 2 minutes.
Example 2:
primary pretreatment: a mixture of 30wt% sulfuric acid and 6wt% hydrochloric acid was used at 45 ℃ for 20 seconds.
Secondary pretreatment: the initial pitting treatment was carried out using a mixture of 30wt% sulfuric acid and 6wt% hydrochloric acid, 0.06g/L ferric chloride, at 55 ℃ and an alternating current frequency of 80Hz, 0.06A/cm2, 8 seconds.
First-stage corrosion: using 35 wt% sulfuric acid and 9 wt% hydrochloric acid mixed solution, at 70 deg.C, adopting 7 intermittent pulse power-on modes to perform electrolytic corrosion, and adopting direct current for 6 times, each power-on time is 18s, and power-off time is 8 s. Pulse energization mode: current density was first attenuated from 1.3A/cm2 to 0.7A/cm2 by applying electricity for 7s, and then attenuated from 0.7A/cm2 to 0.02A/cm2 by applying electricity for 11 s.
Secondary corrosion: the corrosive liquid is 9 wt% nitric acid and 0.1g/L sodium polystyrene sulfonate, the temperature is 65 ℃, direct current is adopted, and the current density is 0.08A/cm2And, 5 minutes.
And (3) post-treatment: 5 wt% nitric acid was used at 60 ℃ for 2 minutes.
Example 3:
primary pretreatment: a mixture of 28wt% sulfuric acid and 4wt% hydrochloric acid was used at 45 ℃ for 20 seconds.
Secondary pretreatment: the initial pitting treatment was carried out using a mixture of 28wt% sulfuric acid and 4wt% hydrochloric acid, 0.08g/L ferric chloride, at 55 ℃ and an alternating current frequency of 80Hz, 0.06A/cm2, 8 seconds.
First-stage corrosion: using 35 wt% sulfuric acid and 9 wt% hydrochloric acid mixed solution, at 70 deg.C, adopting 7 intermittent pulse power-on modes to perform electrolytic corrosion, and adopting direct current for 6 times, each power-on time is 18s, and power-off time is 8 s. Pulse energization mode: the current density was reduced from 1.3A/cm2 to 0.6A/cm2 by adding 8s, and from 0.6A/cm2 to 0.02A/cm2 by adding 10 s.
Secondary corrosion: the corrosive liquid is 9 wt% nitric acid and 0.1g/L sodium polystyrene sulfonate, the temperature is 65 ℃, direct current is adopted, and the current density is 0.1A/cm2 for 4 minutes.
And (3) post-treatment: 5 wt% nitric acid was used at 60 ℃ for 2 minutes.
Example 4:
primary pretreatment: a mixture of 30wt% sulfuric acid and 6wt% hydrochloric acid was used at 45 ℃ for 20 seconds.
Secondary pretreatment: the initial pitting treatment was carried out using a mixture of 30wt% sulfuric acid and 6wt% hydrochloric acid, 0.06g/L ferric chloride, at 55 ℃ and an alternating current frequency of 50Hz, 0.1A/cm2, 5 seconds.
First-stage corrosion: using 35 wt% sulfuric acid and 9 wt% hydrochloric acid mixed solution, at 70 deg.C, adopting 7 intermittent pulse power-on modes to perform electrolytic corrosion, and adopting direct current for 6 times, each power-on time is 18s, and power-off time is 8 s. Pulse energization mode: the current density was reduced from 1.4A/cm2 to 0.8A/cm2 by applying electricity for 5s, and from 0.8A/cm2 to 0.02A/cm2 by applying electricity for 13 s.
Secondary corrosion: the corrosive liquid is 9 wt% nitric acid and 0.1g/L sodium polystyrene sulfonate, the temperature is 65 ℃, direct current is adopted, and the current density is 0.1A/cm2 for 4 minutes.
And (3) post-treatment: 5 wt% nitric acid was used at 60 ℃ for 2 minutes.
The performance of the electrode foils for aluminum electrolytic capacitors prepared in the above examples and comparative examples was tested according to the standard "electrode foil for SJ/T11140-.
The above description is only a preferred embodiment of the present invention, and the scope of the present invention is not limited to the above embodiment, but equivalent modifications or changes made by those skilled in the art according to the present disclosure should be included in the scope of the present invention as set forth in the appended claims.
Claims (6)
1. An etching method for ultrahigh pressure etching foil is characterized in that: the etching method comprises the following steps:
primary pretreatment: using 8-40wt% sulfuric acid and 1-10 wt% hydrochloric acid mixed solution, the temperature is 20-50 ℃, and the treatment time is controlled at 10-30 seconds;
secondary pretreatment: using 8-40wt% sulfuric acid and 1-10 wt% hydrochloric acid mixed solution, adding a small amount of ferric chloride, wherein the ferric chloride content is 0.01-1g/L, the temperature is 30-60 ℃, and performing initial pitting treatment by adopting alternating current with the frequency of 50-100HZ and low power;
first-stage corrosion: using 8-40wt% sulfuric acid and 1-10 wt% hydrochloric acid mixed solution, at 50-80 deg.C, performing electrolytic corrosion in intermittent pulse power-on mode, cutting off power for 6 times, each power-on time being 13-23s, and cutting off power for 8s, and using direct current;
secondary corrosion: the corrosion solution is 1-10 wt% of nitric acid and corrosion inhibitor, the temperature is 30-80 ℃, direct current is adopted, and the current density is 0.05-0.2A/cm2；
And (3) post-treatment: 1-10 wt% of nitric acid is adopted, the temperature is 30-70 ℃, and the cleaning time is 1-5 minutes; then cleaning with pure water, and drying in an oven at 100 ℃.
2. The method of claim 1, wherein the etching step comprises: in the first-stage pretreatment, oil stains on the surface of the aluminum foil are removed by soaking for a short time.
3. The method of claim 1, wherein the etching step comprises: in the secondary pretreatment, a plurality of etching pits are formed in the area which is not easy to generate holes by adding metal ions and applying high-frequency low-electricity alternating current corrosion, so that the density and the uniformity of the etching pits are improved.
4. The method of claim 1, wherein the etching step comprises: in the first stage corrosion, the pulse energization mode is that the first energization for 3-8s in the first stage attenuates the current density from 1.5-1A/cm2 to 0.75-0.5A/cm2, and the second energization for 10-15s in the second stage attenuates the current density from 0.75-0.5A/cm2 to 0.2-0.01A/cm 2.
5. The method of claim 4, wherein the etching step comprises: in the pulse electrification, the high current density attenuation in the first stage promotes the generation of corrosion pits on the surface of the aluminum foil, the hole density on the surface of the aluminum foil is ensured, the attenuation process in the second stage provides energy for the continuous growth of holes, and the holes are ensured to grow to a certain length; the formation of adjacent holes was promoted by 7 intermittent energization with a continuous increase in the hole density.
6. The method of claim 1, wherein the etching step comprises: in the secondary corrosion, the corrosion inhibitor adopts a substance with larger molecular weight, and has good adsorption performance on the surface of the aluminum foil so as to achieve the corrosion inhibition effect; the current is preferably a small current.
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