CN114592226A - Preparation process of high-density anode film suitable for Display Dry Etcher - Google Patents
Preparation process of high-density anode film suitable for Display Dry Etcher Download PDFInfo
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- CN114592226A CN114592226A CN202210219536.7A CN202210219536A CN114592226A CN 114592226 A CN114592226 A CN 114592226A CN 202210219536 A CN202210219536 A CN 202210219536A CN 114592226 A CN114592226 A CN 114592226A
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- 238000002360 preparation method Methods 0.000 title claims abstract description 7
- 238000000034 method Methods 0.000 claims abstract description 21
- 239000003792 electrolyte Substances 0.000 claims abstract description 16
- 239000000463 material Substances 0.000 claims abstract description 15
- 230000000630 rising effect Effects 0.000 claims abstract description 15
- 238000007743 anodising Methods 0.000 claims abstract description 5
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims description 33
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 27
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 13
- 229910052782 aluminium Inorganic materials 0.000 claims description 13
- 235000006408 oxalic acid Nutrition 0.000 claims description 11
- 238000005406 washing Methods 0.000 claims description 11
- 239000002253 acid Substances 0.000 claims description 10
- 239000002585 base Substances 0.000 claims description 10
- 238000005238 degreasing Methods 0.000 claims description 10
- 239000003513 alkali Substances 0.000 claims description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- 238000004519 manufacturing process Methods 0.000 claims description 4
- 238000007781 pre-processing Methods 0.000 claims description 4
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical group O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 3
- 239000012530 fluid Substances 0.000 claims description 3
- 229910017604 nitric acid Inorganic materials 0.000 claims description 3
- 238000005498 polishing Methods 0.000 claims description 3
- 230000003746 surface roughness Effects 0.000 claims description 3
- 238000002203 pretreatment Methods 0.000 claims 3
- 239000012528 membrane Substances 0.000 claims 2
- 238000002048 anodisation reaction Methods 0.000 claims 1
- 230000003647 oxidation Effects 0.000 abstract description 8
- 238000007254 oxidation reaction Methods 0.000 abstract description 8
- 239000000758 substrate Substances 0.000 abstract description 4
- 230000007547 defect Effects 0.000 abstract description 3
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 4
- 230000007797 corrosion Effects 0.000 description 4
- 238000005260 corrosion Methods 0.000 description 4
- 238000005530 etching Methods 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000004519 grease Substances 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
- C25D11/02—Anodisation
- C25D11/04—Anodisation of aluminium or alloys based thereon
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
- C25D11/02—Anodisation
- C25D11/04—Anodisation of aluminium or alloys based thereon
- C25D11/06—Anodisation of aluminium or alloys based thereon characterised by the electrolytes used
- C25D11/10—Anodisation of aluminium or alloys based thereon characterised by the electrolytes used containing organic acids
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
- C25D11/02—Anodisation
- C25D11/04—Anodisation of aluminium or alloys based thereon
- C25D11/16—Pretreatment, e.g. desmutting
Abstract
The invention discloses a preparation process of a high-density anode film suitable for Display Dry Etcher, which belongs to the technical field of an upper electrode anodic oxidation process, and comprises the steps of firstly preparing electrolyte and then pretreating a base material; and finally, anodizing the base material by adopting a segmented current rising mode, wherein a rectification mode is carried out by adopting a direct current and alternating current plus pulse mode, the alternating current output time is 0-300 s, the direct current output time is 0-300 s, and the output time of pulse current is 0-100 s, wherein the direct current and the alternating current are alternately output, and the pulse current is simultaneously superposed according to a set frequency, wherein the output proportion range of the alternating current is 30-50%, the output proportion range of the direct current is 70-50%, the frequencies of the alternating current and the direct current are both 50 HZ-100 HZ, and the frequency of the pulse is 50-100 HZ. The process can ensure to obtain the anode film with good performance, and can improve the defect of weak combination of the substrate and the anode film on local (particularly chamfer) parts of the product.
Description
Technical Field
The invention belongs to the technical field of an anodic oxidation process of an upper electrode, and particularly relates to a preparation process of a high-density anode film suitable for Display Dry Etcher.
Background
The upper electrode is used for uniformly dispersing Plasma in the Etcher process on the glass substrate through the electrode holes, when Plasma gas is dispersed on the glass substrate through the 0.4 hole diameter on the upper electrode, the gas is corrosive, and the upper electrode is made of aluminum material, so that the upper electrode is required to be subjected to anode treatment in advance, and the corrosion resistance of the product is improved. With the increasing demand of the Display market for large-size and high-quality products, the corrosion resistance and voltage resistance of the upper electrode are also promoted to meet the requirements of customers. At present, the anode process of the upper electrode comprises a sulfuric acid method (using a DC rectifier), a mixed acid method (adding oxalic acid into sulfuric acid) and the like, but an anode film prepared by an oxalic acid solution has the problem of easy peeling, and is particularly obvious at the chamfer part of a product.
Disclosure of Invention
In view of the above, the present invention provides a high density anode film manufacturing process suitable for Display Dry Etcher, which can solve the above technical problems.
In order to achieve the purpose, the invention provides the following technical scheme:
the invention relates to a preparation process of a high-density anode film suitable for Display Dry Etcher, which comprises the following steps:
s1, preparing electrolyte, wherein the electrolyte comprises oxalic acid, citric acid and pure water;
s2, preprocessing, namely preprocessing the base material;
s3, anodizing the base material by adopting a segmented current rising mode, rectifying by adopting a direct current and alternating current plus pulse mode, wherein the alternating current output time is 0-300S, the direct current output time is 0-300S, and the output time of pulse current is 0-100S, the direct current and the alternating current are alternately output, and the pulse current is simultaneously superposed according to a set frequency, wherein the output proportion range of the alternating current is 30-50%, the output proportion range of the direct current is 70-50%, the frequencies of the alternating current and the direct current are both 50 HZ-100 HZ, and the frequency of the pulse is 50-100 HZ.
Further, the segmented rising flow manner in step S3 includes four stages, and the setting conditions in the first stage are: the current density is 0-0.5A/dm2The rising time is 10s, and the steady flow time is 290 s; the setting conditions of the second stage are as follows: the current density is 0.5 to 1.0A/dm2The rising time is 10s, the steady flow time is 290s, and the setting conditions of the third stage are as follows: the current density is 1.0-1.5A/dm2The rising time is 10s, the steady flow time is 290s, and the setting conditions of the fourth stage are as follows: the current density is 1.5-2.0A/dm2The rise time was 10s and the stationary flow time was 5690 s.
Further, in the anodic oxidation, the ratio of the surface area of the cathode to the surface area of the anode is 2: 1-3: 1.
further, in step S1, the concentration of oxalic acid is 5% to 10%, and the concentration of citric acid is 1% to 5%.
Further, the temperature of the electrolyte in the anodic oxidation process is controlled to be less than 25 ℃.
Further, the pretreatment process is as follows: polishing an aluminum test piece, degreasing, washing, treating in an alkali tank, washing, treating in an acid tank and washing.
Further, in the pretreatment process, the surface roughness Ra of the polished aluminum test piece is less than 0.4; the degreasing fluid is NP-8, and the concentration is 4-10 g/L; the degreasing treatment time is 5-10 min.
Further, in the pretreatment process, the solution treated by the alkali tank is an NAOH solution with the concentration of 15-30 g/L, the alkali tank is treated for 10-15 min, the solution treated by the acid tank is nitric acid with the concentration of 200-400 g/L, and the acid tank is treated for 5-10 min.
The invention has the beneficial effects that:
the invention is suitable for the preparation process of the high-density anode film of Display Dry Etcher, the rectification mode is changed from the common DC to the mode of DC + AC + pulse, the rectification mode can ensure to obtain the anode film with good performance, and the defect of weak combination of the substrate on the local part (particularly the chamfer) of the product and the anode film can be improved.
Additional advantages, objects, and features of the invention will be set forth in the description which follows and in part will become apparent to those having ordinary skill in the art upon examination of the following or may be learned from practice of the invention. The objectives and other advantages of the invention may be realized and attained by the means of the instrumentalities and combinations particularly pointed out hereinafter.
Drawings
In order to make the object, technical scheme and beneficial effect of the invention more clear, the invention provides the following drawings for explanation:
FIG. 1 is a diagram showing the superposition of alternating current and direct current and the pulse according to the present invention; (ii) a
FIG. 2 is a schematic illustration of the staged upflow of the present invention;
FIG. 3 is an SEM image of the anodic film of example 1.
Detailed Description
Example 1: the embodiment 1 of the invention comprises the following steps: and S1, preparing an electrolyte, wherein the electrolyte comprises oxalic acid, citric acid and pure water.
S2, pre-treating, and pre-treating the base material to obtain an ideal aluminum test piece.
S3, anodizing, wherein the cathode plate is made of an aluminum plate, and the surface area ratio of the cathode to the anode is 2: 1-3: 1. the method comprises the steps of carrying out anodic oxidation on a base material by adopting a segmented current rising mode, carrying out rectification by adopting a direct current and alternating current plus pulse mode, wherein the alternating current output time is 0-300 s, the direct current output time is 0-300 s, and the output time of pulse current is 0-100 s, wherein the direct current and alternating current are alternately output, and the pulse current is simultaneously superposed according to a set frequency, wherein the output proportion range of the alternating current is 30-50%, the output proportion range of the direct current is 70-50%, the output proportion refers to the ratio of the direct current to the alternating current in a rated current, the frequency of the alternating current and the direct current is 50-100 HZ, and the frequency of the pulse is 50-100 HZ.
Example 2: the embodiment 2 of the invention comprises the following steps: s1, preparing an electrolyte, wherein the electrolyte comprises oxalic acid, citric acid and pure water, the concentration of the oxalic acid is 5% -10%, the concentration of the citric acid is 1-5%, and the temperature of the electrolyte in the anodic oxidation process is controlled to be not more than 25 ℃.
S2, pretreatment, namely, carrying out pretreatment on the base material, and sequentially polishing, degreasing, washing, treating in an alkali tank, washing, treating in an acid tank and washing. The surface roughness Ra of the polished aluminum test piece is less than 0.4, the surface can not have obvious scratches and the like, and the effect of a long film is prevented from being influenced by the surface defects of the base material; the degreasing fluid is NP-8, and the concentration is 4-10 g/L; the degreasing treatment time is 5-10 min. Impurities such as grease on the surface of the test piece are removed, and then washing is performed. And after degreasing, carrying out alkali etching treatment, wherein the solution treated in an alkali tank is an NAOH solution with the concentration of 15-30 g/L, treating in the alkali tank for 10-15 min, removing impurities such as Smut on the surface of the test piece, and then washing with water. After the alkali etching treatment, acid etching treatment is performed. The solution treated in the acid tank is nitric acid with the concentration of 200-400 g/L, and the acid tank is used for treating for 5-10 min. The Desmut component on the aluminum coupon was removed and washed with water. An ideal aluminum test piece can be obtained.
S3, anodizing, wherein the cathode plate is made of an aluminum plate, and the surface area ratio of the cathode to the anode is 2: 1-3: 1. carrying out anodic oxidation on the base material by adopting a sectional upflow mode, controlling the oxidation current, wherein the sectional upflow mode comprises four stages, and the setting conditions of the first stage are as follows: the current density is 0-0.5A/dm 2, the rising time is 10s, and the steady flow time is 290 s; the setting conditions of the second stage are as follows: the current density is 0.5-1.0A/dm 2, the rising time is 10s, the steady flow time is 290s, and the setting conditions of the third stage are as follows: the current density is 1.0-1.5A/dm 2, the rising time is 10s, the steady flow time is 290s, and the setting conditions of the fourth stage are as follows: the current density is 1.5-2.0A/dm 2, the rising time is 10s, and the steady flow time is 5690 s.
The rectification mode is carried out by adopting a direct current and alternating current plus pulse mode, the alternating current output time is 0-300 s, the direct current output time is 0-300 s, and the output time of pulse current is 0-100 s, wherein the direct current and the alternating current are alternately output, and the pulse current is simultaneously superposed according to a set frequency, wherein the output proportion range of the alternating current is 30-50%, the output proportion range of the direct current is 70-50%, the frequencies of the alternating current and the direct current are both 50 HZ-100 HZ, and the frequency of the pulse is 50-100 HZ.
Example 3: the embodiment 3 of the invention comprises the following steps: and S1, preparing an electrolyte, wherein the electrolyte comprises oxalic acid, citric acid and pure water.
S2, pretreatment, the base material is pretreated to obtain the ideal aluminum test piece.
S3: the rectification mode adopts a single DC rectification mode.
Example 4:
the embodiment 4 of the invention comprises the following steps: and S1, preparing an electrolyte, wherein the electrolyte comprises oxalic acid, citric acid and pure water.
S2, pretreatment, the base material is pretreated to obtain the ideal aluminum test piece.
S3: the rectification mode adopts a single AC rectification mode.
FIG. 3 is a thickness chart of the anodic film obtained by SEM in example 1, and the film length at the R-chamfer is uniform and the film is well bonded to the base material as seen from the SEM screen shot. For examples 3 and 4, the original rectification mode was DC mode or AC rectification, and the film thickness at the horizontal part of the perforated product was larger than the film thickness at the R corner and in the hole wall, and the anode film at the corner was very likely to peel off. According to the invention, through the adjustment of the AC/DC pulse mode, the problem of uneven film thickness of the perforated product can be well solved, a product with higher quality can be provided, the weak part on the product is improved, and the corrosion resistance is improved by 30%. Compared with the embodiment 1, the embodiment 2 can further improve the compactness problem of the anode film at the weak part of the product, so that the corrosion resistance is improved by 2-5%.
Finally, it is noted that the above-mentioned preferred embodiments illustrate rather than limit the invention, and that, although the invention has been described in detail with reference to the above-mentioned preferred embodiments, it will be understood by those skilled in the art that various changes in form and detail may be made therein without departing from the scope of the invention as defined by the appended claims.
Claims (8)
1. The preparation process of the high-density anode film suitable for Display Dry Etcher is characterized by comprising the following steps of:
s1, preparing an electrolyte, wherein the electrolyte comprises oxalic acid, citric acid and pure water;
s2, preprocessing, namely preprocessing the base material;
s3, anodizing the base material by adopting a segmented current rising mode, rectifying by adopting a direct current and alternating current plus pulse mode, wherein the alternating current output time is 0-300S, the direct current output time is 0-300S, and the output time of pulse current is 0-100S, the direct current and the alternating current are alternately output, and the pulse current is simultaneously superposed according to a set frequency, wherein the output proportion range of the alternating current is 30-50%, the output proportion range of the direct current is 70-50%, the frequencies of the alternating current and the direct current are both 50 HZ-100 HZ, and the frequency of the pulse is 50-100 HZ.
2. The process of claim 1, wherein the staged up-flow mode in step S3 includes four stages, and the conditions for the first stage are as follows: the current density is 0-0.5A/dm2The rising time is 10s, and the steady flow time is 290 s; the setting conditions of the second stage are as follows: the current density is 0.5 to 1.0A/dm2The rising time is 10s, the steady flow time is 290s, and the setting conditions of the third stage are as follows: the current density is 1.0-1.5A/dm2The rising time is 10s, the steady flow time is 290s, and the setting conditions of the fourth stage are as follows: the current density is 1.5-2.0A/dm2The rise time was 10s and the stationary flow time was 5690 s.
3. The process of claim 2, wherein the ratio of the surface areas of the anode and the cathode is 2: 1-3: 1.
4. the process for preparing a high-density anode membrane suitable for Display Dry Etcher as claimed in claim 3, wherein in step S1, the concentration of oxalic acid is 5-10% and the concentration of citric acid is 1-5%.
5. The process of claim 4, wherein the temperature of the electrolyte during the anodization process is controlled to be less than 25 ℃.
6. The process of claim 5, wherein the pre-treatment process comprises: polishing an aluminum test piece, degreasing, washing, treating in an alkali tank, washing, treating in an acid tank and washing.
7. The process for preparing a high-density anode film suitable for Display Dry Etcher as claimed in claim 6, wherein the surface roughness Ra of the polished aluminum coupon during the pre-treatment process is less than 0.4; the degreasing fluid is NP-8, and the concentration is 4-10 g/L; the degreasing treatment time is 5-10 min.
8. The process for preparing a high-density anode membrane suitable for Display Dry Etcher as claimed in claim 7, wherein in the pre-treatment process, the solution treated in the alkaline tank is a NAOH solution with a concentration of 15-30 g/L for 10-15 min, the solution treated in the acid tank is nitric acid with a concentration of 200-400 g/L for 5-10 min.
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Cited By (1)
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CN114808075A (en) * | 2022-05-27 | 2022-07-29 | 重庆臻宝实业有限公司 | Method for preparing anode film layer with plasma corrosion resistance and low gas overflow amount |
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