CN118028798A - Preparation method of high-corrosion-resistance golden chromate conversion film of aluminum alloy - Google Patents
Preparation method of high-corrosion-resistance golden chromate conversion film of aluminum alloy Download PDFInfo
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- CN118028798A CN118028798A CN202211668837.4A CN202211668837A CN118028798A CN 118028798 A CN118028798 A CN 118028798A CN 202211668837 A CN202211668837 A CN 202211668837A CN 118028798 A CN118028798 A CN 118028798A
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- aluminum alloy
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- chromate conversion
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- 229910000838 Al alloy Inorganic materials 0.000 title claims abstract description 27
- 238000006243 chemical reaction Methods 0.000 title claims abstract description 27
- ZCDOYSPFYFSLEW-UHFFFAOYSA-N chromate(2-) Chemical compound [O-][Cr]([O-])(=O)=O ZCDOYSPFYFSLEW-UHFFFAOYSA-N 0.000 title claims abstract description 26
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- 238000004140 cleaning Methods 0.000 claims abstract description 39
- 230000007797 corrosion Effects 0.000 claims abstract description 26
- 238000005260 corrosion Methods 0.000 claims abstract description 26
- 239000003513 alkali Substances 0.000 claims abstract description 19
- 238000005498 polishing Methods 0.000 claims abstract description 19
- 238000000034 method Methods 0.000 claims abstract description 16
- 239000002253 acid Substances 0.000 claims abstract description 13
- 238000005238 degreasing Methods 0.000 claims abstract description 13
- 238000000861 blow drying Methods 0.000 claims abstract description 6
- 239000000463 material Substances 0.000 claims abstract description 6
- 239000000758 substrate Substances 0.000 claims abstract description 5
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 claims abstract description 4
- 239000002585 base Substances 0.000 claims abstract description 4
- 230000015572 biosynthetic process Effects 0.000 claims abstract description 4
- 229910052804 chromium Inorganic materials 0.000 claims abstract description 4
- 239000011651 chromium Substances 0.000 claims abstract description 4
- JOPOVCBBYLSVDA-UHFFFAOYSA-N chromium(6+) Chemical compound [Cr+6] JOPOVCBBYLSVDA-UHFFFAOYSA-N 0.000 claims abstract description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 20
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 18
- 238000005406 washing Methods 0.000 claims description 18
- 239000008367 deionised water Substances 0.000 claims description 14
- 229910021641 deionized water Inorganic materials 0.000 claims description 14
- 238000005554 pickling Methods 0.000 claims description 12
- 238000001035 drying Methods 0.000 claims description 11
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 6
- 238000005237 degreasing agent Methods 0.000 claims description 6
- 239000013527 degreasing agent Substances 0.000 claims description 6
- 229910017604 nitric acid Inorganic materials 0.000 claims description 6
- 230000035484 reaction time Effects 0.000 claims description 6
- 235000015510 Cucumis melo subsp melo Nutrition 0.000 claims description 3
- 244000137852 Petrea volubilis Species 0.000 claims description 3
- FJJCIZWZNKZHII-UHFFFAOYSA-N [4,6-bis(cyanoamino)-1,3,5-triazin-2-yl]cyanamide Chemical compound N#CNC1=NC(NC#N)=NC(NC#N)=N1 FJJCIZWZNKZHII-UHFFFAOYSA-N 0.000 claims description 3
- 230000002159 abnormal effect Effects 0.000 claims description 3
- 230000007547 defect Effects 0.000 claims description 3
- 238000001514 detection method Methods 0.000 claims description 3
- 239000004744 fabric Substances 0.000 claims description 3
- 238000000227 grinding Methods 0.000 claims description 3
- 239000003960 organic solvent Substances 0.000 claims description 3
- 238000007670 refining Methods 0.000 claims description 3
- 238000005507 spraying Methods 0.000 claims description 3
- 230000003746 surface roughness Effects 0.000 claims description 3
- 239000004094 surface-active agent Substances 0.000 claims description 3
- 238000004506 ultrasonic cleaning Methods 0.000 claims description 3
- 238000007744 chromate conversion coating Methods 0.000 claims 10
- 244000241257 Cucumis melo Species 0.000 claims 1
- 239000004065 semiconductor Substances 0.000 abstract description 7
- 238000004381 surface treatment Methods 0.000 abstract description 4
- FFRBMBIXVSCUFS-UHFFFAOYSA-N 2,4-dinitro-1-naphthol Chemical group C1=CC=C2C(O)=C([N+]([O-])=O)C=C([N+]([O-])=O)C2=C1 FFRBMBIXVSCUFS-UHFFFAOYSA-N 0.000 abstract description 2
- 239000000956 alloy Substances 0.000 abstract description 2
- 238000005034 decoration Methods 0.000 abstract description 2
- 238000005562 fading Methods 0.000 abstract description 2
- 229910052751 metal Inorganic materials 0.000 abstract description 2
- 239000002184 metal Substances 0.000 abstract description 2
- 230000001590 oxidative effect Effects 0.000 abstract description 2
- 150000003839 salts Chemical class 0.000 abstract description 2
- 239000007921 spray Substances 0.000 abstract description 2
- 241000219112 Cucumis Species 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000000356 contaminant Substances 0.000 description 1
- 238000005137 deposition process Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005530 etching Methods 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
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- Chemical Treatment Of Metals (AREA)
Abstract
The invention belongs to the technical field of IC semiconductor surface treatment, and particularly relates to a preparation method of an aluminum alloy high corrosion resistance golden chromate conversion film. The method comprises the steps of taking aluminum alloy as a base material, and performing pretreatment, golden chromate conversion film formation and post-treatment, wherein a film layer of the golden chromate conversion film is a chromate film layer composed of trivalent chromium and hexavalent chromium; the pretreatment comprises mechanical polishing, degreasing cleaning, rinsing, alkali cleaning and acid cleaning, and the post-treatment comprises rinsing, blow-drying and baking. Unlike insulating film layers produced by oxidizing the surfaces of other metal substrates, the film layer provided by the invention has the characteristic of low resistance, and the conductive performance of the part is not affected. The preparation method provided by the invention can greatly improve the corrosion resistance of the surface of the aluminum alloy material, no corrosion point is generated on the surface after 168 hours of salt spray test, the surface of the part is golden yellow, the color is bright and uniform, the binding force of the film layer is high, the fading and the like are not easy to occur, and the preparation method is suitable for improving the corrosion resistance of the aluminum alloy part and being used as decoration.
Description
Technical Field
The invention belongs to the technical field of IC semiconductor surface treatment, and particularly relates to a preparation method of an aluminum alloy high corrosion resistance golden chromate conversion film.
Background
The corrosion resistance of semiconductor materials in the IC field is very strict, and the corrosion resistance of semiconductor equipment parts is directly related to the quality of processed wafer products. The semiconductor device parts are made of aluminum alloy, and the aluminum alloy is subjected to a proper surface treatment process to ensure the ultra-high corrosion resistance. Low corrosion resistance devices or parts can result in the precipitation of large amounts of contaminants and other metal ions, which can have a significant impact on the etching or deposition process of semiconductor processing, and once encapsulated, can contaminate other vacuum connection cavities, resulting in greater losses. Therefore, improving the corrosion resistance of aluminum alloy parts is an important requirement for semiconductor materials.
Disclosure of Invention
In order to solve the technical problems, the invention provides a preparation method of an aluminum alloy high corrosion-resistant golden chromate conversion film.
The specific technical scheme is as follows:
the preparation method of the high corrosion resistant golden chromate conversion film of the aluminum alloy comprises the steps of taking the aluminum alloy as a base material, and performing pretreatment, golden chromate conversion film formation and post-treatment, wherein the film layer of the golden chromate conversion film is a chromate film layer composed of trivalent chromium and hexavalent chromium; the pretreatment comprises mechanical polishing, degreasing cleaning, rinsing, alkali cleaning and acid cleaning, and the post-treatment comprises rinsing, blow-drying and baking.
The pretreatment specifically comprises the following steps:
(1) Mechanical polishing, namely mechanically polishing and grinding the surface of the substrate until the surface roughness Ra is less than 0.8 mu m;
(2) Degreasing and cleaning: after mechanical polishing, confirming that the surface of the part has no abnormal problem, and cleaning the surface dirt by using a degreasing agent and controlling the temperature to be 40-70 ℃ and the cleaning time to be 5-10 minutes;
(3) Rinsing: rinsing with deionized water after degreasing and cleaning to remove surface dirt and residual degreasing agent;
(4) Alkali washing: placing the degreased and cleaned part in sodium hydroxide solution for alkali cleaning to remove an oxide layer on the surface of the part, washing the surface of the part with deionized water after alkali cleaning to remove residual alkali liquor of the part;
(5) Acid washing: placing the part in a nitric acid solution after alkali washing, pickling the surface of the part to remove surface oxides, spraying deionized water to the surface after pickling to remove residual acid, and removing residual acid in the through holes, blind holes and gaps by ultrasonic cleaning.
And (3) performing mechanical polishing, namely firstly performing primary polishing by using 600# sand paper until no macroscopic defect exists, and then refining surface grains by using melon cloth.
The degreasing cleaning in the step (2) can also be performed by cleaning with high-pressure water or cleaning the insides of the small hole stations with a steam gun.
And (3) after rinsing, the water film continuity detection is carried out twice, so that the surface of the part is clean and free of greasy dirt.
And (3) the concentration of the sodium hydroxide solution used in the alkaline washing in the step (4) is 50-200g/L, the alkaline washing is controlled at 20-45 ℃ and the reaction time is 10-60 seconds.
And (3) the nitric acid solution used in the pickling in the step (5) is 15-35% in concentration, and the pickling temperature is controlled to be 20-45 ℃.
The golden chromate conversion film is formed by the following specific steps:
Placing the pickled part in a solution composed of an organic solvent, inorganic chromate and a surfactant, and stirring the solution in the reaction process, wherein the temperature is controlled to be 15-30 ℃ and the reaction time is controlled to be 1-5 minutes. And after the reaction is finished, the surface of the part is rinsed by deionized water, and after the part is rinsed, the surface of the part is dried by clean compressed air, wherein the pressure of an air gun is controlled to be 10-30psi in the drying process, and the part is dried in an oven after the part is dried.
The post-treatment specifically comprises the following steps:
(1) Rinsing: rinsing the surface of the part by deionized water after the reaction is completed;
(2) Blow-drying: after the parts are washed clean, the surfaces of the parts are dried by clean compressed air, and the pressure of an air gun is controlled to be 10-30psi in the drying process;
(3) Baking: drying the parts in a drying oven after drying, and controlling the baking temperature to be 20-50 ℃.
Compared with the prior art, the invention has the following beneficial technical effects:
unlike insulating film layers produced by oxidizing the surfaces of other metal substrates, the film layer provided by the invention has the characteristic of low resistance, and the conductive performance of the part is not affected. The preparation method provided by the invention can greatly improve the corrosion resistance of the surface of the aluminum alloy material, no corrosion point is generated on the surface after 168 hours of salt spray test, the surface of the part is golden yellow, the color is bright and uniform, the binding force of the film layer is high, the fading and the like are not easy to occur, and the preparation method is suitable for improving the corrosion resistance of the aluminum alloy part and being used as decoration. Can effectively improve the corrosion resistance of the surface of the part. The golden chromate conversion film is a conductive oxide film layer, and is a better surface treatment mode for improving the service life of parts with the surface having conductive requirements.
Detailed Description
The present invention will be described in detail with reference to the following examples, but the scope of the present invention is not limited by the examples.
The preparation method of the high corrosion resistant golden chromate conversion film of the aluminum alloy comprises the steps of taking the aluminum alloy as a base material, and performing pretreatment, golden chromate conversion film formation and post-treatment, wherein the film layer of the golden chromate conversion film is a chromate film layer composed of trivalent chromium and hexavalent chromium; the pretreatment comprises mechanical polishing, degreasing cleaning, rinsing, alkali cleaning and acid cleaning, and the post-treatment comprises rinsing, blow-drying and baking.
The pretreatment specifically comprises the following steps:
(1) Mechanical polishing: in order to make the comprehensive performance of the prepared golden chromate conversion film better, firstly, mechanically polishing and grinding the surface of a substrate until the surface roughness Ra is less than 0.8 mu m;
(2) Degreasing and cleaning: after mechanical polishing, confirming that the surface of the part has no abnormal problem, and cleaning the surface dirt by using a degreasing agent and controlling the temperature to be 40-70 ℃ and the cleaning time to be 5-10 minutes;
(3) Rinsing: rinsing with deionized water after degreasing and cleaning to remove surface dirt and residual degreasing agent;
(4) Alkali washing: placing the degreased and cleaned part in sodium hydroxide solution for alkali cleaning to remove an oxide layer on the surface of the part, washing the surface of the part with deionized water after alkali cleaning to remove residual alkali liquor of the part;
(5) Acid washing: placing the part in a nitric acid solution after alkali washing, pickling the surface of the part to remove surface oxides, spraying deionized water to the surface after pickling to remove residual acid, and removing residual acid in the through holes, blind holes and gaps by ultrasonic cleaning.
And (3) performing mechanical polishing, namely firstly performing primary polishing by using 600# sand paper until no macroscopic defect exists, and then refining surface grains by using melon cloth.
The degreasing cleaning in the step (2) can also be performed by cleaning with high-pressure water or cleaning the insides of the small hole stations with a steam gun.
And (3) after rinsing, the water film continuity detection is carried out twice, so that the surface of the part is clean and free of greasy dirt.
And (3) the concentration of the sodium hydroxide solution used in the alkaline washing in the step (4) is 50-200g/L, the alkaline washing is controlled at 20-45 ℃ and the reaction time is 10-60 seconds.
And (3) the nitric acid solution used in the pickling in the step (5) is 15-35% in concentration, and the pickling temperature is controlled to be 20-45 ℃.
The golden chromate conversion film is formed by the following specific steps:
Placing the pickled part in a solution composed of an organic solvent, inorganic chromate and a surfactant, and stirring the solution in the reaction process, wherein the temperature is controlled to be 15-30 ℃ and the reaction time is controlled to be 1-5 minutes. And after the reaction is finished, the surface of the part is rinsed by deionized water, and after the part is rinsed, the surface of the part is dried by clean compressed air, wherein the pressure of an air gun is controlled to be 10-30psi in the drying process, and the part is dried in an oven after the part is dried.
Claims (9)
1. A preparation method of an aluminum alloy high corrosion resistance golden chromate conversion coating is characterized by comprising the following steps: the method comprises the steps of taking aluminum alloy as a base material, and performing pretreatment, golden chromate conversion film formation and post-treatment, wherein a film layer of the golden chromate conversion film is a chromate film layer composed of trivalent chromium and hexavalent chromium; the pretreatment comprises mechanical polishing, degreasing cleaning, rinsing, alkali cleaning and acid cleaning, and the post-treatment comprises rinsing, blow-drying and baking.
2. The method for preparing the high corrosion resistant golden chromate conversion coating of aluminum alloy according to claim 1, wherein the pretreatment comprises the following specific steps:
(1) Mechanical polishing, namely mechanically polishing and grinding the surface of the substrate until the surface roughness Ra is less than 0.8 mu m;
(2) Degreasing and cleaning: after mechanical polishing, confirming that the surface of the part has no abnormal problem, and cleaning the surface dirt by using a degreasing agent and controlling the temperature to be 40-70 ℃ and the cleaning time to be 5-10 minutes;
(3) Rinsing: rinsing with deionized water after degreasing and cleaning to remove surface dirt and residual degreasing agent;
(4) Alkali washing: placing the degreased and cleaned part in sodium hydroxide solution for alkali cleaning to remove an oxide layer on the surface of the part, washing the surface of the part with deionized water after alkali cleaning to remove residual alkali liquor of the part;
(5) Acid washing: placing the part in a nitric acid solution after alkali washing, pickling the surface of the part to remove surface oxides, spraying deionized water to the surface after pickling to remove residual acid, and removing residual acid in the through holes, blind holes and gaps by ultrasonic cleaning.
3. The method for preparing the high corrosion resistant golden chromate conversion coating of aluminum alloy according to claim 1, wherein the method comprises the following steps: and (3) performing mechanical polishing, namely firstly performing primary polishing by using 600# sand paper until no macroscopic defect exists, and then refining surface grains by using melon cloth.
4. The method for preparing the high corrosion resistant golden chromate conversion coating of aluminum alloy according to claim 1, wherein the method comprises the following steps: the degreasing cleaning in the step (2) can also be performed by cleaning with high-pressure water or cleaning the insides of the small hole stations with a steam gun.
5. The method for preparing the high corrosion resistant golden chromate conversion coating of aluminum alloy according to claim 1, wherein the method comprises the following steps: and (3) after rinsing, the water film continuity detection is carried out twice, so that the surface of the part is clean and free of greasy dirt.
6. The method for preparing the high corrosion resistant golden chromate conversion coating of aluminum alloy according to claim 1, wherein the method comprises the following steps: and (3) the concentration of the sodium hydroxide solution used in the alkaline washing in the step (4) is 50-200g/L, the alkaline washing is controlled at 20-45 ℃ and the reaction time is 10-60 seconds.
7. The method for preparing the high corrosion resistant golden chromate conversion coating of aluminum alloy according to claim 1, wherein the method comprises the following steps: and (3) the nitric acid solution used in the pickling in the step (5) is 15-35% in concentration, and the pickling temperature is controlled to be 20-45 ℃.
8. The method for preparing the high corrosion resistant golden chromate conversion coating of aluminum alloy according to claim 1, wherein the golden chromate conversion coating is formed by the following steps:
Placing the pickled part in a solution composed of an organic solvent, inorganic chromate and a surfactant, wherein the solution needs to be stirred in the reaction process, the temperature is controlled to be 15-30 ℃, and the reaction time is controlled to be 1-5 minutes; and after the reaction is finished, the surface of the part is rinsed by deionized water, and after the part is rinsed, the surface of the part is dried by clean compressed air, wherein the pressure of an air gun is controlled to be 10-30psi in the drying process, and the part is dried in an oven after the part is dried.
9. The method for preparing the high corrosion resistant golden chromate conversion coating of aluminum alloy according to claim 1, wherein the post-treatment comprises the following steps:
(1) Rinsing: rinsing the surface of the part by deionized water after the reaction is completed;
(2) Blow-drying: after the parts are washed clean, the surfaces of the parts are dried by clean compressed air, and the pressure of an air gun is controlled to be 10-30psi in the drying process;
(3) Baking: drying the parts in a drying oven after drying, and controlling the baking temperature to be 20-50 ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211668837.4A CN118028798A (en) | 2022-12-24 | 2022-12-24 | Preparation method of high-corrosion-resistance golden chromate conversion film of aluminum alloy |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211668837.4A CN118028798A (en) | 2022-12-24 | 2022-12-24 | Preparation method of high-corrosion-resistance golden chromate conversion film of aluminum alloy |
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| Publication Number | Publication Date |
|---|---|
| CN118028798A true CN118028798A (en) | 2024-05-14 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202211668837.4A Pending CN118028798A (en) | 2022-12-24 | 2022-12-24 | Preparation method of high-corrosion-resistance golden chromate conversion film of aluminum alloy |
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| Country | Link |
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| CN (1) | CN118028798A (en) |
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2022
- 2022-12-24 CN CN202211668837.4A patent/CN118028798A/en active Pending
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