CN1278462A - Method of coating sol-gel onto surface of easy-to-oxidize metal - Google Patents
Method of coating sol-gel onto surface of easy-to-oxidize metal Download PDFInfo
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- CN1278462A CN1278462A CN 00109801 CN00109801A CN1278462A CN 1278462 A CN1278462 A CN 1278462A CN 00109801 CN00109801 CN 00109801 CN 00109801 A CN00109801 A CN 00109801A CN 1278462 A CN1278462 A CN 1278462A
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- Prior art keywords
- sol
- base material
- coating
- metal base
- coated
- Prior art date
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- 229910052751 metal Inorganic materials 0.000 title claims abstract description 30
- 239000002184 metal Substances 0.000 title claims abstract description 30
- 238000000034 method Methods 0.000 title claims abstract description 4
- 239000011248 coating agent Substances 0.000 title abstract description 29
- 238000000576 coating method Methods 0.000 title abstract description 29
- 230000003647 oxidation Effects 0.000 claims abstract description 24
- 238000007254 oxidation reaction Methods 0.000 claims abstract description 24
- 239000000463 material Substances 0.000 claims abstract description 16
- 239000012298 atmosphere Substances 0.000 claims abstract description 11
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 16
- 238000004506 ultrasonic cleaning Methods 0.000 claims description 16
- 239000000758 substrate Substances 0.000 claims description 14
- 238000003980 solgel method Methods 0.000 claims description 10
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 8
- 238000005202 decontamination Methods 0.000 claims description 8
- 230000003588 decontaminative effect Effects 0.000 claims description 8
- 239000012153 distilled water Substances 0.000 claims description 8
- 238000011010 flushing procedure Methods 0.000 claims description 8
- 238000010792 warming Methods 0.000 claims description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 2
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 2
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 claims description 2
- 239000004411 aluminium Substances 0.000 claims description 2
- 229910052782 aluminium Inorganic materials 0.000 claims description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 2
- 239000005002 finish coating Substances 0.000 claims description 2
- 239000010936 titanium Substances 0.000 claims description 2
- 229910052719 titanium Inorganic materials 0.000 claims description 2
- 229910052726 zirconium Inorganic materials 0.000 claims description 2
- 238000005260 corrosion Methods 0.000 abstract description 11
- 230000007797 corrosion Effects 0.000 abstract description 11
- 238000010438 heat treatment Methods 0.000 abstract description 9
- 239000011247 coating layer Substances 0.000 abstract 2
- 238000004140 cleaning Methods 0.000 abstract 1
- 238000001816 cooling Methods 0.000 abstract 1
- 238000001035 drying Methods 0.000 abstract 1
- 239000012535 impurity Substances 0.000 abstract 1
- 229910000851 Alloy steel Inorganic materials 0.000 description 12
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 12
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 12
- 239000002585 base Substances 0.000 description 12
- 229910052802 copper Inorganic materials 0.000 description 12
- 239000010949 copper Substances 0.000 description 12
- 239000011159 matrix material Substances 0.000 description 10
- 229910000975 Carbon steel Inorganic materials 0.000 description 7
- 239000010962 carbon steel Substances 0.000 description 7
- 238000009413 insulation Methods 0.000 description 7
- 230000003026 anti-oxygenic effect Effects 0.000 description 6
- 229910052786 argon Inorganic materials 0.000 description 6
- 229910000831 Steel Inorganic materials 0.000 description 5
- 239000010959 steel Substances 0.000 description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- 229910010413 TiO 2 Inorganic materials 0.000 description 4
- 239000012299 nitrogen atmosphere Substances 0.000 description 4
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- 229960004424 carbon dioxide Drugs 0.000 description 2
- 229910002090 carbon oxide Inorganic materials 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 125000004435 hydrogen atom Chemical class [H]* 0.000 description 2
- 239000011261 inert gas Substances 0.000 description 2
- 239000007769 metal material Substances 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 125000004430 oxygen atom Chemical group O* 0.000 description 2
- 229910004298 SiO 2 Inorganic materials 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 150000004703 alkoxides Chemical class 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 125000004429 atom Chemical group 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 238000005524 ceramic coating Methods 0.000 description 1
- 229910052809 inorganic oxide Inorganic materials 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000011253 protective coating Substances 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
Landscapes
- Other Surface Treatments For Metallic Materials (AREA)
Abstract
The method for coating oxidable metal surface with sol-gel includes the following steps: cleaning oxidable metal base material, removing impurities, uniformly applying sol whose thickness is 0.1-1 micrometer on the metal base plate, drying under the condition of room temp. and atmosphere, placing the oxidable metal base material coated with sol in vacuum or atmosphere protection furnace, for heating and implementing heat-treatment, cooling to room temp. to obtain the invented smooth, compact, crack-free, high-quality and high cohesion strength coating layer on the metal base material. Said coating layer can obviously raise resistance to corrosion and resistance to oxidation of metal base material.
Description
The present invention relates to a kind of sol-gel process, belong to metal material protection field in the easy oxidation metal surface-coated.
In metal surface coated ceramic coating,, carried out research and development to a certain degree abroad by sol-gel process with the corrosion and the oxidation of opposing medium (acid, alkali, salt, atmosphere) to metallic matrix.The coating that protection is used to metal substrate has Al
2O
3Deng (referring to " solid film " 1999 349 volumes 186-190 page or leaf); under certain condition, the protective coating that sol-gel process applies can improve that metal is corrosion-resistant, oxidation resistance reaches 2～8 times, therefore; prolong the service life of material, and then brought great economic benefit.
But above-mentioned sol-gel process only is applicable to metal materials such as stainless steel itself that have resistance to oxidation character, nickel-base alloy, and is then inapplicable for metals such as the carbon steel of easy oxidation, low-alloy steel, copper.Because coating need be heat-treated, and during heating treatment, oxidation can take place matrix, cause coating discontinuous, do not adhere to, easily come off.
The objective of the invention is to propose a kind of sol-gel process in the easy oxidation metal surface-coated, adopt sol-gel process on the easy oxidation metal base material, to apply to have the inorganic coating of excellent surface quality and high bond strength, and then corrosion-resistant, the oxidation resistance of raising metal.
The sol-gel process in the easy oxidation metal surface-coated that the present invention proposes comprises following each step::
(1) to easy oxidation metal base material (comprising carbon steel, low-alloy steel, copper etc.) clean, decontamination.Matting is: ultrasonic cleaning 15min in the acetone, use distilled water ultrasonic cleaning 15min then, and use alcohol flushing again, use dry-air blower rapid draing at last.
(2) even Ludox, titanium colloidal sol, aluminium colloidal sol, zirconium colloidal sol or the complex sol that applies 0.1～1 μ m thickness on metal substrate.
(3) behind dry 1h under room temperature, the atmosphere; the easy oxidation metal base material that is coated with colloidal sol is placed vacuum or atmosphere (inert gases such as hydrogen, nitrogen and argon gas) protection stove; be warming up to 400～1000 ℃ to be not more than 40 ℃/min speed; insulation 1～6h; heat-treat; cool to room temperature then with the furnace, promptly finish coating the metal surface.
Adopt process of the present invention to apply smooth, fine and close, flawless coating with great surface quality on the easy oxidation metal substrate, this coating and matrix have high bond strength, can significantly improve corrosion-resistant, the non-oxidizability of metallic matrix.
Content of the present invention: it is to be the characteristic of predecessor with the metal alkoxide that the present invention makes full use of sol-gel process, itself just contains enough oxygen atoms these predecessors, under oxygen in not having atmosphere participates in, during heat treatment, the oxygen atom that is contained in the predecessor can directly combine with metallic atom, generate the oxide coating of being expected, thereby, form fine and close, uniform inorganic coating on the easy oxidation metal surface.Therefore, the present invention is to easy oxidation metal, and the inorganic oxide coating that can obtain expecting is heat-treated in employing (inert gas shieldings such as vacuum or hydrogen, nitrogen and argon gas) in oxygen-free atmosphere.
Embodiment one:
Commute oxidation low alloy steel plate cleans, decontamination, and matting is: ultrasonic cleaning 15min in the acetone, use distilled water ultrasonic cleaning 15min then, and use alcohol flushing again, use dry-air blower rapid draing at last.
Apply 1 μ m thickness SiO at surface of low-alloy steel
2Colloidal sol.To be coated with SiO
2The low-alloy steel base material of colloidal sol places the nitrogen atmosphere protection stove, is warming up to 400 ℃ with 5 ℃/min speed, and insulation 6h heat-treats, and cools to room temperature then with the furnace.Obtain being coated on the SiO on the low-alloy steel substrate
2Coating.
After the nitrogen atmosphere protection heat treatment, the SiO that surface of low-alloy steel applies
2Coating is smooth, fine and close, flawless, and coating and substrate combinating strength reach 40Mpa, and corrosion-resistant comparing with uncoated matrix with antioxygenic property improved 8.7 and 6.8 times respectively.
Embodiment two:
Commute oxidation copper coin cleans, decontamination, and matting is: ultrasonic cleaning 15min in the acetone, use distilled water ultrasonic cleaning 15min then, and use alcohol flushing again, use dry-air blower rapid draing at last.
At copper coin surface-coated 0.8 μ m thickness A l
2O
3Colloidal sol.To be coated with Al
2O
3The copper base material of colloidal sol places argon atmospher protection stove, is warming up to 500 ℃ with 10 ℃/min speed, and insulation 5h heat-treats, and cools to room temperature then with the furnace.Obtain being coated on the Al on the copper base
2O
3Coating.
After the argon atmospher protection heat treatment, the Al of copper surface-coated
20
3Coating is smooth, fine and close, flawless, and coating and substrate combinating strength reach 28Mpa, and corrosion-resistant comparing with uncoated matrix with antioxygenic property improved 3.3 and 4.1 times respectively.
Embodiment three:
Commute carbonoxide steel plate cleans, decontamination, and matting is: ultrasonic cleaning 15min in the acetone, use distilled water ultrasonic cleaning 15min then, and use alcohol flushing again, use dry-air blower rapid draing at last.
Apply 0.6 μ m thickness Z rO at steel surface
2Colloidal sol.To be coated with ZrO
2The carbon steel base material of colloidal sol places the vacuum protection stove, is warming up to 600 ℃ with 15 ℃/min speed, and insulation 4h heat-treats, and cools to room temperature then with the furnace.Obtain being coated on the ZrO on the carbon steel substrate
2Coating.
After the vacuum heat, the ZrO that steel surface applies
2Coating is smooth, fine and close, flawless, and coating and substrate combinating strength reach 35Mpa, and corrosion-resistant comparing with uncoated matrix with antioxygenic property improved 6.3 and 5.0 times respectively.
Embodiment four:
Commute oxidation low alloy steel plate cleans, decontamination, and matting is: ultrasonic cleaning 15min in the acetone, use distilled water ultrasonic cleaning 15min then, and use alcohol flushing again, use dry-air blower rapid draing at last.
Apply 0.4 μ m thickness SiO at surface of low-alloy steel
2-Al
2O
3Colloidal sol.To be coated with SiO
2-Al
2O
3The low-alloy steel base material of colloidal sol places argon atmospher protection stove, is warming up to 700 ℃ with 20 ℃/min speed, and insulation 3h heat-treats, and cools to room temperature then with the furnace.Obtain being coated on the SiO on the low-alloy steel substrate
2-Al
2O
3Coating.
After the argon atmospher protection heat treatment, the SiO that surface of low-alloy steel applies
2-Al
2O
3Coating is smooth, fine and close, flawless, and coating and substrate combinating strength reach 35Mpa, and corrosion-resistant comparing with uncoated matrix with antioxygenic property improved 5.2 and 3.1 times respectively.
Embodiment five:
Commute carbonoxide steel plate cleans, decontamination, and matting is: ultrasonic cleaning 15min in the acetone, use distilled water ultrasonic cleaning 15min then, and use alcohol flushing again, use dry-air blower rapid draing at last.
Apply 0.2 μ m thickness SiO at steel surface
2-TiO
2Colloidal sol.To be coated with SiO
2-TiO
2The carbon steel base material of colloidal sol places helium-atmosphere protection stove, is warming up to 800 ℃ with 30 ℃/min speed, and insulation 2h heat-treats, and cools to room temperature then with the furnace.Obtain being coated on the SiO on the carbon steel substrate
2-TiO
2Coating.
After the helium-atmosphere protection heat treatment, the SiO of carbon steel sheet surface-coated
2-TiO
2Coating is smooth, fine and close, flawless, and coating and substrate combinating strength reach 22Mpa, and corrosion-resistant comparing with uncoated matrix with antioxygenic property improved 3.6 and 4.5 times respectively.
Embodiment six:
Commute oxidation copper coin cleans, decontamination, and matting is: ultrasonic cleaning 15min in the acetone, use distilled water ultrasonic cleaning 15min then, and use alcohol flushing again, use dry-air blower rapid draing at last.
At copper coin surface-coated 0.1 μ m thickness SiO
2-ZrO
2Colloidal sol.To be coated with SiO
2-ZrO
2The copper base material of colloidal sol places the nitrogen atmosphere protection stove, is warming up to 1000 ℃ with 40 ℃/min speed, and insulation 1h heat-treats, and cools to room temperature then with the furnace.Obtain being coated on the SiO on the copper base
2-ZrO
2Coating.
After the nitrogen atmosphere protection heat treatment, the SiO of copper surface-coated
2-ZrO
2Coating is smooth, fine and close, flawless, and coating and substrate combinating strength reach 18Mpa, and corrosion-resistant comparing with uncoated matrix with antioxygenic property improved 2.2 and 3.4 times respectively.
Claims (1)
1, a kind of sol-gel process in the easy oxidation metal surface-coated is characterized in that, this method comprises following each step:
(1) to the easy oxidation metal base material clean, decontamination, matting is: ultrasonic cleaning is 15 minutes in the acetone, uses the distilled water ultrasonic cleaning then 15 minutes, uses alcohol flushing again, uses dry-air blower rapid draing at last;
(2) even Ludox, titanium colloidal sol, aluminium colloidal sol, zirconium colloidal sol or the wherein any two kinds complex sol that applies 0.1～1 μ m thickness on metal substrate;
(3) after under room temperature, the atmosphere dry 1 hour; the easy oxidation metal base material that is coated with colloidal sol is placed vacuum or atmosphere protection stove; be warming up to 400～1000 ℃ to be lower than 40 ℃ of/minute clock rate; be incubated 1～6 hour; heat-treat; cool to room temperature then with the furnace, promptly finish coating the metal surface.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 00109801 CN1278462A (en) | 2000-07-07 | 2000-07-07 | Method of coating sol-gel onto surface of easy-to-oxidize metal |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 00109801 CN1278462A (en) | 2000-07-07 | 2000-07-07 | Method of coating sol-gel onto surface of easy-to-oxidize metal |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN1278462A true CN1278462A (en) | 2001-01-03 |
Family
ID=4579872
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 00109801 Pending CN1278462A (en) | 2000-07-07 | 2000-07-07 | Method of coating sol-gel onto surface of easy-to-oxidize metal |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1278462A (en) |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1317770C (en) * | 2002-03-13 | 2007-05-23 | 精工爱普生株式会社 | Device making method and apparatus, device and electronic machine thereof |
| CN102876097A (en) * | 2012-09-20 | 2013-01-16 | 吴江市天源塑胶有限公司 | Weather-resistant emulsion paint |
| CN104141122A (en) * | 2013-10-28 | 2014-11-12 | 中国石油化工集团公司 | Metal matrix surface alumina coating and preparation method thereof |
| CN109487244A (en) * | 2018-11-23 | 2019-03-19 | 中国人民解放军国防科技大学 | Wear-resistant hydrophobic ZrO2Low-temperature rapid preparation method of coating |
| CN113355658A (en) * | 2021-06-02 | 2021-09-07 | 中广核工程有限公司 | Metal matrix surface anti-corrosion ceramic coating and preparation method thereof |
| CN114538961A (en) * | 2021-12-28 | 2022-05-27 | 中核四0四有限公司 | SiC/Y on surface of C-based material2O3Method for repairing coating crack |
| CN114769592A (en) * | 2022-06-01 | 2022-07-22 | 浙江佳泰气动元件有限公司 | Machining process of pneumatic connector |
-
2000
- 2000-07-07 CN CN 00109801 patent/CN1278462A/en active Pending
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1317770C (en) * | 2002-03-13 | 2007-05-23 | 精工爱普生株式会社 | Device making method and apparatus, device and electronic machine thereof |
| US7364622B2 (en) | 2002-03-13 | 2008-04-29 | Seiko Epson Corporation | Method and apparatus for fabricating a device, and the device and an electronic equipment |
| CN102876097A (en) * | 2012-09-20 | 2013-01-16 | 吴江市天源塑胶有限公司 | Weather-resistant emulsion paint |
| CN104141122A (en) * | 2013-10-28 | 2014-11-12 | 中国石油化工集团公司 | Metal matrix surface alumina coating and preparation method thereof |
| CN104141122B (en) * | 2013-10-28 | 2018-02-16 | 中国石油化工集团公司 | A kind of metal base surface aluminum oxide coating layer and preparation method thereof |
| CN109487244A (en) * | 2018-11-23 | 2019-03-19 | 中国人民解放军国防科技大学 | Wear-resistant hydrophobic ZrO2Low-temperature rapid preparation method of coating |
| CN113355658A (en) * | 2021-06-02 | 2021-09-07 | 中广核工程有限公司 | Metal matrix surface anti-corrosion ceramic coating and preparation method thereof |
| CN113355658B (en) * | 2021-06-02 | 2022-08-12 | 中广核工程有限公司 | Metal matrix surface anti-corrosion ceramic coating and preparation method thereof |
| CN114538961A (en) * | 2021-12-28 | 2022-05-27 | 中核四0四有限公司 | SiC/Y on surface of C-based material2O3Method for repairing coating crack |
| CN114538961B (en) * | 2021-12-28 | 2023-01-03 | 中核四0四有限公司 | SiC/Y on surface of C-based material 2 O 3 Method for repairing coating crack |
| CN114769592A (en) * | 2022-06-01 | 2022-07-22 | 浙江佳泰气动元件有限公司 | Machining process of pneumatic connector |
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