CN109881168B - Preparation method of transparent anti-discoloration ceramic membrane - Google Patents
Preparation method of transparent anti-discoloration ceramic membrane Download PDFInfo
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- CN109881168B CN109881168B CN201910309641.8A CN201910309641A CN109881168B CN 109881168 B CN109881168 B CN 109881168B CN 201910309641 A CN201910309641 A CN 201910309641A CN 109881168 B CN109881168 B CN 109881168B
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Abstract
The invention discloses a preparation method of a transparent anti-discoloration ceramic membrane, and belongs to the field of nano membrane layers. Carrying out surface cleaning treatment on the base material, putting the cleaned base material on a sample rack of coating equipment, and carrying out vacuum pumping treatment by using a suction pump; and carrying out ion sputtering coating treatment on the base material in a position mode that the target material is arranged above and the base material is arranged below, wherein the distance between the base material and the target material is 150mm, and during coating, the sample rack rotates automatically at the speed of 150mm/s, so that the nano transparent film layer is deposited on the surface of the base material. According to the invention, niobium is selected as a target material, and the surface of the base material is coated by using an ion sputtering technology, so that the nano-ceramic membrane is uniformly deposited on the surface of the base material, and the nano-ceramic membrane has strong oxidation resistance and light transmittance, so that the base material can keep the original color and glossiness for a long time; meanwhile, the nano ceramic film has more reliable wear resistance, and the change of the appearance color wear caused by accidental friction on the surface of the base material is prevented.
Description
Technical Field
The invention relates to the field of nano film layers, in particular to a preparation method of a transparent anti-tarnishing ceramic film.
Background
The ion sputtering coating technology is that glow discharge is produced in a partial vacuum sputtering chamber to produce positive gas ions, and under the acceleration action of voltage between a target material and a base material, the positively charged ions bombard the surface of the target material to atomize the surface material of the target material, so that formed neutral atoms are sputtered out from all directions and fall onto the surface of the base material to form a uniform film on the surface of the base material. The ceramic film is produced by the most advanced nano technology and the superior sputtering technology, and has the characteristics of low light reflection, high light transmission, high toughness and the like.
In the prior art, in order to protect clocks and ornaments from corrosion, the surfaces of the clocks and ornaments are generally treated by a vacuum coating technology. Vacuum deposition is a method of forming a thin film by heating a metal or non-metal material under high vacuum to evaporate and condense the material on the surface of a workpiece (metal, semiconductor or insulator). However, after the common vacuum coating treatment, the surface color and luster of the clock jewelry and the like are not problematic, the color of the surface is slowly changed along with the time, the surface is oxidized, the film layer is worn out of the base material, and the base material is corroded.
Accordingly, the prior art is deficient and needs improvement.
Disclosure of Invention
The technical problem to be solved by the invention is as follows: provides a preparation method of the transparent discoloration-preventing ceramic film which can prevent the discoloration of the metal ornaments, and has corrosion resistance, oxidation resistance and strong wear resistance.
The invention comprises the following steps:
1) carrying out surface cleaning treatment on the base material; the process flow of the surface cleaning treatment comprises the following steps: cleaning the surface of the base material by water, and then baking the base material by moisture at the temperature of 50-80 ℃;
2) putting the base material obtained in the step 1) on a sample rack of a coating device, and performing vacuum pumping treatment on the coating device to ensure that the vacuum degree reaches 6 x 10-3Pa；
3) Performing ion sputtering coating treatment on the base material obtained in the step 2) in a position mode that the target material is arranged on the upper part and the base material is arranged on the lower part, so that a nano transparent film layer is deposited on the surface of the base material;
wherein the target material is niobium; the distance between the substrate and the target is 150 mm; the ion sputtering coating treatment process conditions are as follows: the sample holder rotates automatically at the speed of 150mm/s, argon with the purity of 99.999 percent is used as working gas, the flow rate of the argon is 200sccm, the current of an ion source is 60-80A, the power of a target is 30-35KW, the electric bias is 150V, the working pressure is 0.3-0.35Pa, and the duty ratio is 50-60 percent.
In the scheme, the thickness of the nano transparent film layer is 3-8 nm.
In the scheme, the processing time of the ion sputtering coating is 46-55 min.
In the above scheme, the base material is an alloy.
The invention has the beneficial effects that:
compared with the prior art, the method selects niobium as the target material, and uses the ion sputtering technology to coat the film on the surface of the base material, during film coating, the target material and the base material keep a specific distance, and simultaneously the base material keeps autorotation, so that the nano ceramic film is uniformly deposited on the surface of the base material, and the nano ceramic film has strong oxidation resistance and light transmittance, and can keep the original color and glossiness of the base material for a long time; meanwhile, the nano ceramic film has more reliable wear resistance, and the change of the appearance color wear caused by accidental friction on the surface of the base material is prevented.
Detailed Description
The present invention will be described in detail below with reference to specific examples.
Example 1
The embodiment relates to a preparation method of a transparent anti-discoloration ceramic membrane, which comprises the following main steps:
1) carrying out surface cleaning treatment on the base material; the base material is an alloy, and in this embodiment, the base material is an alloy steel sheet.
The process flow of the surface cleaning treatment comprises the following steps: the surface of the substrate is cleaned with water, and then subjected to moisture baking treatment at a temperature of 50 to 80 ℃, in this embodiment, the substrate is subjected to moisture baking treatment at a temperature of 50 ℃ being more preferable.
2) Putting the base material obtained in the step 1) on a sample rack of a coating device, and performing vacuum pumping treatment on the coating device by using an air pump to ensure that the vacuum degree reaches 6 x 10-3Pa。
3) Performing ion sputtering coating treatment on the base material obtained in the step 2) by adopting a position mode that the target material is arranged on the upper part and the base material is arranged on the lower part, so that the nano transparent film layer is deposited on the surface of the base material.
The target is selected from a rare metal material niobium. The distance between the substrate and the target is 150 mm. The ion sputtering coating treatment process conditions are as follows: the sample holder rotates automatically at the speed of 150mm/s, argon with the purity of 99.999 percent is used as working gas, the flow of the argon is 200sccm, and the current of an ion source: 60-80A, more preferably ion source current 60A; target material power: 30-35KW, preferably 30KW of target power; electrical biasing: 100-150V, more preferably 120V; working air pressure: 0.3-0.35Pa, and preferably 0.3 Pa; duty ratio: 50% -60%, and the duty ratio is preferably 50%. The ion sputtering coating treatment time is generally 46-55min, and a nano transparent film layer with the thickness of 3-8nm is obtained. In the embodiment, the ion sputtering coating treatment time is 46min, and the nano ceramic membrane steel sheet with the thickness of 3nm is finally obtained.
Example 2
The embodiment relates to a preparation method of a transparent anti-discoloration ceramic membrane, which comprises the following main steps:
1) carrying out surface cleaning treatment on the base material; the base material is an alloy, and in this embodiment, the base material is an alloy steel sheet.
The process flow of the surface cleaning treatment comprises the following steps: the surface of the substrate is cleaned with water, and then subjected to moisture baking treatment at a temperature of 50 to 80 ℃, in this embodiment, the substrate is subjected to moisture baking treatment at a temperature of more preferably 60 ℃.
2) Putting the base material obtained in the step 1) on a sample rack of a coating device, and performing vacuum pumping treatment on the coating device by using an air pump to ensure that the vacuum degree reaches 6 x 10-3Pa。
3) Performing ion sputtering coating treatment on the base material obtained in the step 2) by adopting a position mode that the target material is arranged on the upper part and the base material is arranged on the lower part, so that the nano transparent film layer is deposited on the surface of the base material.
The target is selected from a rare metal material niobium. The distance between the substrate and the target is 150 mm. The ion sputtering coating treatment process conditions are as follows: the sample holder rotates automatically at the speed of 150mm/s, argon with the purity of 99.999 percent is used as working gas, the flow of the argon is 200sccm, and the current of an ion source: 60-80A, more preferably 70A; target material power: 30-35KW, preferably 30KW of target power; electrical biasing: 100-150V, more preferably 130V; working air pressure: 0.3-0.35Pa, and preferably 0.35 Pa; duty ratio: 50% -60%, and the duty ratio is preferably 50%. The ion sputtering coating treatment time is generally 46-55min, and a nano transparent film layer with the thickness of 3-8nm is obtained. In the embodiment, the ion sputtering coating treatment time is selected to be 50min, and the nano ceramic membrane steel sheet with the thickness of 5nm is finally obtained.
Example 3
The embodiment relates to a preparation method of a transparent anti-discoloration ceramic membrane, which comprises the following main steps:
1) carrying out surface cleaning treatment on the base material; the base material is an alloy, and in this embodiment, the base material is an alloy steel sheet.
The process flow of the surface cleaning treatment comprises the following steps: the surface of the substrate is cleaned with water, and then subjected to moisture baking treatment at a temperature of 50 to 80 ℃, in this example, the substrate is subjected to moisture baking treatment at a temperature of more preferably 65 ℃.
2) Putting the base material obtained in the step 1) on a sample rack of a coating device, and performing vacuum pumping treatment on the coating device by using an air pump to ensure that the vacuum degree reaches 6 x 10-3Pa。
3) Performing ion sputtering coating treatment on the base material obtained in the step 2) by adopting a position mode that the target material is arranged on the upper part and the base material is arranged on the lower part, so that the nano transparent film layer is deposited on the surface of the base material.
The target is selected from a rare metal material niobium. The distance between the substrate and the target is 150 mm. The ion sputtering coating treatment process conditions are as follows: the sample holder rotates automatically at the speed of 150mm/s, argon with the purity of 99.999 percent is used as working gas, the flow of the argon is 200sccm, and the current of an ion source: 60-80A, more preferably ion source current 80A; target material power: 30-35KW, preferably 35KW of target power; electrical biasing: 100-150V, more preferably 150V; working air pressure: 0.3-0.35Pa, and preferably 0.35 Pa; duty ratio: 50% -60%, and the duty ratio is preferably 50%. The ion sputtering coating treatment time is generally 46-55min, and a nano transparent film layer with the thickness of 3-8nm is obtained. In the embodiment, the ion sputtering coating treatment time is selected to be 55min, and the nano ceramic membrane steel sheet with the thickness of 8nm is finally obtained.
Compared with the prior art, the method selects niobium as the target material, and uses the ion sputtering technology to coat the film on the surface of the base material, during film coating, the target material and the base material keep a specific distance, and simultaneously the base material keeps autorotation, so that the nano ceramic film is uniformly deposited on the surface of the base material, and the nano ceramic film has strong oxidation resistance and light transmittance, and can keep the original color and glossiness of the base material for a long time; meanwhile, the nano ceramic film has more reliable wear resistance, and the change of the appearance color wear caused by accidental friction on the surface of the base material is prevented.
The present invention is not limited to the above preferred embodiments, and any modifications, equivalent substitutions and improvements made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (2)
1. The preparation method of the transparent anti-discoloration ceramic membrane is characterized by comprising the following steps:
1) carrying out surface cleaning treatment on the base material; the process flow of the surface cleaning treatment comprises the following steps: cleaning the surface of the base material by water, and then baking the base material by moisture at the temperature of 50-65 ℃;
2) putting the base material obtained in the step 1) on a sample rack of a coating device, and performing vacuum pumping treatment on the coating device to ensure that the vacuum degree reaches 6 x 10-3Pa；
3) Performing ion sputtering coating treatment on the base material obtained in the step 2) in a position mode that the target material is arranged on the upper part and the base material is arranged on the lower part, so that a nano transparent film layer is deposited on the surface of the base material;
wherein the target material is niobium; the distance between the substrate and the target is 150 mm; the ion sputtering coating treatment process conditions are as follows: the sample holder rotates automatically at the speed of 150mm/s, argon with the purity of 99.999 percent is used as working gas, the flow of the argon is 200sccm, the current of an ion source is 60-80A, the power of a target is 30-35KW, the electric bias is 100-150V, the working pressure is 0.3-0.35Pa, and the duty ratio is 50-60 percent; the thickness of the nano transparent film layer is 3-8 nm; the processing time of the ion sputtering coating is 46-55 min.
2. The method for preparing a transparent discoloration-preventing ceramic film according to claim 1, wherein: the substrate is an alloy.
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| ITRM20050258A1 (en) * | 2005-05-25 | 2006-11-26 | Istituto Naz Fisica Nucleare | JEWELERY PRODUCTION PROCEDURE, USING PVD DEPOSITION TECHNIQUES AND METAL OR MINERAL FILM MASKING ON METALLIC, MINERAL, PLASTIC AND SELF-STICK SUBSTRATES. |
| CN101463462B (en) * | 2007-12-20 | 2011-11-02 | （沈阳）中国印钞造币总公司沈阳造币技术研究所 | Invisible fastness anti-tarnishing layer for silver coin surface and preparation method |
| CN101745147A (en) * | 2009-12-24 | 2010-06-23 | 中山大学 | Zinc oxide coating modified in vivo implanted artificial organ and preparation method thereof |
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Effective date of registration: 20230526 Address after: 523000 Room 102, building 2, No. 1, xierxiang, Xiegang square Middle Road, Xiegang Town, Dongguan City, Guangdong Province Patentee after: Guangdong SenMei Nano Technology Co.,Ltd. Address before: 518000 1st floor, building F, Dahua Industrial Zone, No.8, Jixiang Road, Pingdi street, Longgang District, Shenzhen City, Guangdong Province Patentee before: SHENZHEN SENTAI METAL TECHNOLOGY Co.,Ltd. |
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