CN114196921B - Magnesium alloy surface coating and preparation method thereof - Google Patents
Magnesium alloy surface coating and preparation method thereof Download PDFInfo
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- CN114196921B CN114196921B CN202210146838.6A CN202210146838A CN114196921B CN 114196921 B CN114196921 B CN 114196921B CN 202210146838 A CN202210146838 A CN 202210146838A CN 114196921 B CN114196921 B CN 114196921B
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/14—Metallic material, boron or silicon
- C23C14/16—Metallic material, boron or silicon on metallic substrates or on substrates of boron or silicon
- C23C14/165—Metallic material, boron or silicon on metallic substrates or on substrates of boron or silicon by cathodic sputtering
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/02—Pretreatment of the material to be coated
- C23C14/021—Cleaning or etching treatments
- C23C14/022—Cleaning or etching treatments by means of bombardment with energetic particles or radiation
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
- C23C14/35—Sputtering by application of a magnetic field, e.g. magnetron sputtering
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/58—After-treatment
- C23C14/5806—Thermal treatment
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/58—After-treatment
- C23C14/5846—Reactive treatment
- C23C14/586—Nitriding
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Abstract
The invention relates to a magnesium alloy surface coating and a preparation method thereof. The invention carries out pretreatment, magnetron sputtering of a metal Ti layer, liquid nitrogen cryogenic treatment and gas nitriding treatment on the medical magnesium alloy in sequence, and a titanium nitrogen layer is obtained on the surface of the medical magnesium alloy. Compared with the traditional method for directly preparing the titanium-nitrogen layer by magnetron sputtering, the preparation method can obtain the titanium-nitrogen layer with more excellent wear resistance. It is worth mentioning that the magnesium alloy must be subjected to room temperature standing treatment after the liquid nitrogen cryogenic treatment, so as to avoid cracks generated in the subsequent use process of the magnesium alloy composite material.
Description
Technical Field
The invention relates to the field of coating materials, in particular to a magnesium alloy surface coating and a preparation method thereof.
Background
The magnesium alloy is formed by adding other elements into magnesium as a matrix and is characterized by small density, good heat dissipation, good shock absorption, high specific strength and excellent specific rigidity. The Young modulus of the magnesium alloy is about 45GPa, which is far lower than that of stainless steel and cobalt-based alloy, is about half of that of titanium alloy, is relatively close to human bone, and can remarkably reduce the stress shielding effect caused by the mismatching of the elastic modulus between the internal plant and the bone. At present, magnesium alloys have been widely used in various fields of clinical medicine as orthopedic internal fixation materials, vascular scaffolds, porous bone tissue engineering materials, and the like. However, the insufficient wear resistance is a defect that magnesium alloys are more remarkable. In view of the above, how to obtain a magnesium alloy medical composite material with excellent wear resistance is a hot research spot.
Disclosure of Invention
Aiming at the problems in the prior art, the invention aims to provide a preparation method of a magnesium alloy surface coating, by which a medical magnesium alloy composite material with excellent wear resistance can be obtained, and the composite material can be used in the field of orthopedic materials.
A preparation method of a magnesium alloy surface coating comprises the following steps:
magnesium alloy surface pretreatment: selecting magnesium alloy as a substrate, and pretreating the substrate;
ion bombardment of the magnesium alloy: carrying out ion bombardment treatment on the pretreated magnesium alloy;
magnetron sputtering of a metal Ti layer: putting the magnesium alloy substrate into a magnetron sputtering coating machine, vacuumizing the coating equipment, preparing a metal Ti layer on the surface of the magnesium alloy by taking a metal titanium target as a sputtering source and argon as working gas, wherein the sputtering temperature is 220 ℃ for plus 180 ℃, the target base distance is 6-8cm, the argon flow is 80-100sccm, the sputtering power is 150W for plus 120 and the sputtering time is 50-80 min;
liquid nitrogen cryogenic treatment: soaking the magnesium alloy coated with the Ti layer in liquid nitrogen for cryogenic treatment;
gas nitriding treatment: the magnesium alloy after the deep cooling treatment is kept stand for 1-2h at room temperature, then is put into a gas nitriding furnace, nitrogen and hydrogen are introduced for nitriding treatment, the temperature is firstly raised to 500 ℃ at the temperature rise rate of 10-15 ℃/min in the nitriding process, the temperature is kept for 3-4h, and the volume ratio of the nitrogen to the hydrogen is 3: 1 in the nitriding process.
Preferably, the pretreatment comprises sanding with 400#, 800#, 1200# precision sand paper until the surface of the magnesium alloy is smooth and has no obvious scratches.
Preferably, the pretreatment comprises washing with absolute ethyl alcohol, acetone and deionized water for 5-10min respectively.
Preferably, the pretreatment comprises blow-drying the magnesium alloy with a blower.
Preferably, the time of the liquid nitrogen cryogenic treatment is 30-120 min.
The invention further provides a magnesium alloy surface coating, which is prepared by the method.
The invention carries out pretreatment, magnetron sputtering of a metal Ti layer, liquid nitrogen cryogenic treatment and gas nitriding treatment on the medical magnesium alloy in sequence, and a titanium nitrogen layer is obtained on the surface of the medical magnesium alloy. Compared with the traditional method for directly preparing the titanium-nitrogen layer by magnetron sputtering, the preparation method can obtain the titanium-nitrogen layer with more excellent wear resistance. It is worth mentioning that the magnesium alloy must be subjected to room temperature standing treatment after the liquid nitrogen cryogenic treatment, so as to avoid cracks generated in the subsequent use process of the magnesium alloy composite material.
Detailed Description
The technical effects of the present invention are demonstrated below by specific examples, but the embodiments of the present invention are not limited thereto.
Example 1
Magnesium alloy surface pretreatment: selecting magnesium alloy as a substrate, polishing the surface of the magnesium alloy by using abrasive paper with the precision of 400#, 800#, 1200#, until the surface is smooth and has no obvious scratch, then respectively cleaning the surface for 5min by using absolute ethyl alcohol, acetone and deionized water, and finally drying the surface by using a blower;
ion bombardment of the magnesium alloy: carrying out ion bombardment treatment on the pretreated magnesium alloy to obtain a magnesium alloy substrate with the surface roughness Ra of about 1.5 mu m;
magnetron sputtering of a metal Ti layer: putting a magnesium alloy substrate into a magnetron sputtering coating machine, vacuumizing a coating device, and preparing a metal Ti layer on the surface of the magnesium alloy by taking a metal titanium target as a sputtering source and argon as a working gas, wherein the sputtering temperature is 220 ℃, the target base distance is 7cm, the argon flow is 100sccm, the sputtering power is 150W, and the sputtering time is 50 min;
liquid nitrogen cryogenic treatment: soaking the magnesium alloy coated with the Ti layer in liquid nitrogen at-196 ℃ for cryogenic treatment, and taking out after 30min of treatment;
gas nitriding treatment: the magnesium alloy after the deep cooling treatment is kept stand for 1h at room temperature, then is put into a gas nitriding furnace, nitrogen and hydrogen are introduced for nitriding treatment, the temperature is firstly raised to 500 ℃ at the heating rate of 10 ℃/min in the nitriding process, the temperature is kept for 4h, and the volume ratio of the nitrogen to the hydrogen in the nitriding process is 3: 1.
Example 2
Magnesium alloy surface pretreatment: selecting magnesium alloy as a substrate, polishing the surface of the magnesium alloy by using abrasive paper with the precision of 400#, 800#, 1200#, until the surface is smooth and has no obvious scratch, then respectively cleaning the surface for 5min by using absolute ethyl alcohol, acetone and deionized water, and finally drying the surface by using a blower;
ion bombardment of the magnesium alloy: carrying out ion bombardment treatment on the pretreated magnesium alloy to obtain a magnesium alloy substrate with the surface roughness Ra of about 1.5 mu m;
magnetron sputtering of a metal Ti layer: putting a magnesium alloy substrate into a magnetron sputtering coating machine, vacuumizing a coating device, and preparing a metal Ti layer on the surface of the magnesium alloy by taking a metal titanium target as a sputtering source and argon as a working gas, wherein the sputtering temperature is 220 ℃, the target base distance is 7cm, the argon flow is 100sccm, the sputtering power is 150W, and the sputtering time is 50 min;
liquid nitrogen cryogenic treatment: soaking the magnesium alloy coated with the Ti layer in liquid nitrogen at-196 ℃ for cryogenic treatment, and taking out after 60min of treatment;
gas nitriding treatment: the magnesium alloy after the deep cooling treatment is kept stand for 1h at room temperature, then is put into a gas nitriding furnace, nitrogen and hydrogen are introduced for nitriding treatment, the temperature is firstly raised to 500 ℃ at the heating rate of 10 ℃/min in the nitriding process, the temperature is kept for 4h, and the volume ratio of the nitrogen to the hydrogen in the nitriding process is 3: 1.
Example 3
Magnesium alloy surface pretreatment: selecting magnesium alloy as a substrate, polishing the surface of the magnesium alloy by using abrasive paper with the precision of 400#, 800#, 1200#, until the surface is smooth and has no obvious scratch, then respectively cleaning the surface for 5min by using absolute ethyl alcohol, acetone and deionized water, and finally drying the surface by using a blower;
ion bombardment of the magnesium alloy: carrying out ion bombardment treatment on the pretreated magnesium alloy to obtain a magnesium alloy substrate with the surface roughness Ra of about 1.5 mu m;
magnetron sputtering of a metal Ti layer: putting a magnesium alloy substrate into a magnetron sputtering coating machine, vacuumizing a coating device, and preparing a metal Ti layer on the surface of the magnesium alloy by taking a metal titanium target as a sputtering source and argon as a working gas, wherein the sputtering temperature is 220 ℃, the target base distance is 7cm, the argon flow is 100sccm, the sputtering power is 150W, and the sputtering time is 50 min;
liquid nitrogen cryogenic treatment: soaking the magnesium alloy coated with the Ti layer in liquid nitrogen at-196 ℃ for cryogenic treatment, and taking out after 90min of treatment;
gas nitriding treatment: the magnesium alloy after the deep cooling treatment is kept stand for 1h at room temperature, then is put into a gas nitriding furnace, nitrogen and hydrogen are introduced for nitriding treatment, the temperature is firstly raised to 500 ℃ at the heating rate of 10 ℃/min in the nitriding process, the temperature is kept for 4h, and the volume ratio of the nitrogen to the hydrogen in the nitriding process is 3: 1.
Example 4
Magnesium alloy surface pretreatment: selecting magnesium alloy as a substrate, polishing the surface of the magnesium alloy by using abrasive paper with the precision of 400#, 800#, 1200#, until the surface is smooth and has no obvious scratch, then respectively cleaning the surface for 5min by using absolute ethyl alcohol, acetone and deionized water, and finally drying the surface by using a blower;
ion bombardment of the magnesium alloy: carrying out ion bombardment treatment on the pretreated magnesium alloy to obtain a magnesium alloy substrate with the surface roughness Ra of about 1.5 mu m;
magnetron sputtering of a metal Ti layer: putting a magnesium alloy substrate into a magnetron sputtering coating machine, vacuumizing a coating device, and preparing a metal Ti layer on the surface of the magnesium alloy by taking a metal titanium target as a sputtering source and argon as a working gas, wherein the sputtering temperature is 220 ℃, the target base distance is 7cm, the argon flow is 100sccm, the sputtering power is 150W, and the sputtering time is 50 min;
liquid nitrogen cryogenic treatment: soaking the magnesium alloy coated with the Ti layer in liquid nitrogen at-196 ℃ for cryogenic treatment, and taking out after 120min of treatment;
gas nitriding treatment: the magnesium alloy after the deep cooling treatment is kept stand for 1h at room temperature, then is put into a gas nitriding furnace, nitrogen and hydrogen are introduced for nitriding treatment, the temperature is firstly raised to 500 ℃ at the heating rate of 10 ℃/min in the nitriding process, the temperature is kept for 4h, and the volume ratio of the nitrogen to the hydrogen in the nitriding process is 3: 1.
Comparative example 1
Magnesium alloy surface pretreatment: selecting magnesium alloy as a substrate, polishing the surface of the magnesium alloy by using abrasive paper with the precision of 400#, 800#, 1200#, until the surface is smooth and has no obvious scratch, then respectively cleaning the surface for 5min by using absolute ethyl alcohol, acetone and deionized water, and finally drying the surface by using a blower;
ion bombardment of the magnesium alloy: carrying out ion bombardment treatment on the pretreated magnesium alloy to obtain a magnesium alloy substrate with the surface roughness Ra of about 1.5 mu m;
magnetron sputtering of a metal Ti layer: putting a magnesium alloy substrate into a magnetron sputtering coating machine, vacuumizing a coating device, and preparing a metal Ti layer on the surface of the magnesium alloy by taking a metal titanium target as a sputtering source and argon as a working gas, wherein the sputtering temperature is 220 ℃, the target base distance is 7cm, the argon flow is 100sccm, the sputtering power is 150W, and the sputtering time is 50 min;
gas nitriding treatment: standing the magnesium alloy coated with the metal Ti layer for 1h at room temperature, then putting the magnesium alloy into a gas nitriding furnace, introducing nitrogen and hydrogen to carry out nitriding treatment, raising the temperature to 500 ℃ at the temperature rise rate of 10 ℃/min in the nitriding process, and preserving heat for 4h, wherein the volume ratio of the nitrogen to the hydrogen in the nitriding process is 3: 1.
Comparative example 2
Magnesium alloy surface pretreatment: selecting magnesium alloy as a substrate, polishing the surface of the magnesium alloy by using abrasive paper with the precision of 400#, 800#, 1200#, until the surface is smooth and has no obvious scratch, then respectively cleaning the surface for 5min by using absolute ethyl alcohol, acetone and deionized water, and finally drying the surface by using a blower;
ion bombardment of the magnesium alloy: carrying out ion bombardment treatment on the pretreated magnesium alloy to obtain a magnesium alloy substrate with the surface roughness Ra of about 1.5 mu m;
magnetron sputtering of a TiN layer: putting the magnesium alloy substrate into a magnetron sputtering film plating machine, vacuumizing a film plating device, preparing a TiN layer on the surface of the magnesium alloy by taking a metal titanium target as a sputtering source and taking nitrogen and argon as working gases, wherein the sputtering temperature is 220 ℃, the target base distance is 7cm, the nitrogen flow is 100sccm, the argon flow is 100sccm, the sputtering power is 150W, and the sputtering time is 50 min.
Next, we evaluated the wear resistance of the samples of examples 1 to 4 and comparative examples 1 to 2 by the following specific methods: the wear resistance of each sample is evaluated by adopting a CETR-3 type friction wear testing machine, the load is 10N, the friction pair is a GCr15 steel ball with the diameter of 5mm, the friction frequency is 12Hz, the friction stroke is 3mm, the friction time is 80min, and the mass before and after the wear is weighed by an electronic balance to calculate the wear loss. The experimental results of the samples are shown in table 1, and the blank group in table 1 is an untreated magnesium alloy.
TABLE 1 abrasion loss of each sample
| Numbering | Abrasion loss/mg |
| Example 1 | 3.5 |
| Example 2 | 2.1 |
| Example 3 | 2.8 |
| Example 4 | 3.9 |
| Comparative example 1 | 8.3 |
| Comparative example 2 | 6.5 |
| Blank group | 21.4 |
Further, the inventor also finds that if the workpiece subjected to liquid nitrogen cryogenic treatment is subjected to nitriding treatment directly, the obtained magnesium alloy material can generate obvious cracks in a wear resistance test. Therefore, the room temperature standing stage after the liquid nitrogen cryogenic treatment is an essential treatment step.
The above description is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, several modifications and variations can be made without departing from the technical principle of the present invention, and these modifications and variations should also be regarded as the protection scope of the present invention.
Claims (6)
1. The preparation method of the magnesium alloy surface coating is characterized by comprising the following steps:
magnesium alloy surface pretreatment: selecting magnesium alloy as a substrate, and pretreating the substrate;
ion bombardment of the magnesium alloy: carrying out ion bombardment treatment on the pretreated magnesium alloy;
magnetron sputtering of a metal Ti layer: putting the magnesium alloy substrate into a magnetron sputtering coating machine, vacuumizing the coating equipment, preparing a metal Ti layer on the surface of the magnesium alloy by taking a metal titanium target as a sputtering source and argon as working gas, wherein the sputtering temperature is 220 ℃ for plus 180 ℃, the target base distance is 6-8cm, the argon flow is 80-100sccm, the sputtering power is 150W for plus 120 and the sputtering time is 50-80 min;
liquid nitrogen cryogenic treatment: soaking the magnesium alloy coated with the Ti layer in liquid nitrogen for cryogenic treatment;
gas nitriding treatment: the magnesium alloy after the deep cooling treatment is kept stand for 1-2h at room temperature, then is put into a gas nitriding furnace, nitrogen and hydrogen are introduced for nitriding treatment, the temperature is firstly raised to 500 ℃ at the temperature rise rate of 10-15 ℃/min in the nitriding process, the temperature is kept for 3-4h, and the volume ratio of the nitrogen to the hydrogen is 3: 1 in the nitriding process.
2. The method according to claim 1, wherein the pre-treatment comprises sanding with 400#, 800#, 1200# precision sand paper until the surface of the magnesium alloy is smooth and has no obvious scratches.
3. The method according to claim 1, wherein the pre-treatment comprises washing with absolute ethanol, acetone, and deionized water for 5-10 min.
4. The method according to claim 1, wherein the pretreatment comprises blow-drying the magnesium alloy with a blower.
5. The method according to claim 1, wherein the liquid nitrogen cryogenic treatment is carried out for a period of 30 to 120 min.
6. A magnesium alloy surface coating, characterized in that it is produced by a process according to any one of claims 1 to 5.
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| CN104032272B (en) * | 2014-06-05 | 2016-08-17 | 淮阴工学院 | In the method that medical magnesium alloy surface prepares amorphous titanium oxide active membrane layer |
| WO2017150908A1 (en) * | 2016-03-02 | 2017-09-08 | 부산대학교 산학협력단 | Method for forming coating film having high heat resistance, high hardness and abrasion resistance, coating film having high heat resistance, high hardness and abrasion resistance, and cutting tool comprising same |
| CN109183020A (en) * | 2018-08-27 | 2019-01-11 | 合肥工业大学 | A kind of preparation method of aluminum alloy surface complex gradient modified layer |
| CN112210756B (en) * | 2020-10-13 | 2022-09-02 | 辽宁科技大学 | Preparation method of iron-based alloy surface strong-corrosion-resistance high-chromium composite nitriding layer |
| CN112391600B (en) * | 2021-01-21 | 2021-04-02 | 中南大学湘雅医院 | Corrosion-resistant medical magnesium alloy surface hydroxyapatite coating and preparation method thereof |
| CN113718191B (en) * | 2021-07-28 | 2024-02-23 | 上海宝冶冶金工程有限公司 | Preparation method of aluminum magnesium alloy surface reinforcing layer |
| CN113637938B (en) * | 2021-08-17 | 2023-06-27 | 中南大学湘雅医院 | High-performance ultrasonic knife and preparation method thereof |
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| CN113897578A (en) * | 2021-10-08 | 2022-01-07 | 中南大学湘雅医院 | Surface modification method for surgical operation instrument metal |
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