CN112593188A - Composite nano multilayer film, preparation method thereof and medical surgical knife - Google Patents
Composite nano multilayer film, preparation method thereof and medical surgical knife Download PDFInfo
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- CN112593188A CN112593188A CN202110239101.4A CN202110239101A CN112593188A CN 112593188 A CN112593188 A CN 112593188A CN 202110239101 A CN202110239101 A CN 202110239101A CN 112593188 A CN112593188 A CN 112593188A
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- 239000002131 composite material Substances 0.000 title claims abstract description 45
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- 239000000758 substrate Substances 0.000 claims abstract description 33
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 claims abstract description 28
- 239000010408 film Substances 0.000 claims description 95
- 238000004544 sputter deposition Methods 0.000 claims description 40
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 38
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 21
- 238000000137 annealing Methods 0.000 claims description 21
- 229910052757 nitrogen Inorganic materials 0.000 claims description 19
- 229910001069 Ti alloy Inorganic materials 0.000 claims description 14
- 238000004140 cleaning Methods 0.000 claims description 14
- 238000005498 polishing Methods 0.000 claims description 14
- 239000010936 titanium Substances 0.000 claims description 14
- 238000000227 grinding Methods 0.000 claims description 13
- 238000000034 method Methods 0.000 claims description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 7
- 239000007864 aqueous solution Substances 0.000 claims description 7
- 239000011248 coating agent Substances 0.000 claims description 7
- 238000000576 coating method Methods 0.000 claims description 7
- 238000001816 cooling Methods 0.000 claims description 7
- 208000028659 discharge Diseases 0.000 claims description 7
- 238000001035 drying Methods 0.000 claims description 7
- 239000007789 gas Substances 0.000 claims description 7
- 238000011065 in-situ storage Methods 0.000 claims description 7
- 238000001755 magnetron sputter deposition Methods 0.000 claims description 7
- 239000000243 solution Substances 0.000 claims description 7
- 230000003746 surface roughness Effects 0.000 claims description 7
- 239000010409 thin film Substances 0.000 claims description 5
- 239000002356 single layer Substances 0.000 claims description 4
- 229910052802 copper Inorganic materials 0.000 claims description 3
- 229910052709 silver Inorganic materials 0.000 claims description 3
- 229910052725 zinc Inorganic materials 0.000 claims description 3
- 239000002923 metal particle Substances 0.000 claims description 2
- 230000008021 deposition Effects 0.000 abstract 1
- 230000000052 comparative effect Effects 0.000 description 4
- 230000000844 anti-bacterial effect Effects 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 238000007373 indentation Methods 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 229910003460 diamond Inorganic materials 0.000 description 1
- 239000010432 diamond Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000007542 hardness measurement Methods 0.000 description 1
- 239000010410 layer Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
Classifications
-
- 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
- C23C14/0641—Nitrides
-
- 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
- C23C14/0021—Reactive sputtering or evaporation
- C23C14/0036—Reactive sputtering
-
- 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
-
- 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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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Physical Vapour Deposition (AREA)
Abstract
A composite nanometer multilayer film and a preparation method thereof and a medical operation cutter are provided, the composite nanometer multilayer film with TiN/ZrN alternate deposition is prepared on the surface of a substrate, and the technical bottleneck that a single film is difficult to break through the technology with the hardness of 30GPa in the prior art is overcome. Further, the influence of different modulation ratios on the hardness of the composite nano-multilayer film at a modulation period of 30nm was intensively studied, and as a result, it was shown that the composite nano-multilayer film exhibited the most excellent surface hardness when the modulation ratio was R = 1.
Description
Technical Field
The invention relates to the field of nano multilayer films, in particular to a medical operation cutter composite nano multilayer film and a preparation method thereof.
Background
The surgical knife is an important tool indispensable in surgical operation, and in order to improve the hardness and corrosion resistance of a pure metal or alloy surgical knife, a modified film is generally required to be coated on the surface of the knife, and a ZrN film and a TiN film are widely applied to the surgical knife due to the excellent surface properties of the ZrN film and the TiN film. However, the hardness of a single TiN film or ZrN film is lower than 30GPa, which greatly limits the use scene.
Disclosure of Invention
Aiming at the problems in the prior art, the invention aims to provide a composite nano multilayer film, which can improve the hardness of a single film and can meet more application scenes.
A preparation method of a composite nano multilayer film comprises the following steps:
A. taking titanium alloy as a substrate, sequentially grinding, polishing, deoiling and cleaning the titanium alloy, and then drying for later use;
B. putting the dried substrate into a magnetron sputtering coating machine for glow discharge treatment;
C. introducing nitrogen as working gas, closing the Zr target, starting the Ti target, and sputtering the TiN film on the surface of the substrate, wherein the sputtering power is 200-250W, the sputtering temperature is 120-150 ℃, and the nitrogen flow is 400-500 sccm;
D. closing the Ti target, starting the Zr target, and sputtering the ZrN film on the surface of the TiN film, wherein the sputtering power is 220-;
E. repeating the steps C and D until the total thickness of the composite nano multilayer film meets the requirement;
F. and carrying out in-situ annealing on the composite nano multilayer film, wherein the annealing temperature is 350-380 ℃, the annealing time is 2-3h, and then cooling along with the furnace.
Further, the surface roughness Ra =5-6 μm of the substrate after the grinding and polishing is ensured.
Further, 15% NaOH aqueous solution is selected for oil removal.
Further, the cleaning solution is absolute ethyl alcohol.
Preferably, the method further comprises doping one or more of metal ions Ag, Cu and Zn into the outermost ZrN thin film.
Furthermore, the thickness of the single-layer TiN film is 5-25nm, and the thickness of the single-layer ZrN film is 5-25 nm.
Further, the total thickness of the composite film was 6 μm.
Furthermore, the modulation period of the nano multilayer film is 30nm, and the modulation ratio is 0.2-5.
The invention also provides a composite nano multilayer film, which is prepared by the method.
The invention also provides a medical surgical knife, and the surface of the surgical knife is provided with the composite nano multilayer film.
The invention prepares the TiN/ZrN alternately deposited composite nano multilayer film on the surface of the substrate, and overcomes the technical bottleneck that the single film in the prior art is difficult to break through the hardness of 30 GPa. In addition, the present inventors have intensively studied the influence of different modulation ratios on the hardness of the composite nano multilayer film at a modulation period of 30nm, and as a result, it was revealed that the composite nano multilayer film exhibited the most excellent surface hardness when the modulation ratio was R = 1.
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
A preparation method of a composite nano multilayer film comprises the following steps:
A. taking titanium alloy as a substrate, sequentially grinding, polishing, deoiling and cleaning the titanium alloy, and then drying for later use; wherein, after grinding and polishing, the surface roughness Ra =5-6 μm of the substrate is ensured, 15% NaOH aqueous solution is selected for oil removal, and the cleaning solution is absolute ethyl alcohol;
B. putting the dried substrate into a magnetron sputtering coating machine for glow discharge treatment;
C. introducing nitrogen as working gas, closing the Zr target, starting the Ti target, and sputtering a TiN film on the surface of the substrate, wherein the sputtering power is 200W, the sputtering temperature is 120 ℃, the nitrogen flow is 400sccm, and the thickness of the TiN film is 5nm;
D. closing the Ti target, starting the Zr target, and sputtering a ZrN film on the surface of the TiN film, wherein the sputtering power is 220W, the sputtering temperature is 100 ℃, the nitrogen flow is 350sccm, and the thickness of the ZrN film is 25nm;
E. repeating the steps C and D until the total thickness of the composite nano multilayer film is 6 mu m;
F. and carrying out in-situ annealing on the composite nano multilayer film, wherein the annealing temperature is 350 ℃, the annealing time is 2 hours, and then cooling along with the furnace.
Example 2
A preparation method of a composite nano multilayer film comprises the following steps:
A. taking titanium alloy as a substrate, sequentially grinding, polishing, deoiling and cleaning the titanium alloy, and then drying for later use; wherein, after grinding and polishing, the surface roughness Ra =5-6 μm of the substrate is ensured, 15% NaOH aqueous solution is selected for oil removal, and the cleaning solution is absolute ethyl alcohol;
B. putting the dried substrate into a magnetron sputtering coating machine for glow discharge treatment;
C. introducing nitrogen as working gas, closing the Zr target, starting the Ti target, and sputtering a TiN film on the surface of the substrate, wherein the sputtering power is 200W, the sputtering temperature is 120 ℃, the nitrogen flow is 400sccm, and the thickness of the TiN film is 10nm;
D. closing the Ti target, starting the Zr target, and sputtering a ZrN film on the surface of the TiN film, wherein the sputtering power is 220W, the sputtering temperature is 100 ℃, the nitrogen flow is 350sccm, and the thickness of the ZrN film is 20nm;
E. repeating the steps C and D until the total thickness of the composite nano multilayer film is 6 mu m;
F. and carrying out in-situ annealing on the composite nano multilayer film, wherein the annealing temperature is 350 ℃, the annealing time is 2 hours, and then cooling along with the furnace.
Example 3
A preparation method of a composite nano multilayer film comprises the following steps:
A. taking titanium alloy as a substrate, sequentially grinding, polishing, deoiling and cleaning the titanium alloy, and then drying for later use; wherein, after grinding and polishing, the surface roughness Ra =5-6 μm of the substrate is ensured, 15% NaOH aqueous solution is selected for oil removal, and the cleaning solution is absolute ethyl alcohol;
B. putting the dried substrate into a magnetron sputtering coating machine for glow discharge treatment;
C. introducing nitrogen as working gas, closing the Zr target, starting the Ti target, and sputtering a TiN film on the surface of the substrate, wherein the sputtering power is 200W, the sputtering temperature is 120 ℃, the nitrogen flow is 400sccm, and the thickness of the TiN film is 15nm;
D. closing the Ti target, starting the Zr target, and sputtering a ZrN film on the surface of the TiN film, wherein the sputtering power is 220W, the sputtering temperature is 100 ℃, the nitrogen flow is 350sccm, and the thickness of the ZrN film is 15nm;
E. repeating the steps C and D until the total thickness of the composite nano multilayer film is 6 mu m;
F. and carrying out in-situ annealing on the composite nano multilayer film, wherein the annealing temperature is 350 ℃, the annealing time is 2 hours, and then cooling along with the furnace.
Example 4
A preparation method of a composite nano multilayer film comprises the following steps:
A. taking titanium alloy as a substrate, sequentially grinding, polishing, deoiling and cleaning the titanium alloy, and then drying for later use; wherein, after grinding and polishing, the surface roughness Ra =5-6 μm of the substrate is ensured, 15% NaOH aqueous solution is selected for oil removal, and the cleaning solution is absolute ethyl alcohol;
B. putting the dried substrate into a magnetron sputtering coating machine for glow discharge treatment;
C. introducing nitrogen as working gas, closing the Zr target, starting the Ti target, and sputtering a TiN film on the surface of the substrate, wherein the sputtering power is 200W, the sputtering temperature is 120 ℃, the nitrogen flow is 400sccm, and the thickness of the TiN film is 20nm;
D. closing the Ti target, starting the Zr target, and sputtering a ZrN film on the surface of the TiN film, wherein the sputtering power is 220W, the sputtering temperature is 100 ℃, the nitrogen flow is 350sccm, and the thickness of the ZrN film is 10nm;
E. repeating the steps C and D until the total thickness of the composite nano multilayer film is 6 mu m;
F. and carrying out in-situ annealing on the composite nano multilayer film, wherein the annealing temperature is 350 ℃, the annealing time is 2 hours, and then cooling along with the furnace.
Example 5
A preparation method of a composite nano multilayer film comprises the following steps:
A. taking titanium alloy as a substrate, sequentially grinding, polishing, deoiling and cleaning the titanium alloy, and then drying for later use; wherein, after grinding and polishing, the surface roughness Ra =5-6 μm of the substrate is ensured, 15% NaOH aqueous solution is selected for oil removal, and the cleaning solution is absolute ethyl alcohol;
B. putting the dried substrate into a magnetron sputtering coating machine for glow discharge treatment;
C. introducing nitrogen as working gas, closing the Zr target, starting the Ti target, and sputtering a TiN film on the surface of the substrate, wherein the sputtering power is 200W, the sputtering temperature is 120 ℃, the nitrogen flow is 400sccm, and the thickness of the TiN film is 25nm;
D. closing the Ti target, starting the Zr target, and sputtering a ZrN film on the surface of the TiN film, wherein the sputtering power is 220W, the sputtering temperature is 100 ℃, the nitrogen flow is 350sccm, and the thickness of the ZrN film is 5nm;
E. repeating the steps C and D until the total thickness of the composite nano multilayer film is 6 mu m;
F. and carrying out in-situ annealing on the composite nano multilayer film, wherein the annealing temperature is 350 ℃, the annealing time is 2 hours, and then cooling along with the furnace.
Comparative example 1
The difference from example 3 is that a TiN thin film of 6 μm thickness is prepared on the substrate surface.
Comparative example 2
The difference from example 3 is that a ZrN thin film of 6 μm thickness was prepared on the substrate surface.
Comparative example 3
The difference from example 3 is that a TiN film of 3 μm thickness + ZrN film of 3 μm thickness was prepared on the substrate surface.
The film materials of examples 1 to 5 (corresponding to A, B, C, D, E) and comparative examples 1 to 3 (corresponding to X, Y, Z) were subjected to hardness testing, and a Nano-indenter G200 Nano indenter produced by MTS was used to perform Nano-indentation experiments on the composite Nano-multilayer film, so as to obtain hardness data of the film, wherein a Berkovich triangular pyramid diamond indenter was used for the experiments, and the indentation depth was not more than 10% of the film thickness. The test results are shown in table 1.
Table 1 hardness test experimental results
| Numbering | A | B | C | D | E | X | Y | Z |
| hardness/GPa | 33.2 | 33.4 | 39.1 | 36.2 | 34.7 | 24.6 | 28.5 | 27.9 |
Research shows that the surface hardness of the composite film can be greatly improved by arranging the nano multilayer film. Further, as a result of examining the nano-multilayer films having different modulation ratios with a modulation period of 30nm in examples 1 to 5, it was found that the nano-multilayer films having different modulation ratios had an influence on the hardness of the same nano-multilayer film, and that the composite nano-multilayer film exhibited excellent high hardness characteristics when the modulation ratio R = 1.
In addition, in view of the requirement that the surgical knife generally has antibacterial performance, the invention can also dope partial antibacterial metal particles such as Ag, Cu, Zn and the like in the ZrN thin film at the outermost layer so as to meet the use requirement of a specific scene.
Claims (8)
1. The preparation method of the composite nano multilayer film is characterized by comprising the following steps of:
A. taking titanium alloy as a substrate, sequentially grinding, polishing, deoiling and cleaning the titanium alloy, and then drying for later use;
B. putting the dried substrate into a magnetron sputtering coating machine for glow discharge treatment;
C. introducing nitrogen as working gas, closing the Zr target, starting the Ti target, and sputtering the TiN film on the surface of the substrate, wherein the sputtering power is 200-250W, the sputtering temperature is 120-150 ℃, and the nitrogen flow is 400-500 sccm;
D. closing the Ti target, starting the Zr target, and sputtering the ZrN film on the surface of the TiN film, wherein the sputtering power is 220-;
E. repeating the steps C and D until the total thickness of the composite nano multilayer film meets the requirement;
F. and carrying out in-situ annealing on the composite nano multilayer film, wherein the annealing temperature is 350-380 ℃, the annealing time is 2-3h, and then cooling along with the furnace.
2. A method of preparing the composite nano-multilayer film of claim 1, wherein: after sanding and polishing, the surface roughness Ra =5-6 μm of the substrate is ensured.
3. A method of preparing the composite nano-multilayer film of claim 1, wherein: the oil removal is carried out by using 15% NaOH aqueous solution.
4. A method of preparing the composite nano-multilayer film of claim 1, wherein: the cleaning solution is absolute ethyl alcohol.
5. A method of preparing the composite nano-multilayer film of claim 1, wherein: and doping one or more of metal particles Ag, Cu and Zn into the outermost ZrN thin film.
6. A method of preparing a composite nano-multilayer film according to claims 1 to 5, characterized in that: the thickness of the single-layer TiN film is 5-25nm, and the thickness of the single-layer ZrN film is 5-25 nm.
7. A composite nano-multilayer film prepared by any one of the methods of claims 1-6.
8. A medical surgical knife, wherein the surface of the knife is covered with the composite nano multilayer film according to claim 7.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112972780A (en) * | 2021-04-26 | 2021-06-18 | 中南大学湘雅医院 | Biliary tract stent surface nano coating and preparation method thereof |
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|---|---|---|---|---|
| CN101200797A (en) * | 2007-11-21 | 2008-06-18 | 中南大学 | PVD nano multiple-layer coating for cutting stainless steel and preparation method thereof |
| CN103273687A (en) * | 2013-05-13 | 2013-09-04 | 山东大学 | TiSiN+ZrSiN composite nanometer coated cutting tool and preparation method thereof |
| CN109207923A (en) * | 2018-09-18 | 2019-01-15 | 广东工业大学 | A kind of TiN/ZrN nano laminated coating and its preparation method and application |
| CN110373639A (en) * | 2019-07-24 | 2019-10-25 | 艾瑞森表面技术（苏州）股份有限公司 | Cutting element composite coating and preparation method thereof |
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- 2021-03-04 CN CN202110239101.4A patent/CN112593188B/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101200797A (en) * | 2007-11-21 | 2008-06-18 | 中南大学 | PVD nano multiple-layer coating for cutting stainless steel and preparation method thereof |
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| CN109207923A (en) * | 2018-09-18 | 2019-01-15 | 广东工业大学 | A kind of TiN/ZrN nano laminated coating and its preparation method and application |
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| Title |
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| X.M. XU,ET AL.: "《Oxidation behavior of TiN/ZrN multilayers annealed in air》", 《THIN SOLID FILMS》 * |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112972780A (en) * | 2021-04-26 | 2021-06-18 | 中南大学湘雅医院 | Biliary tract stent surface nano coating and preparation method thereof |
| CN112972780B (en) * | 2021-04-26 | 2021-07-20 | 中南大学湘雅医院 | Biliary tract stent surface nano coating and preparation method thereof |
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