CN111748781A - Composite antibacterial target material and preparation method and application thereof - Google Patents

Composite antibacterial target material and preparation method and application thereof Download PDF

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Publication number
CN111748781A
CN111748781A CN202010560027.1A CN202010560027A CN111748781A CN 111748781 A CN111748781 A CN 111748781A CN 202010560027 A CN202010560027 A CN 202010560027A CN 111748781 A CN111748781 A CN 111748781A
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antibacterial
target material
composite
metal
target
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CN111748781B (en
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林孝发
林孝山
胡征宇
王汉春
李日红
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Jomoo Kitchen and Bath Co Ltd
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Jomoo Kitchen and Bath Co Ltd
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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
    • C23C14/3407—Cathode assembly for sputtering apparatus, e.g. Target
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/10—Metallic powder containing lubricating or binding agents; Metallic powder containing organic material
    • 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
    • C23C14/0015—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterized by the colour of the layer
    • 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
    • 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
    • C23C14/3407—Cathode assembly for sputtering apparatus, e.g. Target
    • C23C14/3414—Metallurgical or chemical aspects of target preparation, e.g. casting, powder metallurgy

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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)
  • Physical Vapour Deposition (AREA)
  • Laminated Bodies (AREA)
  • Agricultural Chemicals And Associated Chemicals (AREA)

Abstract

The invention discloses a composite antibacterial target, which comprises raw materials of a target main metal, a load type antibacterial material and an auxiliary agent, wherein the addition amount of the load type antibacterial material is 0.1-10% of the mass of the raw materials; the load type antibacterial material is a carrier loaded with nano antibacterial metal, and the content of the nano antibacterial metal is 1-5% of the mass of the load type antibacterial material. The invention also discloses a preparation method of the composite antibacterial target material and application of the antibacterial film layer prepared by vacuum coating. The invention can make the nanometer antibacterial metal particles attach to the surface of the product in a more stable form relative to the metal simple substance, greatly reduce the release speed of the antibacterial metal particles, endow the product with durable antibacterial performance and obtain stable coating color appearance.

Description

Composite antibacterial target material and preparation method and application thereof
Technical Field
The invention relates to the technical field of functional materials, in particular to a composite antibacterial target material and a preparation method and application thereof.
Background
Due to the problems of bacterial growth, infection with infectious diseases, etc., the demand for antibacterial products is increasingly gaining attention. In the surface treatment technology of the prior bathroom products, most of the vacuum coating layers are used as the outermost layers, and in order to realize the antibacterial performance, the prior method comprises the following steps: 1. plating a film by adopting metal such as pure silver, copper and the like; 2. the target material adopts pure metal elements such as pure silver, copper and the like. If the metal coating such as pure silver, copper and the like is adopted, firstly, the silver, the copper and the like belong to active heavy metals and cannot be directly used for antibiosis of household products with higher health requirements; secondly, the antibacterial components such as silver, copper and the like are directly exposed in the environment and can be oxidized, and the product is easy to change color; moreover, the surface of the product is in the color of silver and copper, and the richer color appearances such as golden yellow, gun color, rose color and the like cannot be obtained through PVD reaction coating. If antibacterial components such as silver, copper and the like are directly added into the target material, the antibacterial durability is poor due to the fast consumption of ions, and the antibacterial performance is obviously reduced in the using process.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provides a composite antibacterial target material and a preparation method and application thereof.
In order to achieve the above purpose, the technical scheme of the invention is as follows:
the invention provides a composite antibacterial target, which comprises the raw materials of a target main metal, a load type antibacterial material and an auxiliary agent, wherein the addition amount of the load type antibacterial material is 0.1-10% of the mass of the raw materials; the load type antibacterial material is a carrier loaded with nano antibacterial metal, and the content of the nano antibacterial metal is 1-5% of the mass of the load type antibacterial material.
Optionally, the support is zeolite, copper phosphate, zirconium phosphate or activated carbon.
Optionally, the size of the carrier is 200-2000 nm.
Optionally, the nano antibacterial metal is at least one of silver and copper.
Optionally, the target primary metal comprises zirconium, titanium and chromium.
Optionally, the auxiliary agent includes a dispersant and a binder. The dispersing agent can be polyamide wax, polyethylene wax, etc., and the adhesive can be sodium polyacrylate.
Optionally, the composite antibacterial target material comprises the following raw materials in percentage by mass: 94-99.4% of target main metal, 0.5-5.5% of load type antibacterial material and the balance of auxiliary agent, wherein the auxiliary agent comprises 0.03-0.1% of dispersant and 0.01-0.05% of adhesive.
The invention also provides a preparation method of the composite antibacterial target material, which is characterized by uniformly mixing the raw materials and preparing the composite antibacterial target material by a powder metallurgy method, wherein the molding temperature is 500-2500 ℃.
The invention also provides a method for preparing the antibacterial film layer by using the composite antibacterial target material, which comprises the steps of installing the composite antibacterial target material on a vacuum coating machine, loading a workpiece to be coated, vacuumizing, and carrying out target material assisted-bombardment, uniform-bombardment, non-reaction coating and reaction coating to obtain the antibacterial film layer.
The invention also provides the antibacterial film layer prepared by the method.
Optionally, the thickness of the antibacterial film layer is 200-500 nm.
The invention has the beneficial effects that:
1) according to the invention, the load-type antibacterial material and the target main metal are mixed to form the composite antibacterial target material and used for vacuum coating, and due to the polyhedron structure and the like of the load-type antibacterial material, nano antibacterial metal particles can be attached to the surface of a product in a more stable form relative to a metal simple substance, so that the release speed of the antibacterial metal particles is greatly reduced, and the product is endowed with a lasting antibacterial property;
2) because the nano antibacterial metal particles are loaded in the carrier and are not directly exposed in the environment, the nano antibacterial metal particles are not easily oxidized while reducing the consumption, the surface of the product is not easily discolored, and the stable coating color appearance is obtained.
Detailed Description
The following specific examples further illustrate the invention.
Examples 1 to 7
Uniformly mixing and stirring the powder of the main metal of the target, the supported antibacterial material, the dispersant and the adhesive according to the mass ratio shown in the following table, and preparing the composite antibacterial target by adopting a hot isostatic pressing method, wherein the molding temperature is 1200 ℃. The main metal of the target material is zirconium, the carrier of the supported antibacterial material is zirconium phosphate, the size of the supported antibacterial material is about 1500nm, the nano antibacterial metal is nano silver, and the content of the nano silver is 2% of the mass of the supported antibacterial material.
And (3) adopting a PVD (physical vapor deposition) process, mounting 8 two rows of the prepared composite antibacterial target materials on a vacuum coating machine, loading a workpiece to be coated, and then vacuumizing for coating. The coating process comprises the steps of target material bombardment assisting, homogeneous bombardment, non-reaction coating and reaction coating, wherein the background vacuum of the coating is 0.005pa, the vacuum of the coating is 0.6pa, the flow of argon is 300sccm, the flow of nitrogen is 450sccm, the flow of acetylene is 80sccm, the bias voltage is set to 80v and 50 percent duty ratio, the coating time is 2 and 90s, and the golden-like antibacterial film layer is obtained, and the thickness of the film layer is about 150 nm.
The mass percentages and antibacterial rates of the raw materials of examples 1-7 (antibacterial performance test, detection criteria and method for detecting two strains of escherichia coli and staphylococcus aureus according to GBT 21510-2008) are shown in the following table:
Figure BDA0002545754760000031
comparative example 1
The load type antibacterial material is replaced by metal silver, and the distribution ratio and the process of the other components are the same as those in example 3.
The antibacterial film layers obtained in examples 1 to 4 and comparative example 1 were subjected to a boiling test:
the water quality degradation (soaking the product in distilled water at 80 ℃. + -. 1 ℃ for 24 h. + -. 10min) the colour change was tested. The test results are shown in the following table, wherein the Delta E is the stability of the film layer in water quality degradation, and the Lab value of the surface color value is changed due to the oxidation and the change of components of the film layer during the boiling process. The larger Δ E, the less stable the film layer.
Example 1:
L a b ΔE
initial 78.98 2.78 25.12
24H 77.54 3.21 26.11 1.80
48H 76.79 3.98 27.32 3.33
72H 76.12 4.32 28.52 4.70
Example 2:
L a b ΔE
initial 76.32 2.33 27.45
24H 75.43 2.98 28.33 1.41
48H 74.15 3.78 29.98 3.63
72H 74.67 4.32 30.49 3.99
Example 3:
L a b ΔE
initial 78.13 1.95 24.02
24H 77.18 2.23 25.55 1.82
48H 76.89 2.32 26.23 2.56
72H 76.12 2.48 27.31 3.89
Example 4:
L a b ΔE
initial 79.11 2.78 24.45
24H 78.21 2.43 25.87 1.71
48H 77.65 3.54 26.31 2.48
72H 76.55 4.13 27.32 4.07
Comparative example 1:
L a b ΔE
initial 78.56 2.25 23.5
24H 77.8 2.62 26.14 2.77
48H 76.62 3.78 27.98 5.11
72H 74.97 4.8 29.22 7.21
Compared with the antibacterial film layer obtained from the silver-zirconium alloy target material, the film stability of the antibacterial film layer formed by the load type antibacterial material is obviously improved. Through verification, compared with the antibacterial film layer obtained by the silver-zirconium alloy target, the antibacterial effect of the load type antibacterial film layer of the embodiment can be prolonged by 3-5 years.
Example 8
Mixing and stirring 94.9% of target main metal powder, 5% of load type antibacterial material, 0.07% of dispersing agent and 0.03% of adhesive uniformly, and preparing the composite antibacterial target by adopting a hot isostatic pressing method, wherein the forming temperature is 1200 ℃. The main metal of the target material is zirconium, the carrier of the supported antibacterial material is copper phosphate, the size of the supported antibacterial material is about 800nm, the nano antibacterial metal is nano copper, and the content of the nano copper is 5% of the mass of the supported antibacterial material.
And (3) adopting a PVD (physical vapor deposition) process, mounting 8 two rows of the prepared composite antibacterial target materials on a vacuum coating machine, loading a workpiece to be coated, and then vacuumizing for coating. The coating process comprises the steps of target material assisted bombardment, uniform bombardment, non-reaction coating and reaction coating, wherein the background vacuum of the coating is 0.005pa, the vacuum of the coating is 0.6pa, the flow of argon is 300sccm, the flow of nitrogen is 200sccm, the bias voltage is set to 100v, the duty ratio of 50 percent is set, the coating time is 2 to 90s, and the stainless steel color-imitated antibacterial film layer is obtained, and the thickness of the film layer is about 150 nm.
In addition, by selecting a proper target main metal material and adjusting process parameters such as nitrogen flow and the like, appearance effects such as rose gold and gun color can be obtained, the color of the obtained antibacterial coating is not influenced by the load type antibacterial material, rich and stable color appearance can be obtained, and the application is wide.
The above embodiments are only used to further illustrate the composite antibacterial target material, the preparation method and the application thereof, but the present invention is not limited to the embodiments, and any simple modification, equivalent change and modification made to the above embodiments according to the technical spirit of the present invention fall within the protection scope of the technical scheme of the present invention.

Claims (10)

1. A composite antibacterial target material is characterized in that: the raw materials of the composite antibacterial target material comprise a target material main metal, a load-type antibacterial material and an auxiliary agent, wherein the addition amount of the load-type antibacterial material is 0.1-10% of the mass of the raw materials; the load type antibacterial material is a carrier loaded with nano antibacterial metal, and the content of the nano antibacterial metal is 1-5% of the mass of the load type antibacterial material.
2. The composite antimicrobial target material according to claim 1, wherein: the carrier is zeolite, copper phosphate, zirconium phosphate or activated carbon.
3. The composite antimicrobial target material according to claim 1, wherein: the size of the carrier is 200-2000 nm.
4. The composite antimicrobial target material according to claim 1, wherein: the nano antibacterial metal is at least one of silver and copper.
5. The composite antimicrobial target material according to claim 1, wherein: the target main metal comprises zirconium, titanium and chromium.
6. The composite antimicrobial target material according to claim 1, wherein: the composite antibacterial target material comprises the following raw materials in percentage by mass: 94-99.4% of target main metal, 0.5-5.5% of load type antibacterial material and the balance of auxiliary agent, wherein the auxiliary agent comprises 0.03-0.1% of dispersant and 0.01-0.05% of adhesive.
7. The preparation method of the composite antibacterial target material of any one of claims 1 to 6, which is characterized by comprising the following steps: the raw materials are uniformly mixed, and the composite antibacterial target material is prepared by a powder metallurgy method, wherein the forming temperature is 500-2500 ℃.
8. A method for preparing an antibacterial film layer by using the composite antibacterial target material of any one of claims 1 to 6, which is characterized by comprising the following steps: and (3) mounting the composite antibacterial target material on a vacuum coating machine, loading a workpiece to be coated, vacuumizing, and performing assisted-bombardment, uniform-bombardment, non-reaction coating and reaction coating on the target material to obtain an antibacterial film layer.
9. An antimicrobial film layer made by the method of claim 8.
10. The antimicrobial film layer of claim 9, wherein: the thickness of the antibacterial film layer is 200-500 nm.
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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2022259184A1 (en) * 2021-06-08 2022-12-15 Moya Alarcon Matias Ignacio A high-efficient decontaminant additive comprising metal oxide nanoparticles in a metallic or semi-metallic nanoparticle matrix, useful to be added in paints, formulations or the like for protecting, coating or decorating, soft or hard, surfaces
CN115572948A (en) * 2022-09-16 2023-01-06 九牧厨卫股份有限公司 PVD alloy target with high comprehensive performance and preparation and application thereof
WO2023143899A1 (en) * 2022-01-31 2023-08-03 Grohe Ag Method for coating a substrate and use of a target for coating a substrate

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2022259184A1 (en) * 2021-06-08 2022-12-15 Moya Alarcon Matias Ignacio A high-efficient decontaminant additive comprising metal oxide nanoparticles in a metallic or semi-metallic nanoparticle matrix, useful to be added in paints, formulations or the like for protecting, coating or decorating, soft or hard, surfaces
WO2023143899A1 (en) * 2022-01-31 2023-08-03 Grohe Ag Method for coating a substrate and use of a target for coating a substrate
CN115572948A (en) * 2022-09-16 2023-01-06 九牧厨卫股份有限公司 PVD alloy target with high comprehensive performance and preparation and application thereof

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