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WO2008028355A1 - Procédé de fabrication de produits antibactériens en surface suivant la technique de déposition physique en phase vapeur - Google Patents

Procédé de fabrication de produits antibactériens en surface suivant la technique de déposition physique en phase vapeur Download PDF

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Publication number
WO2008028355A1
WO2008028355A1 PCT/CN2006/003275 CN2006003275W WO2008028355A1 WO 2008028355 A1 WO2008028355 A1 WO 2008028355A1 CN 2006003275 W CN2006003275 W CN 2006003275W WO 2008028355 A1 WO2008028355 A1 WO 2008028355A1
Authority
WO
WIPO (PCT)
Prior art keywords
antibacterial
vapor deposition
physical vapor
plating
target
Prior art date
Application number
PCT/CN2006/003275
Other languages
English (en)
Chinese (zh)
Inventor
Peiqi Jiang
Original Assignee
Peiqi Jiang
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Priority claimed from CNB200610121944XA external-priority patent/CN100519821C/zh
Application filed by Peiqi Jiang filed Critical Peiqi Jiang
Publication of WO2008028355A1 publication Critical patent/WO2008028355A1/fr

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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
    • C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/24—Vacuum evaporation
    • C23C14/243—Crucibles for source 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
    • C23C14/0021—Reactive sputtering or evaporation

Definitions

  • the present invention relates to a method for preparing a surface antibacterial article, and more particularly to a method for producing a surface antibacterial article by physical vapor deposition.
  • antibacterial ability of antibacterial products is mainly reflected on the surface of antibacterial products.
  • Conventional antibacterial products are made by directly incorporating antibacterial materials into substrates such as metal materials, polymer materials, and glazes. 'This method causes a large amount of waste material to be wasted, and the manufacturing process is complicated and the processing cost is too high.
  • some new technologies for manufacturing surface antibacterial products by physical vapor deposition technology have appeared, such as Chinese patent application "A surface antibacterial, wear-resistant stainless steel product and its preparation method" (application number: 200410027063. 2), The technology provides a method for preparing wear-resistant and antibacterial stainless steel products by magnetron sputtering.
  • the method is purely used for the production of stainless steel products, and the use range is too small, and is not practical in many fields.
  • Wear-resistant technology such as disposable antibacterial catheter, medical wound suture surface, and ventilator tube inner wall; 2 the antibacterial material used is only silver and copper, which cannot meet the requirements in special technical fields, such as photocatalysis.
  • the existing photocatalytic material Ti0 2 can only have an antibacterial effect under ultraviolet light of 387. 5 nm or less, and it is not antibacterial at 387. 5 nm or more; 3
  • This coating method has directionality and is not applicable. Plated parts on complex surfaces, such as the inner wall of a ventilator pipe.
  • a reaction gas such as oxygen, nitrogen, acetylene gas or hydrogen sulfide is added to cause the target material to become an oxide, a carbide, a nitride, a sulfide or the like.
  • Ion plating refers to the application of a bias current to the forged workpiece, so that the deposited material has directionality and high-speed kinetic energy, so that the plating material and the substrate are more closely combined.
  • the material utilization rate of the sputtering plane target is only 20%, and the material utilization rate of the sputtering cylinder target is 80%.
  • the precious metal materials such as silver are mostly used for the cylindrical target, which will be made.
  • the silver tube is placed over the copper target. During the use, the silver sleeve will undergo lateral expansion and longitudinal shrinkage, that is, the silver tube becomes thicker and shorter, which separates the silver tube from the copper core and affects the sputtering effect.
  • the reaction is not comprehensive, that is, the pure black product is not plated. This is because the multi-arc plating uses the arc method to evaporate the target and generate a large amount of ion gas flow. A large amount of ionic gas stream repels the reaction gas to the surface of the workpiece to be plated.
  • Target poisoning is prone to occur during magnetron sputtering black plating. This is because the molten carbon gas is filled into the furnace cavity for the plating of pure black products, which causes the concentration of argon ions to decrease, which affects the sputtering effect.
  • the object of the present invention is to overcome the above-mentioned drawbacks of the prior art, and to provide a method for manufacturing a surface antibacterial product by physical vapor deposition technology with low cost, wider use range and simple and convenient fabrication, and the method of the invention has 1 antibacterial method.
  • the material is plated onto the surface of the complex surface to be plated; 2 to enhance the antibacterial effect of the photocatalytic antibacterial material; 3 to provide more antibacterial materials; 4 to solve the separation of the casing and the core of the cylindrical target; 5 with pure multi-arc plating Black film process; 6 magnetron sputtering is used to plate pure black film, and it also prevents target poisoning.
  • a method for manufacturing a surface antibacterial article by using a physical vapor deposition technique comprising: using a physical vapor deposition technique to plate an antibacterial target or an evaporant onto a surface of a substrate to form a film layer, wherein: the antibacterial material is Ti, Zn, Among Ca, Si, Mg, Zr, Cd, As, Sb, Se, Ce, Re, Cu, Ag, Pb, Hg, Co, Ni, Al, Fe and their oxides, sulfides, nitrides, carbides
  • One or more of the reaction gases charged in the physical vapor deposition technique are 0 2 , N 2 , M 3 , CH 4 , ( 2 or 3.;
  • the physical vapor deposition technique is evaporative plating, magnetron sputtering, multi-arc plating or plasma plating; the plasma plating is immersion plasma plating, magnetron sputtering, ion plating, radio frequency plasma plating, microwave plasma plating, and heat.
  • the ionized cluster deposition plasma plating apparatus is a heating source, an ionization device, an accelerating electrode and a substrate from bottom to top, and is installed inside the heating source, and is 3 to 5;
  • the ionization device is a microwave ionization device
  • the ratio of the antibacterial material in the film layer is 0.01% ⁇ 100%;
  • the cylindrical target is composed of an inner core made of a copper tube and a jacket made of an antibacterial material, and the antibacterial material is made into a metal strip and wound around the inner core;
  • the cylindrical target is composed of an inner core made of a copper tube and a jacket made of an antibacterial material, and the inner core and the outer sleeve are screwed;
  • the substrate is a dry solid material, which may be a metal material, a non-metal material, a fiber product, a polymer material, a dried plant material or a leather material;
  • the surface antibacterial product is a stainless steel cutter, and the manufacturing process is that the silver or copper-containing stainless steel plate is first welded or pasted on the blade edge of the cutter main body, and then the blade edge is ground, and then the physical vapor deposition coating is applied to the wear-resistant antibacterial surface layer. .
  • the antimicrobial material can be plated onto the surface of a complex article, such as the inner wall of a ventilator tube.
  • the present invention employs immersion plasma plating.
  • a magnetron sputtering glow discharge plasma a pulse voltage is applied to a plated member at a voltage of several tens of kilovolts, and the plated member is immersed in the plasma, and ions in the plasma are applied to the surfaces of the workpiece. It can be plated in hooks and holes.
  • magnetron sputtering plasma there is RF plasma, Microwave plasma, hot wire cathode assisted plasma, can be used for antibacterial coating.
  • Photocatalytic antibacterial materials include: Ti0 2 , ZnO, CaO, Si0 2 , MgO, Zr0 2 , CdS , Se0 2 , SiC; These materials have low photocatalytic activity and show no antibacterial effect under natural light. When rare earth lanthanum, cerium or antibacterial materials such as Cu, Ag, Pb, etc. are added during the coating process, they have strong antibacterial effect under natural light.
  • the material is one or more of elemental materials or compounds, and is added to rare earth lanthanum, cerium or Cu, Ag, One or more materials in Pb are mixed and plated, and the corresponding gas 02 is charged to deposit a specific photocatalytic composite antibacterial material.
  • the invention prepares surface antibacterial products by physical vapor deposition technology, the process is simple and convenient to manufacture, high in efficiency, low in cost, and the invention arranges and combines antibacterial materials having different characteristics according to requirements. Therefore, surface antibacterial products suitable for different technical fields are obtained, such as surface antibacterial products such as human implant materials and utensils prepared by using Ag, Cu, Zn, Ce, Ca which are safe and non-toxic to human body; safe Co, Ni, Al , Fe, S to prepare surface antibacterial products such as human contact materials; use antibacterial materials As, Sb, Se, Hg with strong bactericidal ability, but toxic to human body to prepare other surface antibacterial products; strong antibacterial such as Ag and antifungal
  • Cu mixed plating is used to prepare a broad-spectrum antibacterial product
  • Zn, Ce and Cr are added to the silver plating material to solve the defect that silver is easily oxidized and blackened, and a surface antibacterial product with beautiful appearance and stable properties is obtained.
  • the charged reaction gas is 0 2 , N 2 , NH 3 , CH 4 , C 2 H 6 , H 2 S, and the above-mentioned antibacterial material and reaction gas can be combined with each other as needed, and the antibacterial materials can also be combined with each other, such as A g S AgCeNi can also be combined with other metal non-metals such as AgW, CrAgN CuZnO, etc., and can be combined into thousands of new combined antibacterial materials. 01% ⁇ 100 ⁇ The proportion of the inorganic material in the coating layer is 0. 01% ⁇ 100%.
  • the antibacterial target material of the invention is a cylindrical target, and the cylindrical target is an inner core made of a copper tube and a jacket made of an antibacterial material.
  • the antibacterial material may be attached to the inner core by a metal strip or may be connected to the inner core by a screw connection. 5.
  • the process of using a multi-arc plating pure black film is realized.
  • the invention is applied to a small air hole around a multi-arc target, and directly passes CH 4 and C 2 H 6 gas into the hole to form high carbon in the plating area. It can be plated with pure black film.
  • the present invention adopts a distribution line on the surface of the workpiece (substrate) to be plated, and gas CH 4 and C 2 are introduced therein.
  • the surface of the workpiece to be plated forms a high carbonized zone, which can effectively prevent target poisoning and can be plated with pure black film.
  • the invention also provides a combined ionizing cluster deposition technique.
  • Ionized cluster deposition is the deposition of thin films using ionized radicals with a certain energy.
  • the ionized atomic group may comprise hundreds or even thousands of atoms, which are deposited on the workpiece to be plated under the acceleration of the electric field. At the moment of contact with the working piece, the atomic group is broken, the atoms are dispersed and deposited on the lining. Bottom surface. This has a variety of materials deposited, the coating has good adhesion, low temperature and controllability.
  • the technology of the present invention requires a plurality of evaporation enthalpy to meet the needs due to the need for composite material coating. Generally, the resistance heating method is used.
  • the present invention designs a carbon-embedded crucible, and a set of emblem-wave heating method.
  • the method has a great advantage.
  • the microwave can give the ionized group a charge, accelerate the ionization effect, and accelerate the sputtering rate of the ionized atomic group.
  • the coating quality is better.
  • Figure 1 is a schematic diagram of a gas pipeline for distributing an arc source target, wherein 5 is an ion arc region;
  • Figure 2 is a cutaway view of the arc source target
  • FIG. 3 is a schematic structural view of a casing cylindrical target made by a metal strip winding method
  • Figure 4 is a schematic view showing the structure of a casing cylindrical target made by screwing
  • Figure 5 is a schematic view showing the principle of surface coating by immersion plasma plating
  • FIG. 6 is a schematic view showing the principle of surface coating by ionizing cluster deposition plasma plating
  • Figure 7 is a schematic diagram showing the structure of an antibacterial stainless steel table knife
  • Figure 8 is a view of the A - ⁇ ⁇ of Figure 7.
  • the surface of the object is coated with an antibacterial layer by evaporation coating technology.
  • the coating technology is carried out in an existing activation reaction evaporation deposition apparatus: wherein the substrate is selected from a dry solid material such as a metal material, a non-metal material, a fiber product, a polymer material, a dried plant material or a leather material, and an antibacterial material.
  • a dry solid material such as a metal material, a non-metal material, a fiber product, a polymer material, a dried plant material or a leather material, and an antibacterial material.
  • the evaporation material is selected from the group consisting of Ti, Zn, Ca, Si, Mg, Zr, Cd, As, Sb, Se, Ce, Re, Cu, Ag, Pb, Hg, Co, Ni, Al, Fe and their oxides, sulfides, One or more of a nitride or a carbide, the amount of which is 0.01% to 100% by weight of the entire film layer, and the reaction gas is 0 2 , N 2 , NH 3 , CH 4 , C 2 H 6 i H 2 S.
  • the anti-bacterial layer is coated on the surface of the object by multi-arc plating technology.
  • the coating technology is carried out in an existing multi-arc ion coating machine: wherein the substrate is selected from dry solid materials such as metal materials, non-metal materials, fiber products, polymer materials, dried plant materials or leather materials, and antibacterial materials.
  • the target is selected from the group consisting of Ti, Zn, Ca, Si, Mg, Zr, Cd, As, Sb, Se, Ce, Re, Cu, Ag, Pb, Hg, Co, Ni, Al, Fe and their oxides, sulfides, One or more of nitrides and carbides, in an amount of 0.01% - 100% by weight of the entire film layer, as shown in Fig. 1.
  • a magnetron sputtering antibacterial target is also disposed in the multi-arc coating furnace, and the antibacterial target 3 is a cylindrical target.
  • the cylindrical target is made of a copper tube inner core 3-1 and made of an antibacterial material.
  • the formed jacket is composed of 3 - 2, and the above-mentioned antibacterial material is formed into a metal strip and wound around the inner core; the reaction gas is 0 2 , N 2 , NH 3 , CH 4 , C 2 H 6 or H 2 S.
  • the coating technology is carried out in an existing magnetron sputtering ion plating machine: wherein the substrate is selected from a dry solid material such as a metal material, a non-metal material, a fiber product, a polymer material, a dried plant material or a leather material.
  • the antibacterial target is selected from the group consisting of Ti, Zn, Ca, Si, Mg, Zr, Cd, As, Sb, Se, Ce, Re, Cu, Ag, Pb, Hg, Co, Ni, Al, Fe and their oxides, and vulcanization.
  • the antibacterial target 3 is a cylindrical target
  • the cylindrical target shown in FIG. 4 is a cylindrical target composed of an inner core 3-1 made of a copper tube and a jacket 3 - 2 made of an antibacterial material, and the inner core and the outer sleeve are threaded. connection.
  • the reaction gas is 0 2 , N 2 , 3 , CH 4 , C 2 H 6 or H 2 S.
  • the preparation of surface antibacterial products is carried out by magnetron sputtering coating technology.
  • the coating technology is carried out in a ionization beam deposition plasma plating apparatus: wherein the substrate is selected from a dry solid material such as a metal material, a non-metal material, a fiber product, a polymer material, a dried plant material or a leather material, and an antibacterial material.
  • a dry solid material such as a metal material, a non-metal material, a fiber product, a polymer material, a dried plant material or a leather material, and an antibacterial material.
  • the target is selected from Ti, Zn, Ca, Si, Mg Zr, Cd, As, Sb, Se, Ce, Re, 'Cu, Ag, Pb, Hg, Co, Ni, Al, Fe and their oxides, sulfides, One or more of nitrides and carbides, used in an amount of 0.01% to 100% by weight of the entire film layer, and the reaction gas is 0 2 , N 2 , NH 3 , CH 4 , C 2 H 6 or H 2 S.
  • FIG. 6 shows the heating source 10, the ionization device 11, the accelerating electrode 12 and the substrate 13 in order from bottom to top, and the crucible 9 is mounted on the heating.
  • the main difference is that there are a plurality of ⁇ 9, generally 3 to 5, which can hold a variety of targets.
  • the coating technology is carried out in a dip plasma plating apparatus, as shown in Figure 5: wherein the substrate is selected Dry solid materials, such as metal materials, non-metallic materials, fiber products, polymer materials, dry plant materials or leather materials, antibacterial.
  • Targets use Ti, Zn, Ca, Si, Mg, Zr, Cd, As, Sb , Se, Ce, Re, Cu, Ag, Pb, Hg, Co, M, Al, Fe and one or more of its oxides, sulfides, nitrides, carbides, the amount of which is the entire film weight From 0.01% to 100%, it is necessary to provide a ventilation tube on the surface of the substrate.
  • the reaction gas is 0 2 , N 2 , NH 3 , C , ( 2 11 6 or 3.
  • the knife In the process of cutting, peeling and cutting, the knife is easy to passivate and the sharpness will decrease. It is necessary to grind the blade. In the process of grinding the blade, the antibacterial surface of the blade will be worn away, and the surface layer will be worn away. No antibacterial effect is achieved.
  • Figure 8 that is, before the coating, the stainless steel knife needs to be pre-treated, specifically to first weld or paste the silver or copper-containing stainless steel plate 15 in the tool body.
  • the steel plate 14 is cut at the cutting edge, and then the blade is ground, and then the physical vapor deposition is applied to the wear-resistant antibacterial surface layer.
  • the specific coating technique can adopt any one of the above embodiments 1 to 4.
  • the antibacterial stainless steel knife prepared by the above method has the following advantages: 1. The blade is still antibacterial after being ground. 2. Save on the use of silver-containing stainless steel.

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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)

Abstract

L'invention concerne un procédé de fabrication de produits antibactériens en surface au moyen d'une technique de déposition physique en phase vapeur, destinée à appliquer des matériaux cibles antibactériens ou des matériaux de vaporisation à la surface d'un substrat, de manière à former une couche de film antibactérien, procédé caractérisé en ce que les matériaux cibles antibactériens ou les matériaux de vaporisation comprennent un ou plusieurs produits sélectionnés dans le groupe ci-après : Ti, Zn, Ca, Si, Mg, Zr, Cd, As, Sb, Se, Ce, Re, Cu, Ag, Pb, Hg, Co, Ni, Al, Fe, ainsi que des oxydes, sulfures, nitrures et carbures de ces produits, un gaz réactionnel utilisé dans la technique de déposition physique en phase vapeur, à savoir : O2, N2, NH3, CH4, C2H6 ou H2S. Des trous (1) sont forés à la surface de la cible (3), en vue d'assurer l'alimentation en gaz par des passages de gaz (2), empêchant ainsi tout empoisonnement de la cible et permettant de réaliser efficacement un revêtement multi-arc et une pulvérisation magnétron, tout en améliorant le rendement du revêtement et la qualité de la couche de film.
PCT/CN2006/003275 2006-08-28 2006-12-04 Procédé de fabrication de produits antibactériens en surface suivant la technique de déposition physique en phase vapeur WO2008028355A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
CN200610121944.X 2006-08-28
CNB200610121944XA CN100519821C (zh) 2006-02-28 2006-08-28 利用物理气相沉积技术制造表面抗菌制品的方法

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WO2008028355A1 true WO2008028355A1 (fr) 2008-03-13

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Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108359937A (zh) * 2018-02-27 2018-08-03 温州驰诚真空机械有限公司 转换式物理气相沉积粒子源
CN111876734A (zh) * 2020-07-16 2020-11-03 贵州大学 一种纳米Ag-Zn双层点阵涂层的制备方法
CN112239848A (zh) * 2020-09-17 2021-01-19 佛山市安齿生物科技有限公司 一种抗菌牙种植体及其制备方法
CN113209722A (zh) * 2021-03-30 2021-08-06 云南前沿新材料科技发展有限公司 一种含铜和银的抑菌抗病毒滤网及其制备方法
CN114345384A (zh) * 2021-07-09 2022-04-15 苏州道一至诚纳米材料技术有限公司 快速杀灭冠状病毒和细菌的膜层材料及其制备方法
CN114369808A (zh) * 2021-12-20 2022-04-19 中国兵器科学研究院宁波分院 一种镁及镁合金表面制备抗菌涂层的方法
CN115537505A (zh) * 2022-11-18 2022-12-30 太原科技大学 一种电脉冲加速含铜钢富铜相析出速度的方法

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Cited By (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108359937A (zh) * 2018-02-27 2018-08-03 温州驰诚真空机械有限公司 转换式物理气相沉积粒子源
CN108359937B (zh) * 2018-02-27 2023-08-22 温州驰诚真空机械有限公司 转换式物理气相沉积粒子源
CN111876734A (zh) * 2020-07-16 2020-11-03 贵州大学 一种纳米Ag-Zn双层点阵涂层的制备方法
CN111876734B (zh) * 2020-07-16 2022-05-17 贵州大学 一种纳米Ag-Zn双层点阵涂层的制备方法
CN112239848A (zh) * 2020-09-17 2021-01-19 佛山市安齿生物科技有限公司 一种抗菌牙种植体及其制备方法
CN112239848B (zh) * 2020-09-17 2022-12-06 广东中科安齿生物科技有限公司 一种抗菌牙种植体及其制备方法
CN113209722A (zh) * 2021-03-30 2021-08-06 云南前沿新材料科技发展有限公司 一种含铜和银的抑菌抗病毒滤网及其制备方法
CN114345384A (zh) * 2021-07-09 2022-04-15 苏州道一至诚纳米材料技术有限公司 快速杀灭冠状病毒和细菌的膜层材料及其制备方法
CN114345384B (zh) * 2021-07-09 2023-11-21 苏州道一至诚纳米材料技术有限公司 快速杀灭冠状病毒和细菌的膜层材料及其制备方法
CN114369808A (zh) * 2021-12-20 2022-04-19 中国兵器科学研究院宁波分院 一种镁及镁合金表面制备抗菌涂层的方法
CN114369808B (zh) * 2021-12-20 2024-02-06 中国兵器科学研究院宁波分院 一种镁及镁合金表面制备抗菌涂层的方法
CN115537505A (zh) * 2022-11-18 2022-12-30 太原科技大学 一种电脉冲加速含铜钢富铜相析出速度的方法

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