CN109652769A - A kind of medical embedded material magnesium-silver coating and preparation method thereof - Google Patents

A kind of medical embedded material magnesium-silver coating and preparation method thereof Download PDF

Info

Publication number
CN109652769A
CN109652769A CN201710935102.6A CN201710935102A CN109652769A CN 109652769 A CN109652769 A CN 109652769A CN 201710935102 A CN201710935102 A CN 201710935102A CN 109652769 A CN109652769 A CN 109652769A
Authority
CN
China
Prior art keywords
magnesium
silver
coating
silver coating
matrix
Prior art date
Legal status (The legal status 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 status listed.)
Pending
Application number
CN201710935102.6A
Other languages
Chinese (zh)
Inventor
于晓明
谭丽丽
杨柯
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Institute of Metal Research of CAS
Original Assignee
Institute of Metal Research of CAS
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
Application filed by Institute of Metal Research of CAS filed Critical Institute of Metal Research of CAS
Priority to CN201710935102.6A priority Critical patent/CN109652769A/en
Publication of CN109652769A publication Critical patent/CN109652769A/en
Pending legal-status Critical Current

Links

Classifications

    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23CCOATING 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
    • C23C14/00Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/06Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/14Metallic material, boron or silicon
    • C23C14/16Metallic material, boron or silicon on metallic substrates or on substrates of boron or silicon
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61LMETHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
    • A61L27/00Materials for grafts or prostheses or for coating grafts or prostheses
    • A61L27/28Materials for coating prostheses
    • A61L27/30Inorganic materials
    • A61L27/306Other specific inorganic materials not covered by A61L27/303 - A61L27/32
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61LMETHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
    • A61L27/00Materials for grafts or prostheses or for coating grafts or prostheses
    • A61L27/50Materials characterised by their function or physical properties, e.g. injectable or lubricating compositions, shape-memory materials, surface modified materials
    • A61L27/54Biologically active materials, e.g. therapeutic substances
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61LMETHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
    • A61L27/00Materials for grafts or prostheses or for coating grafts or prostheses
    • A61L27/50Materials characterised by their function or physical properties, e.g. injectable or lubricating compositions, shape-memory materials, surface modified materials
    • A61L27/58Materials at least partially resorbable by the body
    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23CCOATING 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
    • C23C14/00Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/06Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/14Metallic material, boron or silicon
    • C23C14/20Metallic material, boron or silicon on organic substrates
    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23CCOATING 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
    • C23C14/00Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/24Vacuum evaporation
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61LMETHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
    • A61L2300/00Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices
    • A61L2300/10Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices containing or releasing inorganic materials
    • A61L2300/102Metals or metal compounds, e.g. salts such as bicarbonates, carbonates, oxides, zeolites, silicates
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61LMETHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
    • A61L2300/00Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices
    • A61L2300/10Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices containing or releasing inorganic materials
    • A61L2300/102Metals or metal compounds, e.g. salts such as bicarbonates, carbonates, oxides, zeolites, silicates
    • A61L2300/104Silver, e.g. silver sulfadiazine
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61LMETHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
    • A61L2300/00Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices
    • A61L2300/40Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices characterised by a specific therapeutic activity or mode of action
    • A61L2300/404Biocides, antimicrobial agents, antiseptic agents
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61LMETHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
    • A61L2300/00Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices
    • A61L2300/40Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices characterised by a specific therapeutic activity or mode of action
    • A61L2300/412Tissue-regenerating or healing or proliferative agents
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61LMETHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
    • A61L2420/00Materials or methods for coatings medical devices
    • A61L2420/02Methods for coating medical devices

Abstract

In order to solve the synosteosis and infection problems of implantation material, the present invention provides a kind of medical embedded material magnesium-silver coatings and preparation method thereof, using evaporation coating technique, magnesium metal-silver coating is prepared on entity or porous structure matrix prepared by pure titanium, titanium alloy, stainless steel, high molecular material, the coating with a thickness of 0.1-200 μm, the mass percent of silver element in coating are as follows: 0% < Ag≤10%.The present invention is able to solve existing implantation material osseo-compatible and infection problems, and Permanent implantation material obtained by this method is suitble to a variety of implant site mechanical property requirements, and has splendid biocompatibility, is provided simultaneously with sterilizing function.

Description

A kind of medical embedded material magnesium-silver coating and preparation method thereof
Technical field
The invention belongs to field of medical materials, in particular to gear division implantation material, joint replacement and tissue defect is filled out Fill material and implantation material antimicrobial technology field;Specially in the magnesium of implant surface-silver coating material and preparation method thereof.
Background technique
Since the undesirable cell reaction that implantation prosthetic loosening and abrasion cause makes the implants such as joint prosthesis there was only 10-15 Service life, be not able to satisfy long-time service require.Meanwhile infection is still one of catastrophic postoperative complications of orthopaedics implant. The metallic foreign body to implant is the risk factor for causing such infection to occur, and a series of internal reactions caused include macrophage The decrease of cell function, passivation of local immune system etc. all create convenient condition for the proliferation of pathogen.In addition, implantation The albumen of object adsorption can also promote bacterial adhesion to cause infection to implant surface.Past people pay close attention to mostly to environment and The removing of individual's pollution and the application of average of operation periods systemic antibiotics, and new method is, for the special machine of such infection morbidity System reduces the risk of infection by implant surface modification.
Metal material is considered to have biological stability all the time, changes although people have carried out various surfaces to its surface Property work, osteocyte adherency growth it is still undesirable.And the magnesium (Mg) in metal material, because of its negative electrode with higher Current potential occurs chemical reaction with water and degrades, is absorbed by the body and is metabolized.Meanwhile magnesium has bioactivity, can induce cell point Change, growth and blood vessel are grown into, after bone implant device implantation organism, osteocyte is degraded to magnesium and the space of reduction increases It grows, breed, as magnesium is gradually degraded, form the new respective organization and organ with original specific function and form, reach and repair The purpose of multiple wound and Reconstruction of The Function.Further, since the alkaline environment that magnesium is degraded and formed can reach the mesh for inhibiting bacterial growth 's.Magnesium is only used for the position of non-bearing, such as finger, toe due to the limitation of its mechanical property.Current Germany Syntellix The MAGNEZIX magnesium alloy compression screw of company's manufacture has passed through CE certification, and the magnesium alloy screw of U. & I. Co., Ltd., South Korea manufacture also leads to The approval for having crossed KFDA, the fracture fixation for articulations digitorum manus.Domestic Metal Inst., Chinese Academy of Sciences etc., it is suitable with Dongguan The medical instruments manufacturers such as peace, Jiangsu creation carry out magnesium-alloy material and declare.However, the said goods are answered in the form of entity bulk With, and it is used for non-bearing position.It has no at present and mg-based material is compound in existing medical embedded material surface in the form of a film Relevant report, mg-based material can be applied to need bearing position, such as joint prosthesis, this new use form in the form of a film It will play a significant role in medical embedded material field.
People use the very long evidence of history of silver-colored (Ag) device, and the bactericidal effect of silver ion is also widely applied by people. American science digest report in 1978, silver can kill 650 kinds of different pathogen.Different with antibiotic, silver can be without distinction Effectively kill various bacteriums, fungi/saccharomycete, virus, mycoplasma and helminth etc..And extremely low concentration, in every liter of water As long as the silver ion for containing 2/1sts milligrams, most of bacterium in water can be killed.Silver sterilizing ability it is strong, to people and animals without Evil, thus airline more than half using silver come purifying drinking water, the swimming pools of many countries using silver ion disinfection and sterilization, Silver ion for sterilization also comes into the appliance fields such as washing machine.Silver ion for sterilization also will play its great function in medical field.
Summary of the invention
In order to solve the combination of implantation materials microstructure and infection problems, the present invention provides a kind of medical embedded material use Magnesium-silver coating and preparation method thereof, using evaporation coating technique, titanium, titanium alloy, stainless steel, high molecular material preparation entity or Porous structure matrix surface prepares magnesium-silver coating, and existing implantation material structure compatibility is not good enough and infection problems to solve, the party Coating obtained by method has splendid biocompatibility, is provided simultaneously with sterilizing function.
Technical scheme is as follows:
A kind of medical embedded material magnesium-silver coating, it is characterised in that: magnesium-silver coating applies with a thickness of 0.1-200 μm The mass percent of silver element in layer are as follows: 0% < Ag≤10% (preferably 2%≤Ag≤6%).
Wherein, matrix used is entity or porous structure, is made of titanium, titanium alloy, stainless steel or high molecular material;Institute It is medical material with entity matrix;Kong Xi Shuai≤80% of porous structure matrix used, aperture are 200 μm of -5mm.
Zn-ef ficiency can be also introduced in coating of the present invention as a preferred technical solution, mass percent is 0% < Zn≤8%, to improve its anti-microbial property.
The present invention also provides the preparation methods of the magnesium-silver coating, it is characterised in that: uses vapour deposition method by magnesium silver alloy Raw material evaporation, and steam is transported to matrix surface with carrier gas and obtains magnesium coating;Or magnesium silver steam is sunk using temperature gradient Product is in matrix surface.
Magnesium-silver coating preparation method of the present invention, it is characterised in that: the magnesium silver alloy raw material is fusing casting It obtains, silver material is the fine silver granules of Chun Du≤99.99%, and magnesium raw material is the pure magnesium granules of Chun Du≤99.99%.
As preferred technique, the flow of carrier gas is 50-300SCCM, and operating air pressure is 1 × 10-4-1×102Pa, magnesium silver Alloy evaporating temperature is 500-800 DEG C, and depositing temperature is 20-150 DEG C.
The present invention prepares magnesium-silver coating, and specific step is as follows:
(1), after matrix successively to be used to deionized water, dehydrated alcohol ultrasonic cleaning, settling chamber is sent into drying nitrogen drying;
(2), magnesium silver alloy raw material is put into vaporization chamber, takes out ultimate vacuum to 10-5Pa cleans minimum 3 with high-purity argon gas repeatedly It is secondary, to remove air, guarantee oxygen-free environment;
(3), settling chamber is warming up to target temperature, and magnesium silver is evaporated to vapor deposition after the completion of matrix surface, deposition with furnace It is cooled to room temperature.
The beneficial effects of the present invention are:
1, the present invention proposes that a kind of medical embedded material magnesium-silver coating, magnesium metal have good biocompatibility, magnesium Chemical reaction occurs with body fluid and degrades, catabolite can be excreted with body metabolism.Magnesium also has self-bone grafting, vascularization promoting etc. Multi-biological functional.Silver has very strong broad-spectrum bactericidal action.Silver may additionally facilitate fibroblast differentiation, to promote wound Healing.Antibacterial, promoting healing and histotrophic multi-biological functional will be played by preparing magnesium-silver coating on implant devices surface.
2, the method for prepares coating proposed by the present invention can coat certain thickness on a variety of orthopedic implanting material surfaces Magnesium-silver coating is suitable for a variety of surfaces, does not need to carry out material surface specially treated, applied widely.
3, the present invention solves the problems, such as that mg-based material is only used for non-bearing position, and the application field of mg-based material is expanded A possibility that opening up bearing position, improving mg-based material application.
Detailed description of the invention
Fig. 1 is depositing device schematic diagram in embodiment 1.In figure, 1 settling chamber's furnace body;2 vaporization chamber furnace bodies;3, matrix;4, it steams It rises;5, vacuum system;6, flow controller;7, dehydration and deoxidation pipe;8, argon gas.
Specific embodiment
As shown in Figure 1, depositing device used in the method for the present invention specifically includes that settling chamber's furnace body 1, vaporization chamber furnace body 2 etc., Matrix 3 is placed in settling chamber's furnace body 1, and evaporation source 4, one end of evaporation source 4 and flow controller are placed in vaporization chamber furnace body 2 6 one end connection, the other end of flow controller 6 connect dehydration and deoxidation pipe 7, and 7 other end of dehydration and deoxidation pipe connects argon gas supply The other end of pipeline, evaporation source 4 is communicated with the settling chamber where matrix 3, and the settling chamber where matrix 3 is communicated with vacuum system 5.
The present invention uses vacuum evaporation system prepares coating, and magnesium silver alloy block or particle are evaporation source, and argon gas is carrier gas, Equipment drawing is as shown in Figure 1.Porous titanium alloy (Ti-6Al-4V) rest body is prepared by 3D printing technique, Kong Xi Shuai≤80%, hole Diameter is 200 μm of -1mm, and reticulated vitreous carbon rest body is infusion process preparation, and Kong Xi Shuai≤80%, aperture is 500 μm of -5mm, branch Frame matrix sample need to be washed through pickling, after alcohol washes, drying nitrogen drying, then it is placed in settling chamber's furnace body 1.
Embodiment 1
Porous titanium alloy (Ti-6Al-4V) sample is placed in settling chamber's furnace body 1, MgAg alloy raw material is put into vaporization chamber furnace Then body 2 connects gas circuit, and checks sealing condition, take out ultimate vacuum (10-5Pa after), argon gas cleans whole system 3 times repeatedly, To ensure that oxygen content is preferably minimized.20 DEG C of depositing temperature of setting, evaporating temperature are 500 DEG C, and operating air pressure is 1 × 10-4Pa sinks Product time 1h, for deposited metal magnesium-silver layer with a thickness of 5 μm, silver-colored mass percent is 2%.For determine coating rush osteogenic action, Alkaline phosphatase (ALP) experiment is carried out, after culture 4 days and 7 days, coating group color is deeper than matrix group, illustrates coating group The activity of alkaline phosphatase is higher than matrix group, shows that coating has and promotees osteogenic action.
Embodiment 2
The pure matrix of plane is placed in settling chamber's furnace body 1, MgAg alloy raw material is put into vaporization chamber furnace body 2, then connects gas Road, and check sealing condition, take out ultimate vacuum (10-5Pa after), argon gas cleans whole system 3 times repeatedly, to ensure oxygen content It is preferably minimized.80 DEG C of depositing temperature of setting, evaporating temperature are 600 DEG C, and operating air pressure is 1 × 10-3Pa, sedimentation time 1h, deposition For magnesium metal-silver layer with a thickness of 50 μm, silver-colored mass percent is 3%.By X-ray diffraction analysis and scanning electron microscope power spectrum Analysis determines that coating is magnesium silver, and since silver content is less, X-ray map can only show the diffraction information of magnesium metal.
Embodiment 3
Plane 316L stainless steel thin slice is placed in settling chamber's furnace body 1, MgAg alloy raw material is put into vaporization chamber furnace body 2, so After connect gas circuit, and check sealing condition, take out ultimate vacuum (10-5Pa after), argon gas cleans whole system 3 times repeatedly, to ensure Oxygen content is preferably minimized.100 DEG C of depositing temperature of setting, evaporating temperature are 700 DEG C, working vacuum degree 1 × 10-1Pa, when deposition Between 1.5h, for deposited metal magnesium-silver layer with a thickness of 100 μm, silver-colored mass percent is 4%.
Embodiment 4
Plane macromolecule thin slice is placed in settling chamber's furnace body 1, MgAg alloy raw material is put into vaporization chamber furnace body 2, is then connected Gas circuit is connect, and checks sealing condition, takes out ultimate vacuum (10-5Pa after), argon gas cleans whole system 3 times repeatedly, to ensure oxygen Content is preferably minimized.50 DEG C of depositing temperature of setting, evaporating temperature are 750 DEG C, working vacuum degree 1Pa, sedimentation time 1h, deposition gold Belong to magnesium-silver layer with a thickness of 120 μm, silver-colored mass percent is 5%.
Embodiment 5
Porous titanium alloy (Ti-6Al-4V) sample is placed in settling chamber's furnace body 1, MgAg alloy raw material is put into vaporization chamber furnace Then body 2 connects gas circuit, and checks sealing condition, take out ultimate vacuum (10-5Pa after), argon gas cleans whole system 3 times repeatedly, To ensure that oxygen content is preferably minimized.150 DEG C of depositing temperature of setting, evaporating temperature are 800 DEG C, working vacuum degree 10Pa, deposition Time 2h, for deposited metal magnesium-silver layer with a thickness of 150 μm, silver-colored mass percent is 4.5%.
Embodiment 6
Plane titanium alloy (Ti-6Al-4V) sample is placed in settling chamber's furnace body 1, MgAg alloy raw material is put into vaporization chamber furnace Then body 2 connects gas circuit, and checks sealing condition, take out ultimate vacuum (10-5Pa after), argon gas cleans whole system 3 times repeatedly, To ensure that oxygen content is preferably minimized.120 DEG C of depositing temperature of setting, evaporating temperature are 650 DEG C, working vacuum degree 1 × 10-2Pa, Sedimentation time 1h, for deposited metal magnesium-silver layer with a thickness of 100 μm, silver-colored mass percent is 6%.
Embodiment 7
Plane titanium alloy (Ti-6Al-4V) sample is placed in settling chamber's furnace body 1, MgAgZn alloy raw material is put into vaporization chamber Then furnace body 2 connects gas circuit, and checks sealing condition, take out ultimate vacuum (10-5Pa after), argon gas cleans whole system 3 repeatedly It is secondary, to ensure that oxygen content is preferably minimized.120 DEG C of depositing temperature of setting, evaporating temperature are 650 DEG C, working vacuum degree 1 × 10- 2Pa, sedimentation time 1h, deposited metal magnesium-silver layer is with a thickness of 100 μm, and the mass percent of Zn is 5%, silver-colored mass percent It is 6%.
By sample according to " JIS Z 2801-2000 " antibacterial fabricated product-antibiotic property test method and antibacterial effect ", The correlation standards such as GB/T 2591-2003 " antibiotic plastic anti-microbial property experimental method and antibacterial effect " " carry out quantitative resist Bacterium performance detection.As a result obtain sample is to the sterilizing rate after frequent infectious bacteria (Escherichia coli, staphylococcus aureus) effect 99% or more.
Embodiment the result shows that, the present invention has the metal for promoting osteogenic action and antibacterial action using evaporation coating technique preparation Magnesium-silver or magnesium-silver-spelter coating.Coating is prepared in porous material with complex geometry shape, planar materials surface.Using The technology can provide magnesium-silver or magnesium-effective covering of silver-spelter coating, can assign while improving medical material Bone Ingrowth ability Give material anti-microbial property.
The above embodiments merely illustrate the technical concept and features of the present invention, and its object is to allow person skilled in the art Scholar cans understand the content of the present invention and implement it accordingly, and it is not intended to limit the scope of the present invention.It is all according to the present invention Equivalent change or modification made by Spirit Essence, should be covered by the protection scope of the present invention.

Claims (10)

1. a kind of medical embedded material magnesium-silver coating, it is characterised in that: magnesium-silver coating is with a thickness of 0.1-200 μm, coating The mass percent of middle silver element are as follows: 0% < Ag≤10%.
2. according to magnesium-silver coating described in claim 1, it is characterised in that: the mass percent of silver element in coating are as follows: 2%≤ Ag≤6%.
3. according to magnesium-silver coating as claimed in claim 1 or 2, it is characterised in that: matrix used is entity or porous structure, is used Titanium, titanium alloy, stainless steel or high molecular material are made.
4. according to magnesium-silver coating described in claim 3, it is characterised in that: entity matrix used is medical material;Porous knot used Kong Xi Shuai≤80% of structure matrix, aperture are 200 μm of -5mm.
5. according to magnesium-silver coating as claimed in claim 1 or 2, it is characterised in that: introduce Zn-ef ficiency, quality hundred in the coating Divide than being 0% < Zn≤8%.
6. magnesium-silver coating preparation method described in a kind of claim 1, it is characterised in that: steamed magnesium silver alloy using vapour deposition method Hair, and steam is transported to matrix surface with carrier gas and obtains magnesium coating;Or utilize temperature gradient by magnesium silver vapor deposition in base Body surface face.
7. according to magnesium-silver coating preparation method described in claim 6, it is characterised in that: the flow of carrier gas is 50-300SCCM, Operating air pressure is 1 × 10-4-1×102Pa。
8. according to magnesium-silver coating preparation method described in claim 6, it is characterised in that: magnesium silver alloy evaporating temperature is 500- 800 DEG C, depositing temperature is 20-150 DEG C.
9. according to magnesium-silver coating preparation method described in claim 6, which is characterized in that specific preparation process is as follows:
(1), after matrix successively to be used to deionized water, dehydrated alcohol ultrasonic cleaning, settling chamber is sent into drying nitrogen drying;
(2), magnesium silver alloy raw material is put into vaporization chamber, takes out ultimate vacuum to 10-5Pa is cleaned minimum 3 times repeatedly with high-purity argon gas, with Air is removed, guarantees oxygen-free environment;
(3), settling chamber is warming up to target temperature, and magnesium silver is evaporated to vapor deposition furnace cooling after the completion of matrix surface, deposition To room temperature.
10. a kind of application of the coating described in claim 1 on medical embedded material, it is characterised in that: the medical embedded material Material is to need implantation material used in bearing position.
CN201710935102.6A 2017-10-10 2017-10-10 A kind of medical embedded material magnesium-silver coating and preparation method thereof Pending CN109652769A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201710935102.6A CN109652769A (en) 2017-10-10 2017-10-10 A kind of medical embedded material magnesium-silver coating and preparation method thereof

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201710935102.6A CN109652769A (en) 2017-10-10 2017-10-10 A kind of medical embedded material magnesium-silver coating and preparation method thereof

Publications (1)

Publication Number Publication Date
CN109652769A true CN109652769A (en) 2019-04-19

Family

ID=66109351

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201710935102.6A Pending CN109652769A (en) 2017-10-10 2017-10-10 A kind of medical embedded material magnesium-silver coating and preparation method thereof

Country Status (1)

Country Link
CN (1) CN109652769A (en)

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112111774A (en) * 2020-08-21 2020-12-22 广东机电职业技术学院 Preparation method of antibacterial micro-arc oxidation film layer
CN113368314A (en) * 2021-05-20 2021-09-10 沈阳理工大学 Magnesium-based metal polymer composite bone guiding regeneration membrane and preparation method thereof
CN114369808A (en) * 2021-12-20 2022-04-19 中国兵器科学研究院宁波分院 Method for preparing antibacterial coating on surface of magnesium and magnesium alloy
CN116815107A (en) * 2023-05-29 2023-09-29 北京大学第三医院(北京大学第三临床医学院) Composite alloy material and preparation method and application thereof

Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101516292A (en) * 2006-09-22 2009-08-26 友和安股份公司 Implants comprising biodegradable metals and method for manufacturing the same
CN102618829A (en) * 2011-01-31 2012-08-01 乐普(北京)医疗器械股份有限公司 Medical magnesium alloy material with amorphous film and preparation method thereof
US20130266616A1 (en) * 2012-04-09 2013-10-10 Ki-Deog Park Method of manufacturing bone graft materials and bone graft materials manufactured thereby
CN103614601A (en) * 2013-12-16 2014-03-05 苏州奥芮济医疗科技有限公司 In-vivo controlled degradable bacteriostatic Mg-Ag-Zn-Mn magnesium alloy implant material and preparation method thereof
CN104593650A (en) * 2013-11-01 2015-05-06 上海交通大学医学院附属第九人民医院 Biodegradable and absorbable magnesium-zinc-copper alloy with antibiotic function, and application thereof
CN107119260A (en) * 2016-02-24 2017-09-01 中国科学院金属研究所 A kind of bone implantation magnesium-copper coating and preparation method thereof

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101516292A (en) * 2006-09-22 2009-08-26 友和安股份公司 Implants comprising biodegradable metals and method for manufacturing the same
CN102618829A (en) * 2011-01-31 2012-08-01 乐普(北京)医疗器械股份有限公司 Medical magnesium alloy material with amorphous film and preparation method thereof
US20130266616A1 (en) * 2012-04-09 2013-10-10 Ki-Deog Park Method of manufacturing bone graft materials and bone graft materials manufactured thereby
CN104593650A (en) * 2013-11-01 2015-05-06 上海交通大学医学院附属第九人民医院 Biodegradable and absorbable magnesium-zinc-copper alloy with antibiotic function, and application thereof
CN103614601A (en) * 2013-12-16 2014-03-05 苏州奥芮济医疗科技有限公司 In-vivo controlled degradable bacteriostatic Mg-Ag-Zn-Mn magnesium alloy implant material and preparation method thereof
CN107119260A (en) * 2016-02-24 2017-09-01 中国科学院金属研究所 A kind of bone implantation magnesium-copper coating and preparation method thereof

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112111774A (en) * 2020-08-21 2020-12-22 广东机电职业技术学院 Preparation method of antibacterial micro-arc oxidation film layer
CN112111774B (en) * 2020-08-21 2022-04-08 广东机电职业技术学院 Preparation method of antibacterial micro-arc oxidation film layer
CN113368314A (en) * 2021-05-20 2021-09-10 沈阳理工大学 Magnesium-based metal polymer composite bone guiding regeneration membrane and preparation method thereof
CN114369808A (en) * 2021-12-20 2022-04-19 中国兵器科学研究院宁波分院 Method for preparing antibacterial coating on surface of magnesium and magnesium alloy
CN114369808B (en) * 2021-12-20 2024-02-06 中国兵器科学研究院宁波分院 Method for preparing antibacterial coating on surface of magnesium and magnesium alloy
CN116815107A (en) * 2023-05-29 2023-09-29 北京大学第三医院(北京大学第三临床医学院) Composite alloy material and preparation method and application thereof

Similar Documents

Publication Publication Date Title
He et al. Biocompatibility, corrosion resistance and antibacterial activity of TiO2/CuO coating on titanium
CN107119260B (en) A kind of bone implant magnesium-copper coating and preparation method thereof
CN113527748B (en) Polyether-ether-ketone surface modification method, polyether-ether-ketone obtained through modification and application of polyether-ether-ketone
CN109652769A (en) A kind of medical embedded material magnesium-silver coating and preparation method thereof
Zhang et al. Sr/ZnO doped titania nanotube array: an effective surface system with excellent osteoinductivity and self-antibacterial activity
Xue et al. Rapid construction of polyetheretherketone (PEEK) biological implants incorporated with brushite (CaHPO4· 2H2O) and antibiotics for anti-infection and enhanced osseointegration
Mahmoudi et al. Antibacterial Ti–Cu implants: A critical review on mechanisms of action
Zhang et al. Evaluation of osteogenic and antibacterial properties of strontium/silver‐containing porous TiO2 coatings prepared by micro‐arc oxidation
Shimabukuro et al. Investigation of realizing both antibacterial property and osteogenic cell compatibility on titanium surface by simple electrochemical treatment
CN100551450C (en) A kind of preparation method of antiseptic biological active titanium coating
Chen et al. Improvement in antibacterial properties and cytocompatibility of titanium by fluorine and oxygen dual plasma-based surface modification
Han et al. Mg/Ag ratios induced in vitro cell adhesion and preliminary antibacterial properties of TiN on medical Ti-6Al-4V alloy by Mg and Ag implantation
CN107937880B (en) Method for modifying surface of metal material, product and application thereof
Lan et al. Promoting bone mesenchymal stem cells and inhibiting bacterial adhesion of acid-etched nanostructured titanium by ultraviolet functionalization
CN108853604A (en) A method of quickly eliminating bone implant surface bacteria biomembrane using near-infrared
Si et al. A heterogeneous TiO2/SrTiO3 coating on titanium alloy with excellent photocatalytic antibacterial, osteogenesis and tribocorrosion properties
Shimabukuro et al. Investigation of antibacterial effect of copper introduced titanium surface by electrochemical treatment against facultative anaerobic bacteria
CN101791433B (en) Molecular sieve antibacterial coating with pure titanium or titanium alloy surface and preparation method thereof
CN112402693A (en) Orthopedic implant instrument with surface provided with bone promoting coating and preparation method
CN106562827A (en) Hydrophilic and antibacterial dental implant system and manufacturing method thereof
CN103751841B (en) A kind of modification medical titanium metal material and preparation method thereof
CN107829123B (en) Aluminum alloy with double-layer coating on surface and preparation method and application thereof
CN106637121B (en) A kind of medical titanium metal alkyl materials and its manufacturing method
CN109652768A (en) A kind of medical embedded material magnesium-strontium coating and preparation method thereof
CN108295307A (en) A kind of bone implantation calcium phosphorous compound-magnesium composite coating and preparation method thereof

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
RJ01 Rejection of invention patent application after publication

Application publication date: 20190419

RJ01 Rejection of invention patent application after publication