CN101003889A - Surface process technique for artificial joint, bone lamella, and bone nail coated by Nano diamond - Google Patents
Surface process technique for artificial joint, bone lamella, and bone nail coated by Nano diamond Download PDFInfo
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- CN101003889A CN101003889A CN 200710003306 CN200710003306A CN101003889A CN 101003889 A CN101003889 A CN 101003889A CN 200710003306 CN200710003306 CN 200710003306 CN 200710003306 A CN200710003306 A CN 200710003306A CN 101003889 A CN101003889 A CN 101003889A
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Abstract
This invention relates to a method for surface-treating artificial joints, bone plates and bone nails with diamond nanofilm. The method utilizes diamond nanofilm for surface modification of Ti alloys, to solve the problems of releasing trace ions, polluting tissues and inducing inflammation, and produce qualified artificial joints, bone plates and bone nails. The method adequately utilizes good biocompatibility and chemical stability of diamond nanofilm. The method adopts chemical or physical vapor deposition to coat Ti alloy substrate with 100 nm-3 mum thick diamond nanofilm or diamond-like carbon nanofilm. After post treatment, the diamond nanofilm can covalently bond molecular interface with high biocompatibility in human tissues.
Description
Technical field
The invention belongs to technical field of biological material, relate to film deposition techniques, particularly titanium alloy surface is modified as the technology of joint prosthesis, Steel Plate For Fixation Of Fracture and the nail of orthopaedics use.
Background technology
Titanium alloy is the functional materials of aspect widespread uses such as orthopaedics, dentistry, plastic surgery.But titanium alloy material still exists and can discharge by micro ion in the state of implant into body, pollutes tissue, causes the problem of untoward reactions such as inflammation.And diamond film has the chemical stability and the excellent biological compatibility of maximum hardness, low-friction coefficient, the best, and therefore, depositing diamond film has the value of practical application on the medical material surface.
Summary of the invention
Purpose of the present invention, provide a kind of employing chemical vapor coating method or physical vapor vapour deposition method, process for modifying surface to associated materials such as titanium alloy artificial joint, hone lamella and nail etc., this nano-diamond film or diamond-like carbon film can be implemented the rear surface again and handle, to cooperate the different tissue consistency demands of implanting environment and position.Method is with after the titanium alloy article surface pre-treatment that is shaped, through chemical vapor coating method or physical vapor vapour deposition method the titanium alloy substrate is coated with, thickness is nano-diamond film or the diamond-like carbon film of 100nm～3 μ m, this diamond thin can be implemented the rear surface again and handle, the rear surface processing mode is meant with hydrogen plasma displacement surface molecular, ion or atom, again with aldehyde radical, the reaction of compound such as amido or thiohydroxy, with covalent bonds the other end fixed dna, protein, peptide, or micromolecular interface layer, the chemical stability that makes full use of diamond film excellent biological compatibility and the best is a functional materials, to cooperate the functional requirement of varying environment and position.
Description of drawings
Fig. 1 is the structural representation of diamond or diamond-like carbon film coating joint prosthesis, hone lamella or nail;
Fig. 2 is the synoptic diagram of diamond high-biocompatibility surface modification treatment process;
Fig. 3 is high SP
3The Raman spectrogram of structural content diamond film;
Fig. 4 is low SP
3The Raman spectrogram of structural content diamond-like carbon film.
Among the figure: 1. the metal sheet carrier of joint prosthesis, hone lamella or nail, 2. high-density stratum nucleare or metallic carbide middle layer, 3. diamond or diamond-like carbon plated film, 4. interface layer is handled in the rear surface.
Embodiment
With reference to each accompanying drawing, the making method of substrate of the present invention is specified as: the diamond coated or diamond-like carbon film coating 3 of applying nano, and to the process for modifying surface of associated metal plate solid support materials 1 such as titanium alloy artificial joint, hone lamella and nail.Method is: after the titanium alloy article surface pre-treatment that will be shaped, through chemical vapor coating method or physical vapor vapour deposition method the titanium alloy substrate is coated with, thickness is nano-diamond film or the diamond-like carbon film 3 of 100nm～3 μ m, this diamond thin can be implemented the rear surface again and handle, in conjunction with the high molecule interface layer 4 of tissue consistency, implant the tissue compatible sexual demands of environment and position with covalent to cooperate difference.
Because answer the demand of different qualities, plated film of the present invention is divided into dual mode, and is as described below.
First kind, refer to contain SP
3The carbon atom bond structure is higher than the nano polycrystal diamond film production of 70% content.For the density that improves coated by Nano diamond bonding strength and nucleating layer 2 greater than 10
9Cm
-1The surface of metal sheet solid support materials 1 such as joint prosthesis, hone lamella and nail uses acid or alkaline solution to handle in advance, microdiamond suspension 400w cleaned by ultrasonic vibration 10-20min by particle diameter 30 μ m, reach 0.3 μ m Nano diamond suspension and be two-part ultra-sonic oscillation processing 10-20min, dry up standby after cleaning with acetone ultrasonic wave mode at last.
And control nucleation period negative bias (Bias) to be worth in 100-280V and reaction gas pressure be 0.8-3.5Kpa.Use 0.1～3.0% CH
4, 20～70% Ar
2And 79.9～27% H
2Mixed gas, plated film under the plasma environment of 500～2100 ℃ chemical vapor coating methods.Above-mentioned chemical vapor coating environment can utilize following method to obtain: hot filament CVD (HFCVD), DC plasma and chemical gas-phase deposition method (DCPCVD), the direct-current plasma spraying method, radio-frequency plasma vapour deposition process (RFPCVD), the high frequency plasma vapour deposition process, the direct current arc electric discharge, microwave plasma CVD method (MWPCVD), ion beam depositing method (IBD) or low-pressure chemical vapor deposition relevant devices such as (LPCVD) are made for the diamond nano film coating 3 that thickness is lower than 3 μ m.
Second kind, refer to contain SP
3The carbon atom bond structure be lower than the nanometer diamond-like carbon film (DLC) of 70% content.Diamond-like carbon plated film (3) is made, generate the diamond-like carbon film that thickness is lower than 1 μ m with physical vapor evaporation environment, this evaporation environment refers to utilize relevant devices such as evaporation (Evaporation Deposition) mode, ion plating (Ion Plating) mode or sputter (Sputtering Deposition) mode, make thickness and be lower than 1 μ m, the diamond-like carbon film deposition 3 of no hydrogen richness realizes hanging down nano level diamond-like carbon (DLC) the film coating of pin hole rate.For improving the surface bonding strength of metal sheet solid support materials 1 such as joint prosthesis, hone lamella and nail, the making of nanometer diamond-like carbon (DLC) film, use earlier metal and graphite to generate the metallic carbide middle layer 2 that thickness is lower than 30nm as the target evaporation, re-using graphite target is raw material, generates the diamond-like carbon film coating that thickness is lower than 1 μ m under physical vapor evaporation environment.
Can implement the rear surface after above-mentioned first and second kind diamond thin or diamond-like carbon film generate again and handle, with covalent in conjunction with the high molecule interface layer 4 of tissue consistency, with the demand of the implantation sexual function that cooperates varying environment and position.The rear surface processing mode is meant with hydrogen plasma displacement surface molecular, ion or atom, again with compound reactions such as aldehyde radical, amido or thiohydroxys, with covalent bonds the other end fixed dna, protein, peptide or micromolecular interface layer, to cooperate the functional requirement of varying environment and position.
Embodiment 1: the diamond coated process for modifying surface to titanium alloy artificial joint, hone lamella and nail material of applying nano
Method is with after the titanium alloy article surface pre-treatment that is shaped, through the chemical vapor coating method titanium alloy substrate is coated with, contain SP3 carbon atom bond structure and be higher than the nano-diamond film 3 that 70% content thickness is 100nm～3 μ m, diamond thin 3 can be implemented the rear surface again and handle, with covalent in conjunction with the high molecule interface layer 4 of tissue consistency.
Implementation method is: associated materials surfaces such as joint prosthesis, hone lamella and nail use acid or alkaline solution to handle in advance, by particle diameter 30 μ m microdiamond suspension 400w cleaned by ultrasonic vibration 10-20min, reach 0.3 μ m Nano diamond suspension and be two-part ultra-sonic oscillation processing 10-20min, dry up standby after cleaning with acetone ultrasonic wave mode at last.And control nucleation period negative bias (Bias) to be worth in 100-280V and reaction gas pressure be 0.8-3.5Kpa, to improve coated by Nano diamond plated film bonding strength and nucleation (2) density greater than 10
9Cm
-1Use 0.1～3.0% CH
4, 20～70% Ar
2And 79.9～27% H
2Mixed gas, evaporation under 800 ℃ microwave plasma CVD method (MWPCVD) environment forms the nano-diamond membrane coating 3 that thickness is lower than 3 μ m.
This nano-diamond film can be implemented the rear surface again and handle, with hydrogen plasma displacement surface molecular, ion or atom, again with compound reactions such as aldehyde radical, amido or thiohydroxys, with covalent bonds the other end fixed dna, protein, peptide or micromolecular interface layer 4, to cooperate the different tissue consistency demands of implanting environment and position.
Embodiment 2: the application class diamond-like carbon film is to the process for modifying surface of titanium alloy artificial joint, hone lamella and nail material.Method is after the article surface pre-treatment with the titanium alloy that is shaped, through the physical vapor vapour deposition method titanium alloy substrate to be coated with, and contains SP
3The carbon atom bond structure is lower than the diamond-like carbon film 3 that 70% content thickness is lower than 1 μ m, and this diamond-like carbon film cooperates the different tissue consistency demands of implanting environment and position, implements the rear surface again and handles binding molecule interface layer 4.
Implementation method is: behind the titanium alloy artificial joint that will be shaped, hone lamella and the nail article surface cleaning-drying; Use metal and graphite target to generate the metallic carbide middle layer 2 that thickness is lower than 30nm, for improving bonding strength in physical vapor sputter (Sputtering Deposition) mode; Re-using graphite target is raw material, generates under physics gas physical vapor sputtering way, and thickness is lower than the diamond-like carbon film coating 3 that 1 μ m does not have hydrogen richness.
This diamond-like carbon film can be implemented the rear surface again and handle, with hydrogen plasma displacement surface molecular, ion or atom, again with compound reactions such as aldehyde radical, amido or thiohydroxys, with covalent bonds the other end fixed dna, protein, peptide or micromolecular interface layer 4, to cooperate the different tissue consistency demands of implanting environment and position.
Claims (8)
1. the process for treating surface of a coated by Nano diamond joint prosthesis, hone lamella and nail, it is the applying nano technology, titanium alloy is carried out surface modification, make it to meet the requirement that is used to make joint prosthesis, hone lamella and nail, it is characterized in that: after the titanium alloy object that will be shaped is done surperficial pre-treatment, through chemical vapor coating method or physical vapor vapour deposition method the titanium alloy substrate is coated with, generation thickness is nano-diamond film or the diamond-like carbon film of 100nm～3 μ m; This diamond thin can be implemented the rear surface again and handle, with covalent binding molecule interface layer.
2. the process for treating surface of coated by Nano diamond joint prosthesis as claimed in claim 1, hone lamella and nail, it is characterized in that: plated body can use various titanium alloy artificial joints, hone lamella and the nail material that is shaped in advance, according to actual demand, be processed into the size that matches.
3. the process for treating surface of coated by Nano diamond joint prosthesis as claimed in claim 1, hone lamella and nail, it is characterized in that: surface treatment titanium alloy substrate in advance, can use acid or alkaline solution to handle, vibrate by particle diameter 30 μ m microdiamond suspension, 400W ultrasonic wave and clean 10-20min; Or do the two-part ultra-sonic oscillation with the Nano diamond suspension of 0.3 μ m and handle 10-20min, standby with drying up after the acetone ultrasonic cleaning again.
4. the process for treating surface of coated by Nano diamond joint prosthesis as claimed in claim 1, hone lamella and nail is characterized in that: coated by Nano diamond is to increase the nucleation density of early growth period greater than 10
9Cm
-1, control nucleation period negative bias values is 100-280V, reaction gas pressure is 0.8-3.5Kpa; Use 0.1～3.0% CH
4, 99.9～97% H
2And 99.9～97% H
2Mixed gas is grown under 500～2100 ℃ plasma environment, and content is higher than 70% SP
3The glomerocryst nano-diamond membrane of carbon atom bond structure generates the nano-diamond membrane coating that thickness is lower than 3 μ m under the chemical vapor coating environment.
5. coated by Nano diamond joint prosthesis as claimed in claim 1, the process for treating surface of hone lamella and nail is characterized in that: described chemical vapor coating method refers to utilize hot filament CVD (HFCVD), DC plasma and chemical gas-phase deposition method (DCPCVD), the direct-current plasma spraying method, radio-frequency plasma vapour deposition process (RFPCVD), the high frequency plasma vapour deposition process, the direct current arc electric discharge, microwave plasma CVD method (MWPCVD), ion beam depositing method (IBD) or low-pressure chemical vapor deposition methods involving growing diamond films such as (LPCVD).
6. the process for treating surface of coated by Nano diamond joint prosthesis as claimed in claim 1, hone lamella and nail, it is characterized in that: the physical vapor vapour deposition method of described diamond-like carbon film coating, refer to utilize relevant processing procedure such as evaporation (Evaporation Deposition) mode, ion plating (Ion Plating) mode or sputter (SputteringDeposition) mode to generate, make plated film reach the diamond-like carbon film deposition of no hydrogen, realize the nano level plated film of low pin hole rate, this film is that content is lower than 70% SP
3Carbon atom bond structure thing.
7. the process for treating surface of coated by Nano diamond joint prosthesis as claimed in claim 1, hone lamella and nail, it is characterized in that: the vapour deposition method of described diamond-like carbon plated film, earlier use metal and graphite to be target, under physical vapor evaporation environment, generate the metallic carbide middle layer that thickness is lower than 30nm, re-using graphite target is raw material, generates the diamond-like carbon film coating that thickness is lower than 1 μ m under physical vapor evaporation environment.
8. the process for treating surface of coated by Nano diamond joint prosthesis as claimed in claim 1, hone lamella and nail, it is characterized in that: described rear surface processing mode, be meant with hydrogen plasma displacement surface molecular, ion or atom, again with compound reactions such as aldehyde radical, amido or thiohydroxys, with covalent bonds the other end fixed dna, protein, peptide or micromolecular interface layer, to cooperate the functional requirement of varying environment and position.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200710003306 CN101003889A (en) | 2007-02-05 | 2007-02-05 | Surface process technique for artificial joint, bone lamella, and bone nail coated by Nano diamond |
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|---|---|---|---|
| CN 200710003306 CN101003889A (en) | 2007-02-05 | 2007-02-05 | Surface process technique for artificial joint, bone lamella, and bone nail coated by Nano diamond |
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| CN101003889A true CN101003889A (en) | 2007-07-25 |
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| CN 200710003306 Pending CN101003889A (en) | 2007-02-05 | 2007-02-05 | Surface process technique for artificial joint, bone lamella, and bone nail coated by Nano diamond |
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2009130073A1 (en) * | 2008-04-25 | 2009-10-29 | Scortecci Gerard | Bone regeneration device |
| CN102051579A (en) * | 2011-01-25 | 2011-05-11 | 中山大学 | Method for preparing carboxyl modified layer on surface of diamond-like carbon (DLC) film and DLC film prepared by method |
| CN102181842A (en) * | 2011-04-14 | 2011-09-14 | 中国科学院上海硅酸盐研究所 | Method for modifying titanium surface |
| CN102958470A (en) * | 2010-07-09 | 2013-03-06 | 斯恩蒂斯有限公司 | Self-detaching layer for easy implant removal |
| CN103866242A (en) * | 2014-03-20 | 2014-06-18 | 常州康鼎医疗器械有限公司 | Physical vapor deposition (PVD) surface coating technique of medical instruments |
| CN106637038A (en) * | 2016-09-21 | 2017-05-10 | 柳州市西朗能源科技有限公司 | Machine for manufacturing nano diamond thin coating film |
| CN107106835A (en) * | 2014-10-28 | 2017-08-29 | 澳大利亚国家Ict有限公司 | The method for forming shell |
| CN107475686A (en) * | 2017-06-30 | 2017-12-15 | 湖北大学 | A kind of preparation method based on ald zirconium oxide corrosion resistance ceramic membrane |
| CN109536804A (en) * | 2018-12-05 | 2019-03-29 | 湖北第二师范学院 | Tantalum alloy, diamond-like-carbon coating tantalum alloy and diamond-like-carbon coating biomedicine implantation tantalum alloy bone pawl and preparation method thereof |
| CN109563612A (en) * | 2016-05-06 | 2019-04-02 | 阿尔托大学注册基金会 | Detonation Nano diamond and diamond-like-carbon are co-deposited to the method on substrate and the composite membrane comprising detonation Nano diamond and diamond-like-carbon |
| CN112593204A (en) * | 2021-03-02 | 2021-04-02 | 中南大学湘雅医院 | Diamond film for scalpel and preparation method thereof |
-
2007
- 2007-02-05 CN CN 200710003306 patent/CN101003889A/en active Pending
Cited By (15)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| FR2930423A1 (en) * | 2008-04-25 | 2009-10-30 | Gerard Scortecci | DEVICE FOR BONE REGENERATION |
| WO2009130073A1 (en) * | 2008-04-25 | 2009-10-29 | Scortecci Gerard | Bone regeneration device |
| CN102958470B (en) * | 2010-07-09 | 2016-04-20 | 斯恩蒂斯有限公司 | For being easy to the self-separation layer removing implant |
| CN102958470A (en) * | 2010-07-09 | 2013-03-06 | 斯恩蒂斯有限公司 | Self-detaching layer for easy implant removal |
| CN102051579A (en) * | 2011-01-25 | 2011-05-11 | 中山大学 | Method for preparing carboxyl modified layer on surface of diamond-like carbon (DLC) film and DLC film prepared by method |
| CN102051579B (en) * | 2011-01-25 | 2013-04-10 | 中山大学 | Method for preparing carboxyl modified layer on surface of diamond-like carbon (DLC) film and DLC film prepared thereby |
| CN102181842A (en) * | 2011-04-14 | 2011-09-14 | 中国科学院上海硅酸盐研究所 | Method for modifying titanium surface |
| CN103866242A (en) * | 2014-03-20 | 2014-06-18 | 常州康鼎医疗器械有限公司 | Physical vapor deposition (PVD) surface coating technique of medical instruments |
| CN107106835A (en) * | 2014-10-28 | 2017-08-29 | 澳大利亚国家Ict有限公司 | The method for forming shell |
| CN109563612A (en) * | 2016-05-06 | 2019-04-02 | 阿尔托大学注册基金会 | Detonation Nano diamond and diamond-like-carbon are co-deposited to the method on substrate and the composite membrane comprising detonation Nano diamond and diamond-like-carbon |
| CN106637038A (en) * | 2016-09-21 | 2017-05-10 | 柳州市西朗能源科技有限公司 | Machine for manufacturing nano diamond thin coating film |
| CN107475686A (en) * | 2017-06-30 | 2017-12-15 | 湖北大学 | A kind of preparation method based on ald zirconium oxide corrosion resistance ceramic membrane |
| CN109536804A (en) * | 2018-12-05 | 2019-03-29 | 湖北第二师范学院 | Tantalum alloy, diamond-like-carbon coating tantalum alloy and diamond-like-carbon coating biomedicine implantation tantalum alloy bone pawl and preparation method thereof |
| CN112593204A (en) * | 2021-03-02 | 2021-04-02 | 中南大学湘雅医院 | Diamond film for scalpel and preparation method thereof |
| CN112593204B (en) * | 2021-03-02 | 2021-05-04 | 中南大学湘雅医院 | Diamond film for scalpel and preparation method thereof |
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