CN109355623A - A kind of wear-resisting acidproof nontoxic artificial graft's object film layer preparation method - Google Patents
A kind of wear-resisting acidproof nontoxic artificial graft's object film layer preparation method Download PDFInfo
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- 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
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- A61L27/00—Materials for grafts or prostheses or for coating grafts or prostheses
- A61L27/28—Materials for coating prostheses
- A61L27/30—Inorganic materials
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- A—HUMAN NECESSITIES
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- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/14—Metallic material, boron or silicon
- C23C14/16—Metallic material, boron or silicon on metallic substrates or on substrates of boron or silicon
- C23C14/165—Metallic material, boron or silicon on metallic substrates or on substrates of boron or silicon by cathodic sputtering
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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
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- 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
- C23C14/3435—Applying energy to the substrate during sputtering
- C23C14/345—Applying energy to the substrate during sputtering using substrate bias
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- 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
- C23C14/35—Sputtering by application of a magnetic field, e.g. magnetron sputtering
- C23C14/352—Sputtering by application of a magnetic field, e.g. magnetron sputtering using more than one target
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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
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- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
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Abstract
The invention discloses a kind of wear-resisting acidproof nontoxic artificial graft's object film layer preparation method, film layer includes by interior from outer adhesive layer, transition zone and the surface layer for being sequentially located at the friction of artificial graft's object and matching secondary surface；The preparation method comprises the following steps: 1) molding of adhesive layer；2) molding of transition zone；3) molding of surface layer.The present invention can be accurately controlled the metallurgical bonding of each coating, solve the stripping problem of coating, and each interlayer that applies sequentially forms gradient, reduce the generation of thermal stress, be greatly improved the service life of artificial tooth film layer.
Description
Technical field
The present invention relates to artificial graft's object film layer preparation fields, more particularly to a kind of wear-resisting acidproof nontoxic artificial graft's object film
Layer preparation method.
Background technique
Joint replacement is that current treatment joint disease is most direct, effective means, with the growth of national economy, manually
Demand of the joint in China is continuously increased.Joint prosthesis has been successfully applied to clinic, and friction is (convex) head-(recessed) with pair
Mortar structure is realized the motor patterns such as hip joint rotation, rotation, swing by the relative motion of ball and socket joint-cotyla respectively, is realized
The function in joint substitutes the diseased organ of patient.Joint prosthesis needs to be on active service (10 years or more or even 30 years for a long time in vivo
More than), during military service, the movement of (convex) head-(recessed) mortar structure relative friction is up to tens million of times, and abrasion caused by rubbing is not
(convex) head-(recessed) mortar structure size can be only set to change, most important harm is the various abrasive dusts generated in wear process
And metal ion will lead to inflammatory reaction and prosthese failure.For the joint prosthesis of clinical application, in addition to patients factors, hand
Outside art factor, wear-resistant, corrosion resistance of the prosthese friction with secondary (the recessed mortar of plush copper -) are the weights for influencing joint prosthesis service life
Want factor.Joint prosthesis metal is prepared nitride film (CrN, TiN/CrN, TiAlN etc.) with secondary surface, or uses ion
Method for implanting (oxonium ion, Nitrogen ion, carbon ion implantation etc.) forms ceramic surface modified layer in metal material surface, to improve gold
Belong to hardness and corrosion resistance with secondary friction surface, but the nitride layer and oxide skin(coating) coefficient of friction due to formation are big, close
The increase rate for saving wearability is limited, therefore not yet realizes clinical application so far.In comparison, DLC film utilizes
Non-equilibrium gas phase process synthesis, is to have both low friction system with carbon or with carbon, hydrogen amorphous carbon based film material as main component
Number, high-wear resistance, high rigidity, as a kind of excellent solid lubricant, DLC film have it is acidproof, non-toxic,
Good bio-compatibility is suitable for artificial joint, artificial new valve.Experiment in vitro is studies have shown that with traditional metal or pottery
Porcelain-macromolecule and metal-metal joint prosthesis are compared, and the modified joint prosthesis abrasion resistance properties in DLC film surface are substantially
Degree improves, the significant reduction of the release of metal ion, but it is in the clinical application in joint prosthesis field and unsuccessful.In 8.5 years,
The peeling of film can occur for the modified joint prosthesis of 45%DLC film surface.Studies have shown that interfacial corrosion and film-substrate cohesion are not
Foot is the main reason for leading to failure in the modified prosthese body in the surface DLC.The modified prosthese in DLC film surface long service in vivo
In the process, internal corrosive medium (such as Cl?、PO43-) by hole arrival film/metallic matrix interface of DLC film, corrode boundary
Surface layer causes DLC film to peel off, while the film fragments generated will lead to serious " three-body " abrasion, accelerates artificial close
Save the failure of prosthese.
Summary of the invention
Wear-resisting acidproof nontoxic artificial graft's object film that the purpose of the present invention is to provide a kind of membranous layer binding forces is big, the service life is long
Layer preparation method.To achieve the above object, the invention adopts the following technical scheme:
A kind of wear-resisting acidproof nontoxic artificial graft's object film layer preparation method, the film layer include sequentially being located at people from outer by interior
Adhesive layer, transition zone and the surface layer of secondary surface are matched in the friction of work graft, and adhesive layer is NiTi layer, and transition zone is that titanium mixes zr element
Diamond-like rock layers, surface layer are to mix the diamond-like rock layers of zr element；
The preparation method comprises the following steps:
1) molding of adhesive layer: using artificial graft's object of metal-metal classification as matrix, using magnetic control sputtering plating method by nickel
Target and titanium target material sputtering sedimentation rub in artificial graft's object matches secondary surface, then molten using laser to form bonding coating
The method covered melts above-mentioned bonding coating, to form adhesive layer；
2) molding of transition zone: titanium target material, zirconium target and carbon target material sputtering sedimentation are being bonded using magnetic control sputtering plating method
Then layer surface melts above-mentioned transition coating using the method for laser melting coating, with forming transition coating thus shape
At transition zone；
3) molding of surface layer: using magnetic control sputtering plating method by zirconium target and carbon target material sputtering sedimentation in transition layer surface, with
Investment precoat is formed, then above-mentioned investment precoat is melted using the method for laser melting coating, to form surface layer.
The parameter of adhesive layer magnetic control sputtering plating in step 1) are as follows: Substrate Negative Bias 70V, nickel target current 2A, substrate revolving speed 2rpm,
Nitrogen flow 5sccm, titanium electric current 2.5A, C2H2Flow 3.5sccm.
The parameter of transition zone magnetic control sputtering plating in step 2) are as follows: Substrate Negative Bias 70-100V, carbon target electric current 4-6A, substrate turn
Fast 2-8rpm, nitrogen flow 5-10sccm, zirconium target current 4-6A, titanium target electric current 2-5A, C2H2Flow 3-7sccm.
The parameter of surface layer magnetic control sputtering plating in step 3) are as follows: substrate bias 70-100V, zirconium target current 2-4A, substrate revolving speed 2-
8rpm, nitrogen flow 5-10sccm, carbon target electric current 5-10A, C2H2Flow 3-10sccm.
The technological parameter of adhesive layer, transition zone and the used laser cladding method of surface layer is equal are as follows: laser power 1000-
2500W, argon flow 1200-2400ml/min, scanning speed 2-8mm/s, laser head inclination angle 0-30 degree, defocusing amount 10-
30mm。
The thickness of the adhesive layer of final molding, transition zone and surface layer is respectively 100-200nm, 200-300nm, 400-
800nm。
The invention has the following advantages:
1, the DLC film coating that the present invention is formed has chemical inertness, the characteristic of bio-compatibility, high resistance against wear.
Prepared by wear-resisting acidproof nontoxic artificial graft's object film layer to above-mentioned laser cladding, the metallurgical bonding of coating can be accurately controlled,
Solve the stripping problem of coating.It applies interlayer and sequentially forms gradient, reduce the generation of thermal stress, be greatly improved artificial graft's object
Wearability.
2, doping metals/ceramic element DLC film internal stress that DLC film can be effectively reduced.It mixes
Hetero atom can form metal-carbon, metal/ceramic-carbon compound with the carbon atom inside film, and then reduce lacking inside film
It falls into, achievees the purpose that reduce stress in thin films.The present invention is changed with secondary surface using laser cladding coating in the friction of artificial graft's object
Property means prepare one layer doping can promote biofilm formed doping zr element DLC film, make it in military service process
In pass through the abrasion of DLC film, control DLC film internal metal ion release, the metal ion catalysis of release
It closes friction and forms one layer of fine and close biofilm with lubricating action with the biomolecule of secondary surface absorption, to friction with secondary abrasion
The defects of position and DLC film micropore, position repaired, and prevented internal corrosive medium (such as Cl-, PO43-) logical
The defect for crossing DLC film reaches DLC film/matrix interface, inhibits interfacial corrosion, improves DLC film
The stability being on active service in vivo reduces the artificial joint wear of metal-metal type, to increase substantially metal-metal type human
The quality of work graft and service life.
Specific embodiment
Embodiment 1, a kind of wear-resisting acidproof nontoxic artificial graft's object film layer preparation method, the film layer include by it is interior from outside according to
Sequence is located at adhesive layer, transition zone and the surface layer that secondary surface is matched in the friction of artificial graft's object, and adhesive layer is NiTi layer, and transition zone is mixed for titanium
The diamond-like rock layers of zr element, surface layer are to mix the diamond-like rock layers of zr element；
The preparation method comprises the following steps:
1) molding of adhesive layer: using artificial graft's object of metal-metal classification as matrix, using magnetic control sputtering plating method by nickel
Target and titanium target material sputtering sedimentation rub in artificial graft's object matches secondary surface, then molten using laser to form bonding coating
The method covered melts above-mentioned bonding coating, to form adhesive layer；
2) molding of transition zone: titanium target material, zirconium target and carbon target material sputtering sedimentation are being bonded using magnetic control sputtering plating method
Then layer surface melts above-mentioned transition coating using the method for laser melting coating, with forming transition coating thus shape
At transition zone；
3) molding of surface layer: using magnetic control sputtering plating method by zirconium target and carbon target material sputtering sedimentation in transition layer surface, with
Investment precoat is formed, then above-mentioned investment precoat is melted using the method for laser melting coating, to form surface layer.
The parameter of adhesive layer magnetic control sputtering plating in step 1) are as follows: Substrate Negative Bias 70V, nickel target current 2A, substrate revolving speed 2rpm,
Nitrogen flow 5sccm, titanium electric current 2.5A, C2H2Flow 3.5sccm.
The parameter of transition zone magnetic control sputtering plating in step 2) are as follows: Substrate Negative Bias 70V, carbon target electric current 4A, substrate revolving speed 2rpm,
Nitrogen flow 5sccm, zirconium target current 4A, titanium target electric current 2A, C2H2Flow 3sccm.
The parameter of surface layer magnetic control sputtering plating in step 3) are as follows: substrate bias 70V, zirconium target current 2A, substrate revolving speed 2rpm, nitrogen
Flow 5sccm, carbon target electric current 5A, C2H2Flow 3sccm.
The technological parameter of adhesive layer, transition zone and the used laser cladding method of surface layer is equal are as follows: laser power 1000W, argon
Throughput 1200ml/min, scanning speed 2mm/s, 0 degree of laser head inclination angle, defocusing amount 10mm.
The thickness of the adhesive layer of final molding, transition zone and surface layer is respectively 100nm, 200nm, 400nm.
Embodiment 2, a kind of wear-resisting acidproof nontoxic artificial graft's object film layer preparation method, the film layer include by it is interior from outside according to
Sequence is located at adhesive layer, transition zone and the surface layer that secondary surface is matched in the friction of artificial graft's object, and adhesive layer is NiTi layer, and transition zone is mixed for titanium
The diamond-like rock layers of zr element, surface layer are to mix the diamond-like rock layers of zr element；
The preparation method comprises the following steps:
1) molding of adhesive layer: using artificial graft's object of metal-metal classification as matrix, using magnetic control sputtering plating method by nickel
Target and titanium target material sputtering sedimentation rub in artificial graft's object matches secondary surface, then molten using laser to form bonding coating
The method covered melts above-mentioned bonding coating, to form adhesive layer；
2) molding of transition zone: titanium target material, zirconium target and carbon target material sputtering sedimentation are being bonded using magnetic control sputtering plating method
Then layer surface melts above-mentioned transition coating using the method for laser melting coating, with forming transition coating thus shape
At transition zone；
3) molding of surface layer: using magnetic control sputtering plating method by zirconium target and carbon target material sputtering sedimentation in transition layer surface, with
Investment precoat is formed, then above-mentioned investment precoat is melted using the method for laser melting coating, to form surface layer.
The parameter of adhesive layer magnetic control sputtering plating in step 1) are as follows: Substrate Negative Bias 70V, nickel target current 2A, substrate revolving speed 2rpm,
Nitrogen flow 5sccm, titanium electric current 2.5A, C2H2Flow 3.5sccm.
The parameter of transition zone magnetic control sputtering plating in step 2) are as follows: Substrate Negative Bias 100V, carbon target electric current 6A, substrate revolving speed
8rpm, nitrogen flow 10sccm, zirconium target current 6A, titanium target electric current 5A, C2H2Flow 7sccm.
The parameter of surface layer magnetic control sputtering plating in step 3) are as follows: substrate bias 100V, zirconium target current 4A, substrate revolving speed 8rpm, nitrogen
Throughput 10sccm, carbon target electric current 10A, C2H2Flow 10sccm.
The technological parameter of adhesive layer, transition zone and the used laser cladding method of surface layer is equal are as follows: laser power 2500W, argon
Throughput 2400ml/min, scanning speed 8mm/s, 30 degree of laser head inclination angle, defocusing amount 30mm.
The thickness of the adhesive layer of final molding, transition zone and surface layer is respectively 200nm, 300nm, 800nm.
Embodiment 3, a kind of wear-resisting acidproof nontoxic artificial graft's object film layer preparation method, the film layer include by it is interior from outside according to
Sequence is located at adhesive layer, transition zone and the surface layer that secondary surface is matched in the friction of artificial graft's object, and adhesive layer is NiTi layer, and transition zone is mixed for titanium
The diamond-like rock layers of zr element, surface layer are to mix the diamond-like rock layers of zr element；
The preparation method comprises the following steps:
1) molding of adhesive layer: using artificial graft's object of metal-metal classification as matrix, using magnetic control sputtering plating method by nickel
Target and titanium target material sputtering sedimentation rub in artificial graft's object matches secondary surface, then molten using laser to form bonding coating
The method covered melts above-mentioned bonding coating, to form adhesive layer；
2) molding of transition zone: titanium target material, zirconium target and carbon target material sputtering sedimentation are being bonded using magnetic control sputtering plating method
Then layer surface melts above-mentioned transition coating using the method for laser melting coating, with forming transition coating thus shape
At transition zone；
3) molding of surface layer: using magnetic control sputtering plating method by zirconium target and carbon target material sputtering sedimentation in transition layer surface, with
Investment precoat is formed, then above-mentioned investment precoat is melted using the method for laser melting coating, to form surface layer.
The parameter of adhesive layer magnetic control sputtering plating in step 1) are as follows: Substrate Negative Bias 70V, nickel target current 2A, substrate revolving speed 2rpm,
Nitrogen flow 5sccm, titanium electric current 2.5A, C2H2Flow 3.5sccm.
The parameter of transition zone magnetic control sputtering plating in step 2) are as follows: Substrate Negative Bias 80V, carbon target electric current 5A, substrate revolving speed 5rpm,
Nitrogen flow 8sccm, zirconium target current 5A, titanium target electric current 3A, C2H2Flow 5sccm.
The parameter of surface layer magnetic control sputtering plating in step 3) are as follows: substrate bias 80V, zirconium target current 3A, substrate revolving speed 5rpm, nitrogen
Flow 8sccm, carbon target electric current 8A, C2H2Flow 6sccm.
The technological parameter of adhesive layer, transition zone and the used laser cladding method of surface layer is equal are as follows: laser power 1700W, argon
Throughput 1800ml/min, scanning speed 5mm/s, 15 degree of laser head inclination angle, defocusing amount 20mm.
The thickness of the adhesive layer of final molding, transition zone and surface layer is respectively 150nm, 250nm, 600nm.
In order to verify the wear-resisting acidproof nontoxic artificial graft's object film layer of one kind made from preparation method of the present invention, to above-mentioned each reality
It applies the artificial graft film layer of the coating present invention in example to be tested for the property, and is comparison with existing magnetic control sputtering plating technical matters, into
Row hardness, wear-resistant, micro-structure, chemical stability, adhesion test result is as follows table:
Claims (6)
1. a kind of wear-resisting acidproof nontoxic artificial graft's object film layer preparation method, it is characterised in that: the film layer includes by interior from outer
It is sequentially located at adhesive layer, transition zone and surface layer that secondary surface is matched in the friction of artificial graft's object, adhesive layer is NiTi layer, and transition zone is titanium
The diamond-like rock layers of zr element are mixed, surface layer is to mix the diamond-like rock layers of zr element；
The preparation method comprises the following steps:
1) molding of adhesive layer: using artificial graft's object of metal-metal classification as matrix, using magnetic control sputtering plating method by nickel target
Match secondary surface in the friction of artificial graft's object with titanium target material sputtering sedimentation, to form bonding coating, then using laser melting coating
Method melts above-mentioned bonding coating, to form adhesive layer；
2) molding of transition zone: using magnetic control sputtering plating method by titanium target material, zirconium target and carbon target material sputtering sedimentation in adhesive layer table
Then above-mentioned transition coating is melted using the method for laser melting coating, with forming transition coating to be formed in face
Cross layer；
3) molding of surface layer: using magnetic control sputtering plating method by zirconium target and carbon target material sputtering sedimentation in transition layer surface, to be formed
Then investment precoat melts above-mentioned investment precoat using the method for laser melting coating, to form surface layer.
2. the wear-resisting acidproof nontoxic artificial graft's object film layer preparation method of one kind according to claim 1, it is characterised in that: step
It is rapid 1) in adhesive layer magnetic control sputtering plating parameter are as follows: Substrate Negative Bias 70V, nickel target current 2A, substrate revolving speed 2rpm, nitrogen flow
5sccm, titanium electric current 2.5A, C2H2Flow 3.5sccm.
3. the wear-resisting acidproof nontoxic artificial graft's object film layer preparation method of one kind according to claim 1, it is characterised in that: step
It is rapid 2) in transition zone magnetic control sputtering plating parameter are as follows: Substrate Negative Bias 70-100V, carbon target electric current 4-6A, substrate revolving speed 2-8rpm, nitrogen
Throughput 5-10sccm, zirconium target current 4-6A, titanium target electric current 2-5A, C2H2Flow 3-7sccm.
4. the wear-resisting acidproof nontoxic artificial graft's object film layer preparation method of one kind according to claim 1, it is characterised in that: step
It is rapid 3) in surface layer magnetic control sputtering plating parameter are as follows: substrate bias 70-100V, zirconium target current 2-4A, substrate revolving speed 2-8rpm, nitrogen stream
Measure 5-10sccm, carbon target electric current 5-10A, C2H2Flow 3-10sccm.
5. the wear-resisting acidproof nontoxic artificial graft's object film layer preparation method of one kind according to claim 1, it is characterised in that: viscous
The technological parameter for connecing layer, transition zone and the used laser cladding method of surface layer is equal are as follows: laser power 1000-2500W, argon flow
1200-2400ml/min, scanning speed 2-8mm/s, laser head inclination angle 0-30 degree, defocusing amount 10-30mm.
6. the wear-resisting acidproof nontoxic artificial graft's object film layer preparation method of one kind according to claim 1, it is characterised in that: most
The thickness of the adhesive layer of final shaping unit, transition zone and surface layer is respectively 100-200nm, 200-300nm, 400-800nm.
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| CN110424008A (en) * | 2019-08-19 | 2019-11-08 | 福建工程学院 | A kind of induction sintering method is used for the method and application of electron beam cladding prepares coating |
| CN115572974A (en) * | 2022-10-17 | 2023-01-06 | 中国船舶集团有限公司第七一一研究所 | Composite coating and preparation method thereof |
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