CN108930023A - A kind of method that Mg alloy surface magnetron sputtering prepares tantalum biological coating - Google Patents
A kind of method that Mg alloy surface magnetron sputtering prepares tantalum biological coating Download PDFInfo
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- CN108930023A CN108930023A CN201810804246.2A CN201810804246A CN108930023A CN 108930023 A CN108930023 A CN 108930023A CN 201810804246 A CN201810804246 A CN 201810804246A CN 108930023 A CN108930023 A CN 108930023A
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- magnetron sputtering
- tantalum
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
- C23C14/35—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
-
- 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
- C23C14/02—Pretreatment of the material to be coated
- C23C14/024—Deposition of sublayers, e.g. to promote adhesion of the coating
- C23C14/025—Metallic sublayers
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- 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
Abstract
The invention belongs to metal material surface coating technology fields, are related to a kind of method that Mg alloy surface magnetron sputtering prepares tantalum biological coating.The present invention first cleans sample with sand paper polishing, cold water wash, acetone oil removing, EtOH Sonicate;Then sample, Al target, Ta target are installed to magnetron sputtering chamber;Magnetron sputtering chamber is vacuumized, is filled with argon gas;Adjustment voltage is 265V-275V, and magnetron sputtering 5-8min prepares Al transition zone;Adjusting voltage again is 245V-255V, and magnetron sputtering 30-40min prepares Ta coating;Coating preparation is completed to close power supply, unloads sample, cleaning, drying.This method has many advantages, such as that easy to operate, required equipment is simple, process stabilizing is reliable, easy to realizations, efficient cryogenic, low damage, is suitable for production and applies.Gained coating binding force is good, even tissue, can improve the corrosion resistance of magnesium alloy and improve its biocompatibility, osteoconductive and bone-inducing activity.
Description
Technical field
The invention belongs to metal material surface coating technology fields, and in particular to a kind of Mg alloy surface magnetron sputtering preparation
The method of tantalum biological coating.
Background technique
Orthopedic implanting material mainly includes joint replacement, bone plate and Dental implantion material etc., ideal orthopedic implanting material
Should have excellent biocompatibility and bioactivity, while have suitable load force, anticorrosive and abrasion resistance properties.Tradition
Stainless steel bone implanting appliance often occur poor biocompatibility in clinical use, be also easy to produce the metal ion etc. being harmful to the human body
Problem;Although titanium alloy when as bone implant material, has preferable corrosion resistance and biocompatibility, its elasticity modulus is still
Higher than the hot bone in day, therefore easily cause " stress shielding " phenomenon.Meanwhile above two common bone implant material is after union
It needs second operation to take out, brings second operation to patient, increase the slight illness and medical treatment cost of patient.
Magnesium alloy is due to good biocompatibility and mechanical compatibility, good degradability (absorption of human body, nothing
Need second operation) and bioactivity and other metal_based materials and high molecular material not available for performance, become a new generation
The candidate material of medical embedded material.But Results of Animal shows: magnesium alloy is as bone implant material in animal body
It is interior to degrade disappearance there is only the short period (60-90 d), it is not on the one hand able to satisfy requirement of the bone growth to mechanical property;
On the other hand, quick corrosion degradation leads to the change of high liberation of hydrogen speed and pH value, receives the limit more than human body, may lead
Human body is caused to generate abnormal response.The above problem seriously constrains the application of magnesium alloy.
Therefore, Research on Surface Modification becomes the application of magnesium alloy that is, in Mg alloy surface prepares coating or surface protection film
Crucial and research emphasis.Existing result of study shows that tantalum (Ta) element has better bio-compatible compared with magnesium, titanium elements
Property, and tantalum element has good osteoconductive and bone-inducing activity, so, preparing tantalum biological coating in Mg alloy surface will be at
For the effective way for improving Properties of Magnesium Alloy.
Magnetron sputtering (Magnetron sputtering, abbreviation MS) is one kind of physical vapour deposition (PVD).It is thin gas
Table of the body in the plasma that abnormal glow discharge generates under the collective effect of electric and magnetic fields, to the target for being placed on cathode
Face is bombarded, and is sputtered the atom of target material surface, molecule, ion and each electron-like by the high-energy of plasma
Come, these ions sputtered out still kinetic energy with higher and along the surface of the direction homed on its target workpiece of setting to
Film is formed on matrix.Magnetron sputtering has the advantages that high speed, low temperature, low damage.
Currently, using in Mg alloy surface, magnetron sputtering technique prepares the technology of preparing of tantalum biological coating and its application still belongs to
Blank.Therefore study and realize the tantalum biology for having biocompatibility, osteoconductive and bone-inducing activity in Mg alloy surface preparation
The technology and methods of coating are of great significance to the application of magnesium alloy.
In conclusion main problem of the existing technology has: 1. magnesium-based material corrosion resistances are poor, in sclerotin
Mechanical property is lost because of corrosion before not healing;2. magnesium and other metals form the magnesium alloy materials corrosion resistance after alloy
Purer magnesium material is greatly improved, but as biological implantable material, bio-compatible sex expression is unsatisfactory;3.
Mg alloy surface still belongs to blank using the technology and application of magnetron sputtering technique preparation biological coating containing tantalum.
Summary of the invention
The purpose of the present invention is aiming at the problems existing in the prior art, provide the anti-corruption that magnesium and magnesium alloy both can be improved
Corrosion energy, but a kind of Mg alloy surface magnetron sputtering that can improve its biocompatibility, osteoconductive and bone-inducing activity prepares tantalum
The method of biological coating.This method also has that easy to operate, required equipment is simple, process stabilizing is reliable, easy to realize, low temperature is high
The advantages that effect, low damage, is suitable for production and application.The good, even tissue by the coating binding force of this method acquisition.
To achieve the above object, first technical solution that the present invention uses is: a kind of Mg alloy surface magnetron sputtering system
Standby tantalum biological coating, which is characterized in that the tantalum biological coating includes aluminium (Al) transition zone and tantalum (Ta) coating, is splashed by magnetic control
Penetrate method preparation.
Further, it using the magnetron sputtering method when Mg alloy surface prepares tantalum biological coating, needs first in magnesium alloy table
Face magnetron sputtering prepares one layer of aluminium (Al) transition zone, then magnetron sputtering prepares tantalum (Ta) coating, and it is raw can to improve entire tantalum in this way
The quality structure of object coating is conducive to the performance for improving entire tantalum biological coating.
Further, 0.1-0.2 microns of transition thickness of the aluminium (Al), the tantalum (Ta) apply thickness 1-2 microns.
Second technical solution that the present invention uses is: a kind of Mg alloy surface magnetron sputtering prepares the side of tantalum biological coating
Method, which is characterized in that need first to prepare one layer of aluminium (Al) transition zone in Mg alloy surface magnetron sputtering, then magnetron sputtering prepares tantalum
(Ta) coating.
Further, the method that the magnetron sputtering prepares tantalum biological coating, which is characterized in that specifically includes the following steps:
S1. sample polishing cleaning: cold water wash after sample is polished with 200#-2000# sand paper, acetone oil removing, EtOH Sonicate are clear
It washes, then drying is stand-by;
S2. it installs: sample, aluminium (Al) target, tantalum (Ta) target being installed to magnetron sputtering chamber, guarantee specimen surface and target
The distance between position is 8-10cm;
S3. it vacuumizes applying argon gas: magnetron sputtering chamber is evacuated to≤1 × 10-3After Pa, argon gas is filled with to 0.4Pa;
S4. magnetron sputtering prepares aluminium (Al) transition zone;
S5. magnetron sputtering prepares tantalum (Ta) coating;
S6. it takes out sample: the sample after the completion of magnetron sputtering is unloaded, EtOH Sonicate cleaning is dried, terminated.
Further, in step S2, purity >=99.99% of aluminium (Al) target, the purity of tantalum (Ta) target >=
99.99%。
Further, step S4. Magnetron Sputtered Al (Al) transition zone, specifically includes the following steps:
S4a. aluminium (Al) target is selected;
S4b. adjustment voltage is 265V-275V, magnetron sputtering 5-8min;
S4c. voltage is closed after the completion of the preparation of aluminium (Al) transition zone.
Preferably, the step S4b is specifically, adjustment voltage is 270V, magnetron sputtering 7min.
Further, the step S5. magnetron sputtering prepares tantalum (Ta) coating, specifically includes the following steps:
S5a. tantalum (Ta) target is selected;
S5b. adjustment voltage is 245V-255V, magnetron sputtering 30-40min;
S5c. voltage is closed after the completion of the preparation of tantalum (Ta) coating.
Preferably, the step S5b is specifically, adjustment voltage is 250V, magnetron sputtering 35min.
Further, acetone oil removing described in step S1 is that sample is put into acetone to impregnate, soaking time >=5min;It is described
EtOH Sonicate scavenging period >=5min.
Further, ethyl alcohol described in step S1 and S6 is dehydrated alcohol, wherein containing CH3CH2OH≥99.7%。
Further, the scavenging period of EtOH Sonicate described in step S6 >=2min.
Further, drying described in step S6 dries up to dry compartment low temperature hot-air seasoning, hair dryer drying or natural wind.
Beneficial effects of the present invention:
1, the present invention solves the technical problem that magnesium and corrosion resistance of magnesium alloy can be poor;
2, the biological coating containing tantalum prepared by the present invention has more excellent biocompatibility, good osteoconductive and lures bone
Activity;
3, equipment needed for prepares coating of the present invention is simple, and process stabilizing is reliable, efficient cryogenic, low damage, is easily achieved, and gained applies
Binding force is good for layer, even tissue.
Detailed description of the invention
Fig. 1 a is the microstructure figure by 1 tantalum biological coating obtained surface of the embodiment of the present invention;
Fig. 1 b is the microstructure figure by 1 tantalum biological coating obtained section of the embodiment of the present invention;
Fig. 2 a is the microstructure figure by 2 tantalum biological coating obtained surface of the embodiment of the present invention;
Fig. 2 b is the microstructure figure by 2 tantalum biological coating obtained section of the embodiment of the present invention;
Fig. 3 a is the microstructure figure by 3 tantalum biological coating obtained surface of the embodiment of the present invention;
Fig. 3 b is the microstructure figure by 3 tantalum biological coating obtained section of the embodiment of the present invention;
Fig. 4 is the structural schematic diagram by 1 tantalum biological coating obtained section of the embodiment of the present invention;
Fig. 5 is the process flow chart that a kind of Mg alloy surface magnetron sputtering of the present invention prepares tantalum biological coating.
Specific embodiment
Technical solution of the present invention is described in detail with reference to the accompanying drawing, but the contents of the present invention are not limited to
This.
Purity >=99.99% of aluminium (Al) target used in following embodiment, the purity of tantalum (Ta) target used >=
99.99%。
Embodiment 1
Mg alloy surface magnetron sputtering prepares tantalum biological coating.
As shown in the process flow chart of Fig. 5, the present embodiment is followed the steps below:
1, sample polishing cleaning: sample cold water wash after the polishing of 200#-2000# sand paper, acetone oil removing, EtOH Sonicate cleaning,
Then drying is stand-by;
2, it installs: sample, aluminium (Al) target, tantalum (Ta) target is installed to magnetron sputtering chamber, guarantee specimen surface away from target
Position is 8cm;
3, it vacuumizes applying argon gas: magnetron sputtering chamber is evacuated to≤1 × 10-3After Pa, argon gas is filled with to 0.4Pa;
4, magnetron sputtering prepares aluminium (Al) transition zone:
4a. selects aluminium (Al) target;
It is 265V, magnetron sputtering 5min that 4b., which adjusts voltage,;
Voltage is closed after the completion of the preparation of 4c. aluminium (Al) transition zone;
5, magnetron sputtering prepares tantalum (Ta) coating:
5a. selects tantalum (Ta) target;
It is 245V, magnetron sputtering 30min that 5b., which adjusts voltage,;
Voltage is closed after the completion of the preparation of 5c. tantalum (Ta) coating;
6, it takes out sample: the sample after the completion of magnetron sputtering is unloaded, EtOH Sonicate cleans 2.5min, and hair dryer drying terminates.
Fig. 1 a and Fig. 1 b are shown in by the microstructure figure on 1 tantalum biological coating obtained surface of embodiment and section respectively.
As shown in figure 4, the tantalum biological coating on magnesium alloy substrate obtained by embodiment 1, mainly by thickness about 0.1-0.2
Aluminium (Al) transition zone and 1-2 microns of tantalum (Ta) the coating composition of micron, realize in Mg alloy surface using magnetron sputtering system
The technology of standby tantalum biological coating, and gained coating quality is good.
Embodiment 2
Mg alloy surface magnetron sputtering prepares tantalum biological coating.
As shown in the process flow chart of Fig. 5, the present embodiment is followed the steps below:
1, sample polishing cleaning: sample cold water wash after the polishing of 200#-2000# sand paper, acetone oil removing, EtOH Sonicate cleaning,
Then drying is stand-by;
2, it installs: sample and aluminium (Al) target, tantalum (Ta) target is installed to magnetron sputtering chamber, guarantee specimen surface away from target
Position is 9cm;
3, it vacuumizes applying argon gas: magnetron sputtering chamber is evacuated to≤1 × 10-3After Pa, argon gas is filled with to 0.4Pa;
4, magnetron sputtering prepares aluminium (Al) transition zone:
4a. selects aluminium (Al) target;
It is 270V, magnetron sputtering 7min that 4b., which adjusts voltage,;
Voltage is closed after the completion of the preparation of 4c. aluminium (Al) transition zone;
5, magnetron sputtering prepares tantalum (Ta) coating:
5a. selects tantalum (Ta) target;
It is 250V, magnetron sputtering 35min that 5b., which adjusts voltage,;
Voltage is closed after the completion of the preparation of 5c. tantalum (Ta) coating;
6, it takes out sample: the sample after magnetron sputtering is unloaded, EtOH Sonicate cleans 2.5min, and hair dryer drying terminates.
Fig. 2 a and Fig. 2 b are shown in by the microstructure figure on 2 tantalum biological coating obtained surface of embodiment and section respectively.
Embodiment 3
Mg alloy surface magnetron sputtering prepares tantalum biological coating.
As shown in the process flow chart of Fig. 5, the present embodiment is followed the steps below:
1, sample polishing cleaning: sample cold water wash after the polishing of 200#-2000# sand paper, acetone oil removing, EtOH Sonicate cleaning,
Then drying is stand-by;
2, it installs: sample and aluminium (Al) target, tantalum (Ta) target is installed to magnetron sputtering chamber, guarantee specimen surface away from target
Position is 10cm;
3, it vacuumizes applying argon gas: magnetron sputtering chamber is evacuated to≤1 × 10-3After Pa, argon gas is filled with to 0.4Pa;
4, magnetron sputtering prepares aluminium (Al) transition zone:
4a. selects aluminium (Al) target;
It is 275V, magnetron sputtering 8min that 4b., which adjusts voltage,;
Voltage is closed after the completion of the preparation of 4c. aluminium (Al) transition zone;
5, magnetron sputtering prepares tantalum (Ta) coating:
5a. selects tantalum (Ta) target;
It is 255V, magnetron sputtering 40min that 5b., which adjusts voltage,;
5c. closing voltage after the completion of the preparation of tantalum (Ta) coating;
6, it takes out sample: the sample after magnetron sputtering is unloaded, EtOH Sonicate cleans 3min, and hair dryer drying terminates.
Fig. 3 a and Fig. 3 b are shown in by the microstructure figure on 3 tantalum biological coating obtained surface of embodiment and section respectively.
The above is only presently preferred embodiments of the present invention, the interest field being not intended to limit the invention.It is any with this
The technical solution or anyone skilled in the art that the interest field that claim is covered is implemented utilize
The method content of the disclosure above makes the scheme of many possible changes and modifications, all belongs to the scope of protection of the present invention.
Claims (10)
1. a kind of tantalum biological coating of Mg alloy surface magnetron sputtering preparation, which is characterized in that the tantalum coating includes aluminium transition
Layer and tantalum coating, are prepared by magnetron sputtering method.
2. a kind of tantalum biological coating of Mg alloy surface magnetron sputtering preparation as described in claim 1, which is characterized in that use institute
Magnetron sputtering method is stated when Mg alloy surface prepares tantalum coating, needs first to prepare one layer of aluminium transition in Mg alloy surface magnetron sputtering
Layer, then magnetron sputtering prepare tantalum coating.
3. a kind of tantalum biological coating of Mg alloy surface magnetron sputtering preparation as described in claim 1, which is characterized in that the aluminium
0.1-0.2 microns of transition thickness, the tantalum applies thickness 1-2 microns.
4. a kind of method that Mg alloy surface magnetron sputtering prepares tantalum biological coating, which is characterized in that first in Mg alloy surface magnetic
Control sputtering one layer of aluminium transition zone of preparation, then magnetron sputtering prepare tantalum coating.
5. a kind of method that Mg alloy surface magnetron sputtering prepares tantalum biological coating as claimed in claim 4, which is characterized in that tool
Body the following steps are included:
S1. sample polishing cleaning: cold water wash after sample is polished with 200#-2000# sand paper, acetone oil removing, EtOH Sonicate are clear
It washes, then drying is stand-by;
S2. it installs: sample, aluminium target, tantalum target being installed to magnetron sputtering chamber, guaranteed between specimen surface and target location
Distance be 8-10cm;
S3. it vacuumizes applying argon gas: magnetron sputtering chamber is evacuated to≤1 × 10-3After Pa, argon gas is filled with to 0.4Pa;
S4. magnetron sputtering prepares aluminium transition zone;
S5. magnetron sputtering prepares tantalum coating;
S6. it takes out sample: the sample after the completion of magnetron sputtering is unloaded, EtOH Sonicate cleaning is dried, terminated.
6. a kind of method that Mg alloy surface magnetron sputtering prepares tantalum biological coating as claimed in claim 5, which is characterized in that step
In rapid S2, purity >=99.99% of the aluminium target, purity >=99.99% of the tantalum target.
7. a kind of method that Mg alloy surface magnetron sputtering prepares tantalum biological coating as claimed in claim 5, which is characterized in that
The step S4 specifically includes the following steps:
S4a. aluminium target is selected;
S4b. adjustment voltage is 265V-275V, magnetron sputtering 5-8min;
S4c. voltage is closed after the completion of the preparation of aluminium transition zone.
8. a kind of method that Mg alloy surface magnetron sputtering prepares tantalum biological coating as claimed in claim 7, which is characterized in that institute
Step S4b is stated specifically, adjustment voltage is 270V, magnetron sputtering 7min.
9. a kind of method that Mg alloy surface magnetron sputtering prepares tantalum biological coating as claimed in claim 5, which is characterized in that
The step S5 specifically includes the following steps:
S5a. tantalum target is selected;
S5b. adjustment voltage is 245 V -255V, magnetron sputtering 30-40min;
S5c. voltage is closed after the completion of the preparation of tantalum coating.
10. a kind of method that Mg alloy surface magnetron sputtering prepares tantalum biological coating as claimed in claim 9, which is characterized in that
The step S5b is specifically, adjustment voltage is 250V, magnetron sputtering 35min.
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Cited By (2)
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CN111411336A (en) * | 2020-03-27 | 2020-07-14 | 温州医科大学附属口腔医院 | Artificial implant |
CN112663008A (en) * | 2020-11-30 | 2021-04-16 | 江苏理工学院 | Method for preparing magnesium-aluminum composite board by utilizing radio frequency magnetic control |
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Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
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CN111411336A (en) * | 2020-03-27 | 2020-07-14 | 温州医科大学附属口腔医院 | Artificial implant |
CN112663008A (en) * | 2020-11-30 | 2021-04-16 | 江苏理工学院 | Method for preparing magnesium-aluminum composite board by utilizing radio frequency magnetic control |
CN112663008B (en) * | 2020-11-30 | 2022-12-23 | 江苏理工学院 | Method for preparing magnesium-aluminum composite board by utilizing radio frequency magnetic control |
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