CN106048548A - Preparation method of biological active nanocrystal beta-Ta coating - Google Patents
Preparation method of biological active nanocrystal beta-Ta coating Download PDFInfo
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- CN106048548A CN106048548A CN201610432221.5A CN201610432221A CN106048548A CN 106048548 A CN106048548 A CN 106048548A CN 201610432221 A CN201610432221 A CN 201610432221A CN 106048548 A CN106048548 A CN 106048548A
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- coating
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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
- C23C14/46—Sputtering by ion beam produced by an external ion source
-
- 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
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- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Prostheses (AREA)
- Materials For Medical Uses (AREA)
Abstract
The invention discloses a preparation method of a biological active nanocrystal beta-Ta coating. The biological active nanocrystal beta-Ta coating is prepared through the double-cathode plasma sputtering deposition method. According to the specific technological parameters, the target voltage is 700-1000 V, the workpiece voltage is 250-350 V, the distance between a target and a workpiece is 10-20 mm, the working air pressure is 25-40 Pa, the deposition temperature is 600-900 DEG C, and the deposition time is 1.0-2.0 h; commercial pure Ta with the purity higher than 99.9% can be used as the sputtering target; and medical titanium alloy implant materials can be used as materials of the workpiece. The nanocrystal beta-Ta coating prepared through the method has high hardness, high tenacity and excellent corrosion resistance and apatite inducing capacity, and the abrasion resistance, corrosion resistance and biological activity of medical titanium alloy can be obviously improved.
Description
Technical field
The present invention relates to surface process and biomedical materials field, particularly relate to a kind of biologically active nanometer crystalline substance β-Ta
The preparation method of coating.
Background technology
In biomedical metallic material, titanium-based metal is because of mechanical property, decay resistance and the good life of its excellence
The thing compatibility, becomes current orthopaedics and implants the preferred material of product.But, titanium-based metal does not possess bone guided and induction osseous tissue
Regeneration function, belongs to bio-inert material, it is impossible to bone formation chemical bonding.Additionally, for the implant of joint type, polishing machine
Deficiency make titanium alloy be easy under mechanical wear effect produce abrasive dust, a large amount of abrasive dusts build up induction body cell produce one
Series bad biological respinse, cause osteolysis and aseptic loosen, ultimately result in implant lost efficacy.Meanwhile, long-term with human body
In interaction process, in titanium alloy, the release of the harmful element such as Ni, Al, V can produce toxic action to body, cause dementia,
Neurological disorders, the generation of osteoporosis diseases.How to improve the biological activity of titanium-based metal implant, wear-resistant and corrosion-resistant
Performance becomes one of medical treatment and material supplier author's focus of paying close attention to for a long time and studying.With advanced process for modifying surface as means,
Preparing bioactivity coatings wear-resistant, corrosion resistant on medical titanium alloy surface is one of effective ways solving the problems referred to above.
Summary of the invention
It is an object of the invention to, with twin cathode plasma sputter deposition technology as means, utilize the unlimited solid solution of Ti, Ta
Feature, prepares high rigidity, high tenacity and is the nanocrystalline β-Ta coating of metallurgical binding with matrix on medical titanium alloy surface, this painting
Layer has special surface nanotopology, can significantly improve titanium alloy corrosion resistance in physiological solution and apatite induction energy
Power.
The present invention is by the following technical solutions:
The preparation method of a kind of biologically active nanometer crystalline substance β-Ta coating, uses twin cathode plasma sputter deposition technology, at workpiece
Surface forms the flawless nanocrystalline β-Ta coating of dense uniform, wherein
A. twin cathode plasma sputter deposition technological parameter: target voltage is 700 ~ 1000 V, workpiece voltage is 250 ~ 350 V,
Target and workpiece spacing are 10 ~ 20 mm, and Ar air pressure is 25 ~ 40 Pa, and depositing temperature is 600 ~ 900 DEG C, sedimentation time is 1.0 ~
2.0 h；
B. the target kind sputtered: commercial pure Ta；
C. the kind of workpiece material: medical titanium alloy.
The present invention uses twin cathode plasma sputter deposition technology, has special receiving in the preparation of Ti-6Al-4V alloy surface
β-Ta the coating of rice pattern.Tests prove that, this coating is made up of the β-Ta nanocrystal of 15-30 nm completely, dense structure
Uniformly zero defect, is well combined with matrix.Electro-chemical test and physiological solution immersion test show that this coating significantly improves Ti-
The corrosion resistance of 6Al-4V matrix and apatite inducibility, demonstrate huge orthopedic implant application potential.
As preferably, target voltage is 800 V.
As preferably, workpiece voltage is 250 V.
As preferably, target and workpiece spacing are 10 mm.
As preferably, Ar air pressure is 35 Pa.
As preferably, depositing temperature is 800 DEG C.
As preferably, sedimentation time is 2.0 h.
Beneficial effect:
1. the nanorize of the present invention improves toughness and the hardness of metal Ta coating.There are two kinds of crystal structures in metal Ta, respectively
α-Ta and the β-Ta of tetragonal for body-centered cubic structure.Conventional metal Ta coating application focuses primarily upon α-Ta, and this is main
If because β-Ta coating presents high black brittleness, it is easy to cracking failure, even large stretch of peeling the most under mechanical action.
The present invention uses metal Ta coating prepared by twin cathode plasma sputter deposition technology completely by the single-phase nanocrystalline (15-of β-Ta
30 nm) composition, make this coating not only have high microhardness (~ 17.1 GPa), and present high toughness.Utilize impression
Method evaluate coating toughness show: do not observe around microhardness impression when loading of pressing in is 9.8 N crackle germinating and
Development.Due in the range of nanoscale the deformation mechanism of material by traditional dislocation formed with motion take as the leading factor be changed into by
Grain Boundary Sliding and diffusion creep are taken as the leading factor, and Grain Boundary Sliding can effectively discharge the stress of crack tip and concentrate, and is passivated crackle, makes to split
Stricture of vagina extension difficulty, thus increase the toughness of nanocrystalline coating.
2. the nanocrystalline β-Ta coating of the present invention has the highest electrochemical corrosion drag in physiological solution.Hanks is molten
Potentiodynamic polarization test in liquid shows, this coating relatively Ti-6Al-4V matrix, the most commercial pure Ta, has low corrosion certainly
Electric current density and passive current density, high polarization impedance, show the electrochemical corrosion drag of excellence.
The apatite inducibility that the most nanocrystalline β-Ta coating is high in simulated body fluid.Immersion in Hanks solution
Test shows, this coating has obvious apatite inducibility compared with the pure Ta of Ti-6Al-4V matrix and commercialization, shows high life
Thing activity.The special Nanoscale Surface shape characteristic of this coating makes coating have great specific surface area and favourable electric charge divides
Ca during cloth, beneficially biomineralization2+, PO4 3-A large amount of absorption, thus show the apatite inducibility of excellence.
Accompanying drawing explanation
Fig. 1 is the light field TEM photo of nanocrystalline β-Ta coating.
Fig. 2 is nanocrystalline β-Ta coating, Ti-6Al-4V matrix and the pure Ta of commercialization galvanic electricity at 37 DEG C in Hanks solution
Bit polarization curve ratio is relatively.
Fig. 3 is that nanocrystalline β-Ta coating, Ti-6Al-4V matrix and the pure Ta of commercialization soak one in Hanks solution at 37 DEG C
Surface SEM photograph after week.
Fig. 4 is the surface A FM photo of nanocrystalline β-Ta coating.
Specific embodiments
Below in conjunction with the accompanying drawings the present invention is described in further detail.
Embodiment 1
The preparation method of a kind of biologically active nanometer crystalline substance β-Ta coating, utilizes twin cathode plasma sputter deposition method, at Ti-6Al-
4V surface of the work forms the flawless nanocrystalline β-Ta coating of dense uniform, wherein
A. twin cathode plasma sputtering technological parameter:
| Target voltage | 800 V |
| Workpiece voltage | 250 V |
| Target and workpiece spacing | 10 mm |
| Ar air pressure | 35 Pa |
| Depositing temperature | 800 ℃ |
| Sedimentation time | 2.0 h |
B. the target kind sputtered: purity is the pure Ta of the commercialization more than 99.9%；
C. the kind of workpiece material: medical titanium alloy Ti-6Al-4V.
Fig. 1 is the light field TEM photo of nanocrystalline β-Ta coating.It can be seen that this coating is by size 15-30 nm
β-Ta nanocrystal composition, average grain size is about 23 nm.The hardness of this coating is 17.1 GPa, and elastic modelling quantity is
245.4 GPa, reach 38 N with the bond strength of matrix.The toughness utilizing indentation method to evaluate coating shows: loading of pressing in is
Germinating and the development of crackle is not observed around microhardness impression, it was demonstrated that this nanocrystalline β-Ta coating has height during 9.8 N
Toughness.
Potentiodynamic polarization test in Hanks solution shown in Fig. 2 shows, nanocrystalline β-Ta coating relatively Ti-6Al-4V matrix
Ta pure with commercialization, has lower corrosion current density and passive current density, high polarization impedance, shows the electricity of excellence
Chemical attack drag.
Soak Test in Hanks solution shown in Fig. 3 shows, nanocrystalline β-Ta coating relatively Ti-6Al-4V matrix and commercialization
Pure Ta has obvious apatite inducibility, shows high biological activity.It can be seen that β-Ta coating surface is complete
Entirely covered by one layer of thicker apatite layer, demonstrate powerful apatite inducibility.And for Ti-6Al-4V matrix and
Commercial pure Ta, surface only has a small amount of apatite and is formed, demonstrates the most weak apatite inducibility.
Fig. 4 is the surface A FM photo of nanocrystalline β-Ta coating, it can be seen that this coating surface shows as numerous
The conoid protuberance of highly 2-4 nm, has the Nanoscale Surface roughness of 3.8-4.3 nm.So shape characteristic makes coating
Have Ca during great specific surface area and favourable CHARGE DISTRIBUTION, beneficially biomineralization2+, PO4 3-A large amount of absorption, because of
And show the apatite inducibility of excellence.
The present invention, with twin cathode plasma sputter deposition technology as means, utilizes the feature of the unlimited solid solution of Ti, Ta, at Ti-
6Al-4V alloy surface is prepared high rigidity, high tenacity and is the nanocrystalline β-Ta coating of metallurgical binding with matrix.This coating has
Special surface nanotopology, can significantly improve titanium alloy corrosion resistance in physiological solution and apatite inducibility, aobvious
Huge orthopedic implant application potential is shown.
Embodiment 2
The preparation method of a kind of biologically active nanometer crystalline substance β-Ta coating, utilizes twin cathode plasma sputter deposition method, at Ti-6Al-
4V surface of the work forms the flawless nanocrystalline β-Ta coating of dense uniform, wherein a. twin cathode plasma sputtering technological parameter:
Target voltage 900 V, workpiece voltage 250 V, target and workpiece spacing 10 mm, Ar air pressure 40 Pa, depositing temperature 900 DEG C is heavy
Long-pending time 1.5 h；B. the target kind sputtered: purity is > 99.9% the pure Ta of commercialization；C. the kind of workpiece material: medical titanium is closed
Gold Ti-6Al-4V.The electrochemical corrosion drag of gained coating is suitable with embodiment 1, but apatite inducibility is less than embodiment
1, after soaking one week in the Hanks solution of 37 DEG C, top layer is covered by apatite the most completely.
Embodiment 3
The preparation method of a kind of biologically active nanometer crystalline substance β-Ta coating, utilizes twin cathode plasma sputter deposition method, at Ti-6Al-
4V surface of the work forms the flawless nanocrystalline β-Ta coating of dense uniform, wherein a. twin cathode plasma sputtering technological parameter:
Target voltage 750 V, workpiece voltage 250 V, target and workpiece spacing 15 mm, Ar air pressure 40 Pa, depositing temperature 700 DEG C is heavy
Long-pending time 2.0 h；B. the target kind sputtered: purity is > 99.9% the pure Ta of commercialization；C. the kind of workpiece material: medical titanium is closed
Gold Ti-6Al-4V.The electrochemical corrosion drag of gained coating is suitable with the pure Ta of business, less than embodiment 1；Apatite inducibility
Suitable with embodiment 1.
Embodiment 4
The preparation method of a kind of biologically active nanometer crystalline substance β-Ta coating, utilizes twin cathode plasma sputter deposition method, at Ti-6Al-
4V surface of the work forms the flawless nanocrystalline β-Ta coating of dense uniform, wherein a. twin cathode plasma sputtering technological parameter:
Target voltage 700 V, workpiece voltage 350 V, target and workpiece spacing 12 mm, Ar air pressure 25 Pa, depositing temperature 700 DEG C is heavy
Long-pending time 1.5 h；B. the target kind sputtered: purity is > 99.9% the pure Ta of commercialization；C. the kind of workpiece material: medical titanium is closed
Gold Ti-6Al-4V.The electrochemical corrosion drag of gained coating is suitable with the pure Ta of business, less than embodiment 1；Apatite inducibility
Less than embodiment 1, after soaking one week in the Hanks solution of 37 DEG C, top layer is covered by apatite the most completely.
Embodiment 5
The preparation method of a kind of biologically active nanometer crystalline substance β-Ta coating, utilizes twin cathode plasma sputter deposition method, at Ti-6Al-
4V surface of the work forms the flawless nanocrystalline β-Ta coating of dense uniform, wherein a. twin cathode plasma sputtering technological parameter:
Target voltage 800 V, workpiece voltage 250 V, target and workpiece spacing 20 mm, Ar air pressure 30Pa, depositing temperature 600 DEG C is heavy
Long-pending time 1.0 h；B. the target kind sputtered: purity is > 99.9% the pure Ta of commercialization；C. the kind of workpiece material: medical titanium is closed
Gold Ti-6Al-4V.The electrochemical corrosion drag of gained coating is suitable with Ti-6Al-4V, less than the pure Ta of business and embodiment 1；Phosphorus
Lime stone inducibility is suitable with embodiment 1.
Claims (7)
1. the preparation method of a biologically active nanometer crystalline substance β-Ta coating, it is characterised in that: use twin cathode plasma sputtering to sink
Long-pending technology, forms the flawless nanocrystalline β-Ta coating of dense uniform at surface of the work, wherein
A. twin cathode plasma sputter deposition technological parameter: target voltage is 700 ~ 1000 V, workpiece voltage is 250 ~ 350 V,
Target and workpiece spacing are 10 ~ 20 mm, and Ar air pressure is 25 ~ 40 Pa, and depositing temperature is 600 ~ 900 DEG C, sedimentation time is 1.0 ~
2.0 h；
B. the target kind sputtered: commercial pure Ta；
C. the kind of workpiece material: medical titanium alloy.
The preparation method of biologically active nanometer crystalline substance β-Ta coating the most according to claim 1, it is characterised in that: target voltage
It is 800 V.
The preparation method of biologically active nanometer crystalline substance β-Ta coating the most according to claim 1, it is characterised in that: workpiece voltage
It is 250 V.
The preparation method of biologically active nanometer crystalline substance β-Ta coating the most according to claim 1, it is characterised in that: target and work
Part spacing is 10 mm.
The preparation method of biologically active nanometer crystalline substance β-Ta coating the most according to claim 1, it is characterised in that: Ar air pressure is
35 Pa。
The preparation method of biologically active nanometer crystalline substance β-Ta coating the most according to claim 1, it is characterised in that: depositing temperature
It it is 800 DEG C.
7., according to the preparation method of the biologically active nanometer crystalline substance β-Ta coating described in any one of claim 1 to 6, its feature exists
In: sedimentation time is 2.0 h.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113235061A (en) * | 2021-05-18 | 2021-08-10 | 南昌大学第一附属医院 | Preparation process of tantalum metal coating of medical screw |
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| CN1316309A (en) * | 2001-03-16 | 2001-10-10 | 太原理工大学 | Process for preparing nm material by dual-glow discharge of hollow cathodes |
| CN1346902A (en) * | 2001-09-28 | 2002-05-01 | 太原理工大学 | Plasma co-diffusion process of metal and non-metal elements |
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| CN113235061A (en) * | 2021-05-18 | 2021-08-10 | 南昌大学第一附属医院 | Preparation process of tantalum metal coating of medical screw |
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