CN107773782A - It is a kind of to put forward high purity titanium and the method for titanium alloy surface cytocompatibility and biocidal property - Google Patents
It is a kind of to put forward high purity titanium and the method for titanium alloy surface cytocompatibility and biocidal property Download PDFInfo
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- CN107773782A CN107773782A CN201610712748.3A CN201610712748A CN107773782A CN 107773782 A CN107773782 A CN 107773782A CN 201610712748 A CN201610712748 A CN 201610712748A CN 107773782 A CN107773782 A CN 107773782A
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- titanium
- titanium alloy
- cytocompatibility
- alloy surface
- high purity
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L27/00—Materials for grafts or prostheses or for coating grafts or prostheses
- A61L27/02—Inorganic materials
- A61L27/04—Metals or alloys
- A61L27/06—Titanium or titanium alloys
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L27/00—Materials for grafts or prostheses or for coating grafts or prostheses
- A61L27/14—Macromolecular materials
- A61L27/16—Macromolecular materials obtained by reactions only involving carbon-to-carbon unsaturated bonds
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L27/00—Materials for grafts or prostheses or for coating grafts or prostheses
- A61L27/50—Materials characterised by their function or physical properties, e.g. injectable or lubricating compositions, shape-memory materials, surface modified materials
-
- 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
- C23C14/48—Ion implantation
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L2400/00—Materials characterised by their function or physical properties
- A61L2400/18—Modification of implant surfaces in order to improve biocompatibility, cell growth, fixation of biomolecules, e.g. plasma treatment
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L2430/00—Materials or treatment for tissue regeneration
- A61L2430/12—Materials or treatment for tissue regeneration for dental implants or prostheses
Abstract
The present invention puies forward high purity titanium and the method for titanium alloy surface cytocompatibility and biocidal property using a kind of, comprises the steps：Handling member is treated using plasma immersion injection technology to be surface-treated, wherein the plasma is argon plasma (as working media and build-up of luminance gas), described pending part is metal or the product for being coated with the metal.Present invention also offers the surface treated metal obtained with methods described and the product for being coated with the surface treated metal, and they are implanted into as human body and the application of intervention material.The present invention uses argon gas as build-up of luminance gas and working media, source of the polytetrafluoroethylene (PTFE) as fluorine element, the cytocompatibility and bacteriostasis of titanium or titanium alloy surface can be improved after treatment, so that after being implanted into human body as bio-medical material using titanium or titanium alloy, its Integrated implant ability and bacteriostasis are improved, and can be applied to the fields such as metallic implant surface processing.
Description
Technical field
The present invention relates to implantation and intervention class medical instruments field, more particularly to one kind to carry high purity titanium and titanium alloy surface bone
The method of cell compatibility and biocidal property, the surface treatment of the biomedical metal material for the tooth implant that is particularly suitable for use in.
Background technology
Titanium or titanium alloy has excellent biocompatibility and mechanical property, is widely used in medical science implantation field.Titanium
Belong to bio-inert material with titanium alloy, bioactivity is poor.Such as dentistry implant be implanted into human body after, as place
Main heteroplasmon is present, and easily deforms, loosens, causes implant to fail.It is living that its biology is assigned using process for modifying surface
Property after, can make new bone be deposited directly to titanium alloy surface formed synostosis, avoid the formation of fibrous connective tissue.But it is being implanted into
And bacterial plaque easily occur after repairing and be piled up in around titanium implant, cause planting body success rate to decline.Therefore titanium alloy table is being ensured
While face has bioactivity, the bacteriostasis property for improving titanium bone grafting material is also that the one kind for improving plantation success rate has efficacious prescriptions
Method.
Fluorine is as one of trace element necessary to body vital movement, in the bone growth and development and maintenance bone of whole body
Play the part of important role in physiological structure function.Fluoride has strong compatibility for calcified tissue, and can be direct
By stimulating bone cell proliferation and strengthening alkaline phosphatase activities, strengthen osteogenic action, while fluorine element Implanted Titanium surface is modified
The surface of material is made up of titanium, oxygen, fluorine, carbon, for pellet shape material being evenly distributed, being dispersed in.Fluorine element can promote bone
The formation of cell adhesion spot, the adhesion for suppressing bacterium so that titanium and titanium alloy surface have good cytocompatibility
And bacteriostasis property.
Fluorine ion can be injected into titanium or titanium alloy top layer by plasma immersion ion injection technique at present, use tetrafluoride
Carbon gas injects source as fluorine ion, and existing difficulty is to be not easy build-up of luminance, and the gas breaks atmospheric ozone layer by carbon tetrafluoride,
It is unfavorable to environmental protection.
At present in titanium and the scheme of titanium alloy surface cytocompatibility and bacteriostasis property is improved, more by fluorine from
The injection of son is realized.Including raising (Liu Huiying, Liu Yang the fluorine ions of titanium and titanium alloy surface cytocompatibility
Cytocompatibility and anti-microbial property [J] China the tooth-planting magazine of Implanted Titanium surface modifying material, 2009,14 (2)：56-
59.) and titanium and titanium alloy surface bacteriostasis raising (Nurhaerani.Plasma-based fluorine ion
implantation into dental materials for inhibition of bacterial adhesion[J]
.Dent Master J, 2006,25 (4):95-100).
The content of the invention
High purity titanium and the side of titanium alloy surface cytocompatibility and biocidal property are carried it is an object of the invention to provide a kind of
Method, the source of fluorine ion are located in the polytetrafluoroethylene solids block in PIC method in plasma immersion ion injection cavity, utilized
Gas ions plasma immersion ion implantation method (PIII) is treated handling member and is surface-treated, wherein described plasma is argon ion
Body and fluorine element, described pending part are metal derby.
Wherein, the process conditions of described PIC method in plasma immersion ion injection and method can be according to this area conventional methods
Selected, the present invention is carried out using following step：In cavity, in argon ion body and the fluorine inspired by argon plasma
In the mixed atmosphere of the composition of element, back bias voltage pulse is loaded on the pending part, by described in plasma injection
The surface of pending part.It is preferred that the air pressure of the cavity is maintained into 0.1Pa~1Pa.To maintain the excellent of the cavity
Air pressure is selected, argon gas is passed through into the cavity, the flow of the gas is preferably the milliliters/second of 1 milliliters/second~100.
In a preferable embodiment of the invention, the concrete operation step of described PIC method in plasma immersion ion injection
For：(1) the pending part is placed on base station, the pending part and the base station electricity UNICOM；(2) placed in cavity
Cavity is evacuated to 10 by the polytetrafluoroethylene solids (3) of certain mass-3Pa magnitudes；(4) gas source is opened, into the cavity
It is passed through argon gas；(5) argon ion body is produced in the cavity containing the gas by radio frequency source and excited by argon plasma
The fluorine element gone out；(5) back bias voltage pulse is produced by bias generator, the back bias voltage pulse is loaded on the pending part, made
Argon ion (Ar+) and the fluorine element processing pending part surface, you can.It is preferred that the air pressure by cavity described in step (4)
Maintain 0.1Pa~1Pa.To maintain the preferred air pressure of the cavity, preferably holding is passed through the argon gas in the cavity
Flow is the milliliters/second of 1 milliliters/second~100.
In the present invention, the power of the radio frequency source can be selected according to common sense in the field, preferably 50~600W, more
It is good for 50W~300W.
In the present invention, the back bias voltage pulse can be selected according to common sense in the field, wherein the voltage of the back bias voltage
Value is preferably 1KV~60KV；The frequency of the back bias voltage pulse is preferably 50Hz~150Hz；The back bias voltage pulse
Width is preferably the microsecond of 5 microseconds~50.The time of the injection can be selected according to common sense in the field, preferable to reach
Surface treatment effect, the present invention preferably 1 minute~180 minutes, to realize that preferable economic effect is more preferably 3 minutes~60 points
Clock.The implantation dosage of the plasma can be by changing injection length, RF source power and adjustment polytetrafluoroethylene solids
Block is exposed to the volume in argon plasma sheaths, is controlled, injection length is longer or RF source power is higher, and treatment dosage is got over
Greatly.
In a preferable embodiment of the invention, described metal is titanium and titanium alloy.
Raw material, reagent and equipment used in the present invention is commercially available.
In the present invention, above-mentioned optimum condition can be combined on the basis of common sense in the field is met, and be produced of the invention each
Preferred embodiments.
The positive effect of the present invention is：
1st, it is provided by the invention it is a kind of put forward high purity titanium and the method for titanium alloy surface cytocompatibility and biocidal property, mainly
Metallic surface is handled using fluorine element.In a preferable embodiment of the invention, through the treated titanium of the inventive method
The surface of category and titanium alloy is made up of titanium, oxygen, fluorine, carbon, for pellet shape material being evenly distributed, being dispersed in.Therefore, this hair
The bright formation that can promote osteocyte focal adhension, the adhesion for suppressing bacterium so that titanium and titanium alloy surface have good bone
Cell compatibility and bacteriostasis property.
2nd, surface treatment method operating process of the invention is simple, and cost is cheap and easily controllable, is not in thermal oxide
The defects of repeatability is poor in method.
Brief description of the drawings
Fig. 1 is the equipment schematic diagram that plasma immersion injection is carried out to titanium and titanium alloy.
Fig. 2 is the x-ray XPS Analysis figure of titanium metal plate surface-element after processing.
Fig. 3 is the Gaussian fitting result figure at surface of test piece Ti2p peaks after fluorine ion injects pure titanium surface of test piece.
Embodiment
The invention will be further described with reference to the accompanying drawings and examples.
Embodiment 1：
Titanium and titanium alloy are surface-treated using equipment shown in Fig. 1：
Titanium metal plate is placed on base station 1, polytetrafluoroethylene solids 9 are exactly in the solid block being placed on inside cavity 6；
The vacuum of cavity 6 is evacuated to 10 using the two-stage (two-speed) pump pumped vacuum systems comprising mechanical pump 2 and molecular pump 3-3Pa magnitudes；Open argon
Source of the gas 4 is passed through argon gas into the low vacuum cavity, and (argon flow amount is controlled in 6 milliliters/seconds, and air pressure in cavity 6 is maintained
0.5Pa)；RF radio frequency sources 7 (power of radio frequency source is 75W) are opened, argon plasma is produced in cavity 6；Open negative bias potential source
8, back bias voltage pulse is loaded on the titanium block, and (magnitude of voltage of back bias voltage is 5KV, pulse frequency 50Hz, and pulse width is
20 μ s) PIC method in plasma immersion ion injection (injection length is 10 minutes) is carried out, so as to form surface treated titanium
Category.
Embodiment 2：
Titanium alloy is surface-treated using equipment shown in Fig. 1：
Titanium alloy piece is placed on base station 1, polytetrafluoroethylene solids 9 are exactly in the solid block being placed on inside cavity 6；
The vacuum of cavity 6 is evacuated to 10 using the pumped vacuum systems of the two-stage (two-speed) pump comprising mechanical pump 2 and molecular pump 3-3Pa magnitudes；Open
Argon gas source 4 to the low vacuum intracavitary is passed through argon gas, and (argon flow amount control maintains air pressure in cavity 6 in 8 milliliters/seconds
1.0Pa)；RF radio frequency sources 7 (power of radio frequency source is 80W) are opened, argon plasma is produced in cavity 6；Open negative bias potential source
8, (magnitude of voltage of back bias voltage is 5KV to the pulse of loading back bias voltage, and pulse frequency 50Hz, pulse width is 20 μ on the titanium alloy
S) PIC method in plasma immersion ion injection (injection length is 40 minutes) is carried out, so as to form surface treated titanium alloy.
The x-ray XPS Analysis of the titanium of effect example 1 and titanium alloy surface element：
The analysis of chemical elements that titanium plate surface is tested after fluorine ion injection is carried out on x-ray photoelectron spectrograph, with C1s=
Being combined on the basis of 284.6eV to correct.
The preparation method of test sample is in embodiment 1 and embodiment 2：
By the sheet metal that business titanium metal plate and titanium alloy piece are processed into a diameter of 30mm, thickness is 1mm, surface is by beating
Grind, be polished to minute surface after tested.After test specimen is cleaned by ultrasonic 20 minutes successively with analytically pure absolute ethyl alcohol and deionized water
It is put into vacuum chamber, polytetrafluoroethylene solids block is as source ion implantation, before ion implanting, Ar+ sputter cleans surface 10 minutes.
The test result of effect example 1：
The titanium metal plate after article on plasma injection processing and titanium alloy piece surface-element carry out x-ray photoelectron spectroscopy point respectively
Analysis, the ion implanting result of wherein titanium metal plate are as shown in Figure 2.
The surface of fluorine ion injection group test specimen is can be seen that mainly by oxygen, fluorine, titanium, carbon from surface of test piece XPS analysis
Composition, that is, newly increased the signal of fluorine element.Visible, the Ti2p by the Gauss curve fitting to Ti2p peaks3/2Appear in 458.7,
459.9 and 461.6eV, Ti2p1/2464.3,465.5 and 466.9eV are appeared in, corresponds respectively to TiO2Ti4+, TiF3Ti3+
And TiF4Ti4+, XPS analysis and Gaussian fitting result show that fluorine ion is successfully introduced titanium and titanium alloy by the present invention
Surface is formed on surface simultaneously contains Ti3+、Ti4+Surface reforming layer.
It is provided by the invention it is a kind of put forward high purity titanium and the method for titanium alloy surface cytocompatibility and biocidal property, including under
State step：Handling member is treated using plasma immersion injection technology to be surface-treated, wherein the plasma is argon etc.
Gas ions (as working media and build-up of luminance gas), described pending part are metal or the product for being coated with the metal.The present invention
Additionally provide the surface treated metal obtained with methods described and be coated with the product of the surface treated metal, and it
As human body implantation and intervention material application.The present invention uses argon gas as build-up of luminance gas and working media, polytetrafluoroethyl-ne
Source of the alkene as fluorine element, after treatment the cytocompatibility and bacteriostasis of titanium or titanium alloy surface can obtain
Improve, so that after being implanted into human body as bio-medical material using titanium or titanium alloy, its Integrated implant ability and antibacterial energy
Power is improved, and can be applied to the fields such as metallic implant surface processing.This method operating process is simple, and cost is cheap and is easy to
Control, injected without using general plasma immersion in fluorine technique and use carbon tetrafluoride gas source, overcome fluoro-gas and be not easy
The defects of build-up of luminance and destruction atmospheric ozone layer, fluorine element implantation concentration of the invention is easy to adjust.
Although the present invention is disclosed as above with preferred embodiment, so it is not limited to the present invention, any this area skill
Art personnel, without departing from the spirit and scope of the present invention, when a little modification and perfect, therefore the protection model of the present invention can be made
Enclose to work as and be defined by what claims were defined.
Claims (8)
1. a kind of put forward high purity titanium and the method for titanium alloy surface cytocompatibility and biocidal property, this method is injected in plasma
In technique, vacuum work intracavitary, polytetrafluoroethylene solids, under caused plasma sheath excites after working gas build-up of luminance,
Fluorine element is discharged so as to inject titanium and titanium alloy surface；Wherein, in described technique, argon gas is filled with working cavity, and
And air pressure maintains 0.1Pa~1Pa.
2. high purity titanium and the side of titanium alloy surface cytocompatibility and biocidal property are carried according to a kind of described in claim 1
Method, it is characterised in that equipment used includes a cavity, and base station is set in the cavity, polytetrafluoroethylene (PTFE) is set on base station
Gu block, chamber Ligation in vitro radio frequency source, argon gas pump, negative bias potential source, mechanical pump and the molecular pump.
3. high purity titanium and the side of titanium alloy surface cytocompatibility and biocidal property are carried according to a kind of described in claim 2
Method, it is characterised in that the polytetrafluoroethylene solids by being placed in certain mass in vacuum work cavity are used as the source of fluorine element.
4. high purity titanium and the side of titanium alloy surface cytocompatibility and biocidal property are carried according to a kind of described in claim 3
Method, it is characterised in that described polytetrafluoroethylene solids are to be injected positioned at plasma between workpiece base station and reaction cavity
Solid block, in the case where being injected without fluorine ion, this polytetrafluoroethylene solids block is covered with aluminium foil.
5. high purity titanium and the side of titanium alloy surface cytocompatibility and biocidal property are carried according to a kind of described in claim 1
Method, it is characterised in that the flow for the argon gas being passed through in reaction cavity is the milliliters/second of 1 milliliters/second~100.
6. high purity titanium and the side of titanium alloy surface cytocompatibility and biocidal property are carried according to a kind of described in claim 3
Method, it is characterised in that the injection rate of the fluorine element of titanium and titanium alloy surface by change injection length, radio frequency source power
And the distance controlling of adjustment processing base station and polytetrafluoroethylene solids block.
7. high purity titanium and the side of titanium alloy surface cytocompatibility and biocidal property are carried according to a kind of described in claim 3
Method, it is characterised in that the power setting of described radio frequency source is 50~600W.
8. high purity titanium and the side of titanium alloy surface cytocompatibility and biocidal property are carried according to a kind of described in claim 3
Method, it is characterised in that in described technique, set the preferable magnitude of voltage of back bias voltage as 1KV~60KV；Set back bias voltage pulse
Preferable frequency is 50Hz~150Hz；The preferable width of back bias voltage pulse is set as the microsecond of 5 microseconds~50.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| JP7400049B2 (en) | 2018-06-01 | 2023-12-18 | 京セラ株式会社 | Composite material manufacturing method |
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