CN108434517A - Antibacterial dental implant and preparation method thereof - Google Patents
Antibacterial dental implant and preparation method thereof Download PDFInfo
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- CN108434517A CN108434517A CN201810157497.6A CN201810157497A CN108434517A CN 108434517 A CN108434517 A CN 108434517A CN 201810157497 A CN201810157497 A CN 201810157497A CN 108434517 A CN108434517 A CN 108434517A
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- 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
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- A—HUMAN NECESSITIES
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- 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
- A61L27/28—Materials for coating prostheses
- A61L27/30—Inorganic materials
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- 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
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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
- A61L27/50—Materials characterised by their function or physical properties, e.g. injectable or lubricating compositions, shape-memory materials, surface modified materials
- A61L27/54—Biologically active materials, e.g. therapeutic substances
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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
- A61L27/50—Materials characterised by their function or physical properties, e.g. injectable or lubricating compositions, shape-memory materials, surface modified materials
- A61L27/56—Porous materials, e.g. foams or sponges
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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
- C23C14/48—Ion implantation
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
- C25D11/02—Anodisation
- C25D11/024—Anodisation under pulsed or modulated current or potential
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
- C25D11/02—Anodisation
- C25D11/026—Anodisation with spark discharge
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
- C25D11/02—Anodisation
- C25D11/26—Anodisation of refractory metals or alloys based thereon
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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
- A61L2300/00—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices
- A61L2300/10—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices containing or releasing inorganic materials
- A61L2300/102—Metals or metal compounds, e.g. salts such as bicarbonates, carbonates, oxides, zeolites, silicates
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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
- A61L2300/00—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices
- A61L2300/10—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices containing or releasing inorganic materials
- A61L2300/102—Metals or metal compounds, e.g. salts such as bicarbonates, carbonates, oxides, zeolites, silicates
- A61L2300/104—Silver, e.g. silver sulfadiazine
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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
- A61L2300/00—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices
- A61L2300/40—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices characterised by a specific therapeutic activity or mode of action
- A61L2300/404—Biocides, antimicrobial agents, antiseptic agents
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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
- A61L2300/00—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices
- A61L2300/60—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices characterised by a special physical form
- A61L2300/606—Coatings
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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
- A61L2420/00—Materials or methods for coatings medical devices
- A61L2420/02—Methods for coating medical devices
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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
- 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 provides a kind of antibacterial dental implants and preparation method thereof.The antibacterial dental implant includes：Dental implant ontology；Differential arc oxidation film layer is arranged on the surface of dental implant ontology；And nanometer antibacterial function material, it is supported on differential arc oxidation film layer.The application on dental implant ontology by being arranged differential arc oxidation film layer, so that the surface pore structure more horn of plenty of dental implant ontology, wherein there is the crateriform pore structure of many classes, therefore the surface roughness of dental implant ontology can both have been increased, surface porosity factor is substantially increased again, the antibiotic functional material of the nano-scale injected at this time by PIC method in plasma immersion ion can not only be infused in the surface of differential arc oxidation film layer, it can especially be injected into the pore structure of differential arc oxidation film layer, considerably increase the load capacity of nanometer antibacterial function material, and when bacterium enters micropore, it can sterilize in time, and then durable antibiotic is achieved the purpose that.
Description
Technical field
The present invention relates to dental implant fields, in particular to a kind of antibacterial dental implant and preparation method thereof.
Background technology
Tooth be in Human Oral Cavity with certain form height calcification tissue, have chewing, help pronounce and retaining surface
The function of portion's good appearance.Currently, China's tooth number of defect or missing caused by the reasons such as dental caries, periodontosis, wound reaches
1000000000 or more, tooth, jawbone, remporomandibular joint defect can cause the physiological dysfunctions of patient, influence beauty, it is also possible to
Cause mental handicape.
Tooth-implanting as it is a kind of with natural teeth function, structure and the quite similar repair mode of aesthetic effect, at
Solve the problems, such as that the first choice of patient's agomphosis, the dental implant of the huge market demand, the at present annual production and marketing in the whole world reach for dentistry
15000000, and China mainland sales volume in 2015 is only 400,000, main cause is that the dental implant in 90% or more China relies on
Import, it is expensive.It there is problems in addition to tooth-implanting is expensive：First：Since dental implant surface biology is lived
Property is not ideal enough, causes sclerous tissues' implant bone regeneration capability poor, bad, bioactivity and bone formation performance are combined with surrounding tissue
It is not ideal enough.Second：Dental implant surface causes the infection of planting body Related Bacteria to occur without antibiotic property.In human body environment and tooth
In the reaction of planting body material, the surface of material plays very important effect.In addition, current planting body mostly uses spiral shell
The columnar configuration design of line-cone is planted at agomphosis position to implant direction, position and the requirement for retaining bone amount etc.
Height, doctor, which needs to carry out largely training, can just master a skill.
Therefore, the ingredient properties and structure, the implantation effect for being effectively improved material of dental implant surface how are controlled, it is inexpensive
The planting body of object U.S. has become the tooth-implanting technology critical issue universal in China.
Currently, have been reported that enhances the anti-microbial property of dental implant by loading silver in dental implant surface, for example pass through
PIC method in plasma immersion ion method for implanting loads silver in dental implant, and still, the quantity for the silver that this method can load has
Limit, it is difficult to achieve the purpose that durable antibiotic.
Invention content
The main purpose of the present invention is to provide a kind of antibacterial dental implants and preparation method thereof, to solve in the prior art
Dental implant the problem of being difficult to reach durable antibiotic purpose.
To achieve the goals above, according to an aspect of the invention, there is provided a kind of antibacterial dental implant, including：Tooth
Planting body ontology；Differential arc oxidation film layer is arranged on the surface of dental implant ontology；And nanometer antibacterial function material, load
On differential arc oxidation film layer.
Further, the thickness of above-mentioned differential arc oxidation film layer is 2~15 μm, preferably 3~10 μm；In differential arc oxidation film layer
The aperture in hole is 2~10 μm, preferably 2~5 μm；The porosity of differential arc oxidation film layer is 5~20%, preferably 8~20%；It is excellent
It includes Ca and P to select the active element in differential arc oxidation film layer.
Further, above-mentioned nanometer antibacterial function material includes nano silver, and preferably nanometer antibacterial function material includes nanometer
Silver and Nano-Zinc.
Further, above-mentioned dental implant ontology is titanium-base alloy ontology, and titanium-base alloy ontology is selected from pure titanium, Ti-6Al-
One kind in 4V, Ti-6Al-17Nb, Ti-13Nb-13Zr and Ti-5Zr-3Mo-15Nb.
According to another aspect of the present invention, a kind of preparation method of antibacterial dental implant is provided, which includes：
Step S1 carries out differential arc oxidation, with the growth in situ differential arc oxidation film layer on dental implant ontology to dental implant ontology；Step
S2, to carrying out PIC method in plasma immersion ion injection by the dental implant ontology of differential arc oxidation, on differential arc oxidation film layer
Load nanometer antibacterial function material.
Further, the PIC method in plasma immersion ion of above-mentioned steps S2 injects using plasma plasma immersion ion implantation
Equipment is implemented, and the vacuum degree for controlling the vacuum chamber of PIC method in plasma immersion ion injection device is 5 × 10-3~8 × 10-3Pa,
Injecting voltage is -50~-30KV, and injection length is 1~3h, and the element of preferred steps S2 injections is silver ion and/or zinc ion.
Further, above-mentioned vacuum degree is 5.5 × 10-3~6.5 × 10-3Pa, injecting voltage are -35~-45KV, injection
Time is 1.5~2.5h.
Further, in electrolyte used by above-mentioned differential arc oxidation, the concentration of calcium constituent is denoted as m mol/L, P elements
Concentration be denoted as n mol/L, as 0.01≤m ＜ 0.2, (0.1m+0.025)≤n ＜ 0.05；As 0.2≤m≤0.6,
When 0.075≤n≤m/0.875, preferably 0.4 ＜ m≤0.6,0.25≤n≤m/0.875；It is preferred that calcium source is selected from calcium acetate, chlorination
The one or more of calcium, calcium dihydrogen phosphate, calcium glycerophosphate, calcium citrate, calcium lactate and calcium oxide；More preferable phosphorus source is selected from sweet
One or more of oleophosphoric acid sodium, sodium dihydrogen phosphate, disodium hydrogen phosphate, calgon and polyphosphate sodium.
Further, above-mentioned electrolyte further includes EDTA-2Na and sodium metasilicate, preferably by sodium hydroxide or potassium hydroxide
Electrolyte ph is adjusted between 11~14.
Further, the differential arc oxidation of above-mentioned steps S1 uses the voltage of power supply for 50~500V, the output pulse of power supply
Frequency is 100~1000Hz, and the pulse width of power supply is 8~500 μ s, and the peak point current of power supply is 0~300A, and oxidization time is
3~30min.
Further, above-mentioned preparation method further includes that the mistake of blasting treatment is carried out to dental implant ontology before step S1
Journey, for the abrasive material preferably used during blasting treatment for SiC or schmigel, the grain size of further preferred abrasive material is 50~300 μ
m；It is preferred that the process of blasting treatment sandblasting distance be 10~15cm, compression pressure be 2~10bar, injecting time be 5~
60s。
Further, above-mentioned dental implant ontology is titanium-base alloy ontology, and titanium-base alloy ontology is selected from pure titanium, Ti-6Al-
One kind in 4V, Ti-6Al-17Nb, Ti-13Nb-13Zr and Ti-5Zr-3Mo-15Nb；It is preferred that dental implant ontology is by increasing material
Manufacturing technology obtains, and increases material manufacturing technology is electron beam melting manufacturing technology and selective laser sintering.
It applies the technical scheme of the present invention, the application on dental implant ontology by being arranged differential arc oxidation film layer so that
The surface pore structure of dental implant ontology more horn of plenty wherein there are the crateriform pore structures of many classes, therefore can both increase
Add the surface roughness of dental implant ontology, and substantially increase surface porosity factor, passes through PIC method in plasma immersion ion at this time
The antibiotic functional material of the nano-scale of injection can not only be infused in the surface of differential arc oxidation film layer, it is particularly possible to be injected into micro-
In the pore structure of arc oxidation film layer, the load capacity of nanometer antibacterial function material is considerably increased, and when bacterium enters micropore,
It can sterilize in time, and then achieve the purpose that durable antibiotic.
Description of the drawings
The accompanying drawings which form a part of this application are used to provide further understanding of the present invention, and of the invention shows
Meaning property embodiment and its explanation are not constituted improper limitations of the present invention for explaining the present invention.In the accompanying drawings：
Fig. 1 shows the tooth-implanting swept-volume electromicroscopic photograph of the embodiment 1 after blasting treatment according to the present invention；
Fig. 2 shows embodiment 1 by sandblasting and differential arc oxidation processing after dental implant surface stereoscan photograph.
Specific implementation mode
It should be noted that in the absence of conflict, the features in the embodiments and the embodiments of the present application can phase
Mutually combination.The present invention will be described in detail below with reference to the accompanying drawings and embodiments.
As the application background technology is analyzed, the silver-colored limited amount that the silver-colored mode of existing load loads leads to tooth kind
Implant is difficult to achieve the purpose that durable antibiotic, in order to solve this problem, provides a kind of antibacterial dental implant, including dental implant
Ontology, differential arc oxidation film layer and nanometer antibacterial function material, differential arc oxidation film layer are arranged on the surface of dental implant ontology；It receives
Nano antibacterial functional material is supported on differential arc oxidation film layer.
The application on dental implant ontology by being arranged differential arc oxidation film layer so that the surface holes knot of dental implant ontology
Structure more horn of plenty, wherein there are the crateriform pore structures of many classes, therefore the surface that can have both increased dental implant ontology is thick
Rugosity, and surface porosity factor is substantially increased, the antibacterial work(of the nano-scale injected at this time by PIC method in plasma immersion ion
Energy material can not only be infused in the surface of differential arc oxidation film layer, it is particularly possible to it is injected into the pore structure of differential arc oxidation film layer,
The load capacity of nanometer antibacterial function material is considerably increased, and when bacterium enters micropore, can sterilized in time, and then reach
The purpose of durable antibiotic.
In a kind of preferred embodiment of the application, the thickness of above-mentioned differential arc oxidation film layer is 2~15 μm, preferably 3~
10μm；The aperture of differential arc oxidation film layer mesoporous is 2~10 μm, preferably 2~5 μm；The porosity of differential arc oxidation film layer be 5~
20%, preferably 8~20%；It is preferred that the active element in differential arc oxidation film layer includes Ca and P.Above-mentioned micro-arc oxidation films layer surface
Coarse pore structure is conducive to seek connections with growth of the osteoblast on its surface, and then is formed securely in bone and dental implant interface
It is chimeric, prevent implantation material from failing, the differential arc oxidation film layer with These characteristics to the packing interaction of bone and dental implant more
For protrusion.In addition, Ca, P isoreactivity element can further increase the bioactivity of dental implant, promote Integrated implant.
The preferably above-mentioned nanometer antibacterial function material of the application includes nano silver, and nanometer Ag ion is embedded into differential arc oxidation film layer
In so that the silver of this nanoscale will not recycle in human body fluid, and be integrally fixed at dental implant surface, therefore can rise
To significant antibacterial action.Additionally, it is preferred that nanometer antibacterial function material includes nano silver and Nano-Zinc, the injection of Zn ions can
It stimulates cellular proliferation, promotes Cellular alkaline phosphatase activity, promote collagen synthesis, to play promotion skeletonization, improve and plant
Enter the combination of material and bone.In addition, when the load capacity of Zn ions reaches certain value, antibacterial action can also be played.
The dental implant ontology of common material in the prior art may be used in the dental implant ontology of the application, preferably above-mentioned
Dental implant ontology is titanium-base alloy ontology, and titanium-base alloy ontology is selected from pure titanium, Ti-6Al-4V, Ti-6Al-17Nb, Ti-
One kind in 13Nb-13Zr and Ti-5Zr-3Mo-15Nb.
In another typical embodiment of the application, a kind of preparation method of antibacterial dental implant, the system are provided
Preparation Method includes：Step S1 carries out differential arc oxidation, with the growth in situ differential of the arc oxygen on dental implant ontology to dental implant ontology
Change film layer；Step S2, to carrying out PIC method in plasma immersion ion injection by the dental implant ontology of differential arc oxidation, in the differential of the arc
Nanometer antibacterial function material is loaded on oxidation film layer.
By differential arc oxidization technique on dental implant ontology growth in situ differential arc oxidation film layer, the differential arc oxidation film layer and
The chimeric degree of dental implant ontology is higher, relatively securely；And make the surface pore structure more horn of plenty of dental implant ontology, wherein
There are the crateriform pore structures of many classes, therefore can not only increase the surface roughness of dental implant ontology, but also greatly improve
The antibiotic functional material of surface porosity factor, the nano-scale injected at this time by PIC method in plasma immersion ion can not only be noted
Enter on the surface of differential arc oxidation film layer, it is particularly possible to be injected into the pore structure of differential arc oxidation film layer, it is anti-to considerably increase nanometer
The load capacity of bacterium functional material, and when bacterium enters micropore, can sterilize in time, and then reached the mesh of durable antibiotic
's.
The implementation of the PIC method in plasma immersion ion injection of the application above-mentioned steps S2 may be used with reference to the prior art, excellent
It selects using plasma plasma immersion ion implantation equipment to implement, and controls the vacuum chamber of PIC method in plasma immersion ion injection device
Vacuum degree be 5 × 10-3~8 × 10-3Pa, injecting voltage are 30~50KV, and injection length is 1~3h, preferred steps S2 injections
Element be silver ion and/or zinc ion.It can securely be supported on micro-arc oxidation films as much as possible with the ion for ensureing injected
On layer, and the quantity of loaded ion is improved as far as possible.
In addition, there is the activity of a large amount of non-ontology element due to after differential arc oxidation is handled, on dental implant ontology
Element so that the load of silver ion, zinc ion for being injected etc. may be affected, in order to improve the injection of ion as far as possible
Amount, preferably above-mentioned vacuum degree are 5.5 × 10-3~6.5 × 10-3Pa, injecting voltage be -25~-35KV, injection length be 1.5~
2.5h。
The electrolyte composition of the application is with the electrolyte currently used for porous metal implants differential arc oxidation at being grouped as
It is similar, that is, contain calcium constituent, P elements and complexing agent, and the usage ratio of calcium constituent and P elements is for being formed by original position
The bioactivity for growing film layer has certain influence.Since calcium ion is different with the electrical property of phosphonium ion, in differential arc oxidation
In calcium ion in finally formed growth in situ film layer and the ratio of phosphonium ion and the ratio of both of electrolyte be also not
With.Based on this in order to improve the bioactivity of growth in situ film layer, in electrolyte used by above-mentioned differential arc oxidation, calcium constituent
Concentration be denoted as mmol/L, the concentration of P elements is denoted as n mol/L, as 0.01≤m ＜ 0.2, (0.1m+0.025)≤n ＜
0.05；As 0.2≤m≤0.6, when 0.075≤n≤m/0.875, preferably 0.4 ＜ m≤0.6,0.25≤n≤m/0.875 makes
It is controllable in optimization range to obtain calcium phosphorus element content, not only can guarantee the good bioactivity of growth in situ film layer of preparation, but also
It can increase to avoid the cost brought because repeatedly blindly attempting, improve productivity effect.Additionally, it is preferred that calcium source be selected from calcium acetate,
The one or more of calcium chloride, calcium dihydrogen phosphate, calcium glycerophosphate, calcium citrate, calcium lactate and calcium oxide；More preferable phosphorus source choosing
From one or more of sodium glycero-phosphate, sodium dihydrogen phosphate, disodium hydrogen phosphate, calgon and polyphosphate sodium.
Further, it is preferable to which above-mentioned electrolyte further includes EDTA-2Na and sodium metasilicate, above-mentioned EDTA-2Na is complexing agent,
It is easy to ionize in the solution, generates free Na+And H2Y2-(wherein Y=[2 (OOCCH2)NCH2CH2N(CH2COO)2]4-),
Ionize the H generated2Y2-Easily with the Ca in electrolyte2+Chelating generates CaY2-, to improve the conductivity of electrolyte.In order to reduce
Arcing voltage adds sodium metasilicate (SiO in the electrolytic solution3 2-), and in order to ensure voltage stabilization, the concentration of preferably above-mentioned sodium metasilicate
For 0.01~0.04mol/L.Electrolyte ph is adjusted between 11~14 preferably by sodium hydroxide or potassium hydroxide, to be formed
Stable alkaline oxygenated environment.
In the application another kind preferred embodiment, the differential arc oxidation of above-mentioned steps S1 use the voltage of power supply for 50~
The output pulse frequency of 500V, power supply are 100~1000Hz, 8~500 μ s of pulse width tail of power supply, the peak point current of power supply
For 0~300A, oxidization time is 3~30min.Within the above range by the control of above-mentioned power supply parameter, it can utilize in Dental implantion
Metastable electric field forms the differential arc oxidation film layer that film layer is thicker and thickness is relatively uniform in body ontology.
In the application another preferred embodiment, above-mentioned preparation method further includes to dental implant before step S1
Ontology carries out the process of blasting treatment, and the abrasive material preferably used during blasting treatment is SiC or schmigel, further preferably
The grain size of abrasive material is 50~300 μm；It is preferred that the sandblasting distance of the process of blasting treatment is 10~15cm, compression pressure 2
~10bar, injecting time are 5~60s.
Dental implant body surface can be effectively removed in conjunction with differential arc oxidation by carrying out blasting treatment to dental implant ontology
Corner angle, clean surface increase surface roughness；Blasting treatment simultaneously can make dental implant body surface that there is certain pressure to answer
Power can offset the tensile stress that follow-up differential arc oxidation generates, and then reduce the stress of differential arc oxidation film layer, improve micro-arc oxidation films
Bond strength of the layer in dental implant surface.
Furthermore it is preferred that above-mentioned dental implant ontology is titanium-base alloy ontology, further preferred titanium-base alloy ontology is selected from pure
One kind in titanium, Ti-6Al-4V, Ti-6Al-17Nb, Ti-13Nb-13Zr and Ti-5Zr-3Mo-15Nb；It is preferred that dental implant sheet
Body is obtained by increases material manufacturing technology, and increases material manufacturing technology is electron beam melting manufacturing technology and selective laser sintering.
In summary, the present invention comprehensively utilizes blasting treatment, differential arc oxidation, PIC method in plasma immersion ion injection technique pair
Dental implant ontology carry out surface modification, can by adjusting sandblasting parameter, electrolyte composition and concentration, differential arc oxidation parameter,
PIC method in plasma immersion ion injection parameter, Optimized Matching so that the elemental composition in the dental implant surface coating of preparation can
Control.Obtained antibacterial dental implant possesses excellent anti-microbial property compared with traditional dental implant.
Below with reference to embodiment and comparative example, the advantageous effect of the application is further illustrated.
Embodiment 1
Dental implant ontology：The medical pure titanium prepared by forging technology is selected to be used as dental implant ontology.
Blasting treatment：Strength blasting treatment is carried out to dental implant ontology, the grain size of abrasive material SiC, abrasive material are 150 μm,
Sandblasting distance is 12cm, compression pressure 8bar, injecting time 30s, the configuration of surface obtained after sandblasting, using sweeping
Electronic Speculum observation is retouched, pattern is as shown in Figure 1.Use the dental implant ontology after sandblasting acetone and deionized water ultrasound thoroughly clear successively
20min is washed, is dried for standby.
Micro-arc oxidation electrolyte is prepared：Calcium acetate, sodium dihydrogen phosphate are dissolved in deionized water, reagent is uniformly mixed,
It is configured to electrolyte, wherein a concentration of 0.01mol/L of calcium acetate, a concentration of 0.035mol/L, EDTA-2Na of sodium dihydrogen phosphate
A concentration of 0.02mol/L, Na2SiO3A concentration of 0.04mol/L, add suitable KOH, adjust solution pH value be 11.Profit
With scanning electron microscopic observation, pattern is as shown in Figure 2.
Differential arc oxidation processing：Dental implant ontology after sandblasting is completely submerged in above-mentioned electrolyte and carries out differential arc oxidation
Processing.The supply voltage for adjusting power supply is 200V, output pulse frequency 500Hz, 300 μ s of pulse width, peak point current setting
150A, oxidization time 20min generate one layer of differential arc oxidation film layer in dental implant body surface.Entire micro-arc oxidation process
The temperature of middle control electrolyte at 20 DEG C hereinafter, taking out sample after reaction, rinse well, is dried for standby by deionized water.
PIC method in plasma immersion ion injection is handled：By differential arc oxidation, treated that dental implant ontology is placed on plasma
Ion implanting is carried out on the vacuum chamber target platform of body plasma immersion ion implantation equipment, vacuum degree in vacuum chamber is 6 × 10-3Pa, injection electricity
Pressure is 40KV, injection length 2h, and injection element is silver ion and zinc ion.
Embodiment 2
The preparation of dental implant ontology：Ti-6Al-4V Dental implantions are manufactured by increasing material manufacturing electron beam melting technology technology
Body ontology.
Blasting treatment：Strength blasting treatment is carried out to dental implant ontology, the grain size of abrasive material SiC, abrasive material are 300 μm,
Sandblasting distance is 12cm, compression pressure 8bar, injecting time 30s.Dental implant ontology after sandblasting is used successively
Acetone and deionized water ultrasound thoroughly clean 20min, are dried for standby.
The other the same as in Example 1.
Embodiment 3
The preparation of dental implant ontology：The medical pure titanium prepared by forging technology is selected to be used as dental implant ontology.
Blasting treatment：Strength blasting treatment is carried out to dental implant ontology, the grain size of abrasive material SiC, abrasive material are 50 μm, spray
Sand distance is 12cm, compression pressure 8bar, injecting time 30s.To the dental implant ontology after sandblasting successively with third
Ketone and deionized water ultrasound thoroughly clean 20min, are dried for standby.
The other the same as in Example 1.
Embodiment 4
The preparation of dental implant ontology：The medical pure titanium prepared by forging technology is selected to be used as dental implant ontology.
Blasting treatment：Strength blasting treatment is carried out to dental implant ontology, the grain size of abrasive material SiC, abrasive material are 150 μm,
Sandblasting distance is 15cm, compression pressure 8bar, injecting time 30s.Dental implant ontology after sandblasting is used successively
Acetone and deionized water ultrasound thoroughly clean 20min, are dried for standby.
The other the same as in Example 1.
Embodiment 5
The preparation of dental implant ontology：The medical pure titanium prepared by forging technology is selected to be used as dental implant ontology.
Blasting treatment：Strength blasting treatment is carried out to dental implant ontology, the grain size of abrasive material SiC, abrasive material are 150 μm,
Sandblasting distance is 10cm, compression pressure 8bar, injecting time 30s.Dental implant ontology after sandblasting is used successively
Acetone and deionized water ultrasound thoroughly clean 20min, are dried for standby.
The other the same as in Example 1.
Embodiment 6
The preparation of dental implant ontology：The medical pure titanium prepared by forging technology is selected to be used as dental implant ontology.
Blasting treatment：Strength blasting treatment is carried out to dental implant ontology, the grain size of abrasive material SiC, abrasive material are 150 μm,
Sandblasting distance is 12cm, compression pressure 10bar, injecting time 30s.Dental implant ontology after sandblasting is used successively
Acetone and deionized water ultrasound thoroughly clean 20min, are dried for standby.
The other the same as in Example 1.
Embodiment 7
The preparation of dental implant ontology：The medical pure titanium prepared by forging technology is selected to be used as dental implant ontology.
Blasting treatment：Strength blasting treatment is carried out to dental implant ontology, the grain size of abrasive material SiC, abrasive material are 150 μm,
Sandblasting distance is 15cm, compression pressure 2bar, injecting time 30s.Dental implant ontology after sandblasting is used successively
Acetone and deionized water ultrasound thoroughly clean 20min, are dried for standby.
The other the same as in Example 1.
Embodiment 8
The preparation of dental implant ontology：The medical pure titanium prepared by forging technology is selected to be used as dental implant ontology.
Blasting treatment：Strength blasting treatment is carried out to dental implant ontology, the grain size of abrasive material SiC, abrasive material are 150 μm,
Sandblasting distance is 12cm, compression pressure 8bar, injecting time 60s.Dental implant ontology after sandblasting is used successively
Acetone and deionized water ultrasound thoroughly clean 20min, are dried for standby.
The other the same as in Example 1.
Embodiment 9
The preparation of dental implant ontology：The medical pure titanium prepared by forging technology is selected to be used as dental implant ontology.
Blasting treatment：Strength blasting treatment is carried out to dental implant ontology, the grain size of abrasive material SiC, abrasive material are 150 μm,
Sandblasting distance is 12cm, compression pressure 8bar, injecting time 5s.To the dental implant ontology after sandblasting successively with third
Ketone and deionized water ultrasound thoroughly clean 20min, are dried for standby.
The other the same as in Example 1.
Embodiment 10
The preparation of dental implant ontology：The medical pure titanium prepared by forging technology is selected to be used as dental implant ontology.
Blasting treatment：Strength blasting treatment is carried out to dental implant ontology, abrasive material is schmigel, and the grain size of abrasive material is 150 μ
M, sandblasting distance are 12cm, compression pressure 8bar, injecting time 30s.Successively to the dental implant ontology after sandblasting
20min is thoroughly cleaned with acetone and deionized water ultrasound, is dried for standby.
The other the same as in Example 1.
Embodiment 11
The preparation of dental implant ontology：The medical pure titanium prepared by forging technology is selected to be used as dental implant ontology.
Blasting treatment：Strength blasting treatment is carried out to dental implant ontology, the grain size of abrasive material SiC, abrasive material are 150 μm,
Sandblasting distance is 18cm, compression pressure 8bar, injecting time 30s.Dental implant ontology after sandblasting is used successively
Acetone and deionized water ultrasound thoroughly clean 20min, are dried for standby.
The other the same as in Example 1.
Embodiment 12
The preparation of dental implant ontology：The medical pure titanium prepared by forging technology is selected to be used as dental implant ontology.
Without sandblasting, the other the same as in Example 1.
Embodiment 13
Micro-arc oxidation electrolyte is prepared：Calcium acetate, sodium dihydrogen phosphate are dissolved in deionized water, reagent is uniformly mixed,
It is configured to electrolyte, wherein a concentration of 0.11mol/L of calcium acetate, a concentration of 0.038mol/L, EDTA-2Na of sodium dihydrogen phosphate
A concentration of 0.2mol/L, Na2SiO3A concentration of 0.04mol/L, add suitable KOH, adjust solution pH value be 11.
Remaining is the same as embodiment 1.
Embodiment 14
Micro-arc oxidation electrolyte is prepared：Calcium acetate, sodium dihydrogen phosphate are dissolved in deionized water, reagent is uniformly mixed,
It is configured to electrolyte, wherein a concentration of 0.18mol/L of calcium acetate, a concentration of 0.045mol/L, EDTA-2Na of sodium dihydrogen phosphate
A concentration of 0.38mol/L, Na2SiO3A concentration of 0.04mol/L, add suitable KOH, adjust solution pH value be 11.
Embodiment 15
Micro-arc oxidation electrolyte is prepared：Calcium acetate, sodium dihydrogen phosphate are dissolved in deionized water, reagent is uniformly mixed,
It is configured to electrolyte, wherein a concentration of 0.2mol/L of calcium acetate, a concentration of 0.21mol/L of sodium dihydrogen phosphate, EDTA-2Na's
A concentration of 1.04mol/L, Na2SiO3A concentration of 0.04mol/L, add suitable KOH, adjust solution pH value be 11.
Remaining is the same as embodiment 1.
Embodiment 16
With embodiment 1 difference lies in, calcium acetate, sodium dihydrogen phosphate are dissolved in deionized water, reagent is uniformly mixed,
It is configured to electrolyte, wherein a concentration of 0.58mol/L of calcium acetate, a concentration of 0.65mol/L of sodium dihydrogen phosphate, EDTA-2Na's
A concentration of 3.8mol/L, Na2SiO3A concentration of 0.04mol/L, add suitable KOH, adjust solution pH value be 11.
Remaining is the same as embodiment 1.
Embodiment 17
With embodiment 1 difference lies in, calcium acetate, sodium dihydrogen phosphate are dissolved in deionized water, reagent is uniformly mixed,
It is configured to electrolyte, wherein a concentration of 0.4mol/L of calcium acetate, a concentration of 0.45mol/L of sodium dihydrogen phosphate, EDTA-2Na's
A concentration of 2.2mol/L, Na2SiO3A concentration of 0.04mol/L, add suitable KOH, adjust solution pH value be 11.
Remaining is the same as embodiment 1.
Embodiment 18
Calcium acetate, sodium dihydrogen phosphate are dissolved in deionized water, reagent is uniformly mixed, is configured to electrolyte, wherein second
Sour calcium concentration be 0.01mol/L, a concentration of 0.02mol/L of a concentration of 0.035mol/L of sodium dihydrogen phosphate, EDTA-2Na,
Na2SiO3A concentration of 0.04mol/L, add suitable KOH, adjust solution pH value be 14.
Remaining is the same as embodiment 1.
Embodiment 19
Differential arc oxidation processing：Dental implant ontology after sandblasting is completely submerged in above-mentioned electrolyte and carries out differential arc oxidation
Processing.The supply voltage for adjusting power supply is 500V, output pulse frequency 500Hz, 300 μ s of pulse width, peak point current setting
150A, oxidization time 20min generate one layer of differential arc oxidation film layer in dental implant body surface.Entire micro-arc oxidation process
The temperature of middle control electrolyte at 20 DEG C hereinafter, taking out sample after reaction, rinse well, is dried for standby by deionized water.
Remaining is the same as embodiment 1.
Embodiment 20
Differential arc oxidation processing：Dental implant ontology after sandblasting is completely submerged in above-mentioned electrolyte and carries out differential arc oxidation
Processing.The supply voltage for adjusting power supply is 50V, output pulse frequency 500Hz, 300 μ s of pulse width, peak point current setting
150A, oxidization time 20min generate one layer of differential arc oxidation film layer in dental implant body surface.Entire micro-arc oxidation process
The temperature of middle control electrolyte at 20 DEG C hereinafter, taking out sample after reaction, rinse well, is dried for standby by deionized water.
Remaining is the same as embodiment 1.
Embodiment 21
Differential arc oxidation processing：Dental implant ontology after sandblasting is completely submerged in above-mentioned electrolyte and carries out differential arc oxidation
Processing.The supply voltage for adjusting power supply is 200V, output pulse frequency 100Hz, 300 μ s of pulse width, peak point current setting
150A, oxidization time 20min generate one layer of differential arc oxidation film layer in dental implant body surface.Entire micro-arc oxidation process
The temperature of middle control electrolyte at 20 DEG C hereinafter, taking out sample after reaction, rinse well, is dried for standby by deionized water.
Remaining is the same as embodiment 1.
Embodiment 22
Differential arc oxidation processing：Dental implant ontology after sandblasting is completely submerged in above-mentioned electrolyte and carries out differential arc oxidation
Processing.The supply voltage for adjusting power supply is 200V, output pulse frequency 1000Hz, 300 μ s of pulse width, peak point current setting
150A, oxidization time 20min generate one layer of differential arc oxidation film layer in dental implant body surface.Entire micro-arc oxidation process
The temperature of middle control electrolyte at 20 DEG C hereinafter, taking out sample after reaction, rinse well, is dried for standby by deionized water.
Remaining is the same as embodiment 1.
Embodiment 23
Differential arc oxidation processing：Dental implant ontology after sandblasting is completely submerged in above-mentioned electrolyte and carries out differential arc oxidation
Processing.The supply voltage for adjusting power supply is 200V, output pulse frequency 500Hz, 80 μ s of pulse width, peak point current setting
150A, oxidization time 20min generate one layer of differential arc oxidation film layer in dental implant body surface.Entire micro-arc oxidation process
The temperature of middle control electrolyte at 20 DEG C hereinafter, taking out sample after reaction, rinse well, is dried for standby by deionized water.
Remaining is the same as embodiment 1.
Embodiment 24
Differential arc oxidation processing：Dental implant ontology after sandblasting is completely submerged in above-mentioned electrolyte and carries out differential arc oxidation
Processing.The supply voltage for adjusting power supply is 500V, output pulse frequency 500Hz, 500 μ s of pulse width, peak point current setting
150A, oxidization time 20min generate one layer of differential arc oxidation film layer in dental implant body surface.Entire micro-arc oxidation process
The temperature of middle control electrolyte at 20 DEG C hereinafter, taking out sample after reaction, rinse well, is dried for standby by deionized water.
Remaining is the same as embodiment 1.
Embodiment 25
Differential arc oxidation processing：Dental implant ontology after sandblasting is completely submerged in above-mentioned electrolyte and carries out differential arc oxidation
Processing.The supply voltage for adjusting power supply is 500V, output pulse frequency 500Hz, 300 μ s of pulse width, peak point current setting
300A, oxidization time 20min generate one layer of differential arc oxidation film layer in dental implant body surface.Entire micro-arc oxidation process
The temperature of middle control electrolyte at 20 DEG C hereinafter, taking out sample after reaction, rinse well, is dried for standby by deionized water.
Remaining is the same as embodiment 1.
Embodiment 26
Differential arc oxidation processing：Dental implant ontology after sandblasting is completely submerged in above-mentioned electrolyte and carries out differential arc oxidation
Processing.The supply voltage for adjusting power supply is 500V, output pulse frequency 500Hz, 300 μ s of pulse width, peak point current setting
15A, oxidization time 20min generate one layer of differential arc oxidation film layer in dental implant body surface.In entire micro-arc oxidation process
The temperature of control electrolyte at 20 DEG C hereinafter, taking out sample after reaction, rinse well, is dried for standby by deionized water.
Remaining is the same as embodiment 1.
Embodiment 27
Differential arc oxidation processing：Dental implant ontology after sandblasting is completely submerged in above-mentioned electrolyte and carries out differential arc oxidation
Processing.The supply voltage for adjusting power supply is 500V, output pulse frequency 500Hz, 300 μ s of pulse width, peak point current setting
150A, oxidization time 30min generate one layer of differential arc oxidation film layer in dental implant body surface.Entire micro-arc oxidation process
The temperature of middle control electrolyte at 20 DEG C hereinafter, taking out sample after reaction, rinse well, is dried for standby by deionized water.
Remaining is the same as embodiment 1.
Embodiment 28
Differential arc oxidation processing：Dental implant ontology after sandblasting is completely submerged in above-mentioned electrolyte and carries out differential arc oxidation
Processing.The supply voltage for adjusting power supply is 500V, output pulse frequency 500Hz, 300 μ s of pulse width, peak point current setting
150A, oxidization time 3min generate one layer of differential arc oxidation film layer in dental implant body surface.In entire micro-arc oxidation process
The temperature of control electrolyte at 20 DEG C hereinafter, taking out sample after reaction, rinse well, is dried for standby by deionized water.
Remaining is the same as embodiment 1.
Embodiment 29
Differential arc oxidation processing：Dental implant ontology after sandblasting is completely submerged in above-mentioned electrolyte and carries out differential arc oxidation
Processing.The supply voltage for adjusting power supply is 600V, output pulse frequency 80Hz, 300 μ s of pulse width, peak point current setting
150A, oxidization time 20min generate one layer of differential arc oxidation film layer in dental implant body surface.Entire micro-arc oxidation process
The temperature of middle control electrolyte at 20 DEG C hereinafter, taking out sample after reaction, rinse well, is dried for standby by deionized water.
Remaining is the same as embodiment 1.
Embodiment 30
PIC method in plasma immersion ion injection is handled：By differential arc oxidation, treated that dental implant ontology is placed on plasma
Ion implanting is carried out on the vacuum chamber target platform of body plasma immersion ion implantation equipment, vacuum degree in vacuum chamber is 5 × 10-3Pa, injection electricity
Pressure is -40KV, injection length 2h, and injection element is silver ion and zinc ion.
Remaining is the same as embodiment 1.
Embodiment 31
PIC method in plasma immersion ion injection is handled：By differential arc oxidation, treated that dental implant ontology is placed on plasma
Ion implanting is carried out on the vacuum chamber target platform of body plasma immersion ion implantation equipment, vacuum degree in vacuum chamber is 8 × 10-3Pa, injection electricity
Pressure is -40KV, injection length 2h, and injection element is silver ion and zinc ion.
Remaining is the same as embodiment 1.
Embodiment 32
PIC method in plasma immersion ion injection is handled：By differential arc oxidation, treated that dental implant ontology is placed on plasma
Ion implanting is carried out on the vacuum chamber target platform of body plasma immersion ion implantation equipment, vacuum degree in vacuum chamber is 6 × 10-3Pa, injection electricity
Pressure is -30KV, injection length 2h, and injection element is silver ion and zinc ion.
Remaining is the same as embodiment 1.
Embodiment 33
PIC method in plasma immersion ion injection is handled：By differential arc oxidation, treated that dental implant ontology is placed on plasma
Ion implanting is carried out on the vacuum chamber target platform of body plasma immersion ion implantation equipment, vacuum degree in vacuum chamber is 6 × 10-3Pa, injection electricity
Pressure is -50KV, injection length 2h, and injection element is silver ion and zinc ion.
Remaining is the same as embodiment 1.
Embodiment 34
PIC method in plasma immersion ion injection is handled：By differential arc oxidation, treated that dental implant ontology is placed on plasma
Ion implanting is carried out on the vacuum chamber target platform of body plasma immersion ion implantation equipment, vacuum degree in vacuum chamber is 6 × 10-3Pa, injection electricity
Pressure is 40KV, injection length 3h, and injection element is silver ion and zinc ion.
Remaining is the same as embodiment 1.
Embodiment 35
PIC method in plasma immersion ion injection is handled：By differential arc oxidation, treated that dental implant ontology is placed on plasma
Ion implanting is carried out on the vacuum chamber target platform of body plasma immersion ion implantation equipment, vacuum degree in vacuum chamber is 6 × 10-3Pa, injection electricity
Pressure is 40KV, injection length 1h, and injection element is silver ion and zinc ion.
Remaining is the same as embodiment 1.
Embodiment 36
PIC method in plasma immersion ion injection is handled：By differential arc oxidation, treated that dental implant ontology is placed on plasma
Ion implanting is carried out on the vacuum chamber target platform of body plasma immersion ion implantation equipment, vacuum degree in vacuum chamber is 5.5 × 10-3Pa, injection
Voltage is -40KV, injection length 2h, and injection element is silver ion and zinc ion.
Remaining is the same as embodiment 1.
Embodiment 37
PIC method in plasma immersion ion injection is handled：By differential arc oxidation, treated that dental implant ontology is placed on plasma
Ion implanting is carried out on the vacuum chamber target platform of body plasma immersion ion implantation equipment, vacuum degree in vacuum chamber is 6.5 × 10-3Pa, injection
Voltage is -40KV, injection length 2h, and injection element is silver ion and zinc ion.
Remaining is the same as embodiment 1.
Embodiment 38
PIC method in plasma immersion ion injection is handled：By differential arc oxidation, treated that dental implant ontology is placed on plasma
Ion implanting is carried out on the vacuum chamber target platform of body plasma immersion ion implantation equipment, vacuum degree in vacuum chamber is 6 × 10-3Pa, injection electricity
Pressure is -35KV, injection length 2h, and injection element is silver ion and zinc ion.
Remaining is the same as embodiment 1.
Embodiment 39
PIC method in plasma immersion ion injection is handled：By differential arc oxidation, treated that dental implant ontology is placed on plasma
Ion implanting is carried out on the vacuum chamber target platform of body plasma immersion ion implantation equipment, vacuum degree in vacuum chamber is 6 × 10-3Pa, injection electricity
Pressure is -45KV, injection length 2h, and injection element is silver ion and zinc ion.
Remaining is the same as embodiment 1.
Embodiment 40
PIC method in plasma immersion ion injection is handled：By differential arc oxidation, treated that dental implant ontology is placed on plasma
Ion implanting is carried out on the vacuum chamber target platform of body plasma immersion ion implantation equipment, vacuum degree in vacuum chamber is 6 × 10-3Pa, injection electricity
Pressure is -40KV, injection length 1.5h, and injection element is silver ion and zinc ion.
Remaining is the same as embodiment 1.
Embodiment 41
PIC method in plasma immersion ion injection is handled：By differential arc oxidation, treated that dental implant ontology is placed on plasma
Ion implanting is carried out on the vacuum chamber target platform of body plasma immersion ion implantation equipment, vacuum degree in vacuum chamber is 6 × 10-3Pa, injection electricity
Pressure is -40KV, injection length 2.5h, and injection element is silver ion and zinc ion.
Remaining is the same as embodiment 1.
Using after the sandblasting of the antibacterial dental implant of the scanning electron microscope Cross Section Method detection institute formation of embodiment 1 to 29 and micro-
The thickness and pore size of superficial film after arc oxidation, 6.0 software tests of stereoscan photograph combination image pro plus
The porosity of planting body film layer, testing result are shown in Fig. 1 and 2 and table 1.Using EDS spectroscopy detections embodiment 1, embodiment 13 to
The element of 41 differential arc oxidation film layer forms and the content of nanometer antibacterial function material.By embodiment treated Dental implantion
The Ag and Zn that body surface face is contained are measured by XPS High Resolution Spectrums.
The antibacterial effect of dental implant prepared by the embodiment of the present invention uses the measurement of fluorescence method bacterial adhesion amount.Specific side
Method is as follows：Dental implant (the embodiment group i.e. in table 2) prepared by various embodiments of the present invention and untreated Dental implantion
Body (control group i.e. in table) is soaked in l × 10 respectively6In CFU/ml bacteria suspensions, dental implant is taken out after 37 DEG C of culture 2h, and
Distilled water flushing is used respectively 3 times, then with the fixation about 0.5 hour of 4 DEG C of 2.5% glutaraldehyde, then dyed with 1% acridine orange room temperature
0.5 hour, fall excess dyestuff with distilled water flushing.Above-mentioned dental implant is respectively placed under 100 times of fluorescence microscope and observes meter
Number, each dental implant sample randomly choose 6 representational regions, and two groups of dental implants are respectively sticked in 20 visuals field of observation
Attached bacteria counts.Testing result is shown in Table 2.
Table 1
Table 2
It can be seen from the above description that the above embodiments of the present invention realize following technique effect：
The sandblasting to dental implant and differential arc oxidation are realized, is finally formd in dental implant surface raw containing Ca, P etc.
Object active element, and containing the film layer of Ag and Zn elements, which not only has porous structure, can improve dental implant life
Object activity, and can be with restraining and sterilizing bacteria.
The application on dental implant ontology by being arranged differential arc oxidation film layer so that the surface holes knot of dental implant ontology
Structure more horn of plenty, wherein there are the crateriform pore structures of many classes, therefore the surface that can have both increased dental implant ontology is thick
Rugosity, and surface porosity factor is substantially increased, the antibacterial work(of the nano-scale injected at this time by PIC method in plasma immersion ion
Energy material can not only be infused in the surface of differential arc oxidation film layer, it is particularly possible to it is injected into the pore structure of differential arc oxidation film layer,
The load capacity of nanometer antibacterial function material is considerably increased, and when bacterium enters micropore, can sterilized in time, and then reach
The purpose of durable antibiotic.
The foregoing is only a preferred embodiment of the present invention, is not intended to restrict the invention, for the skill of this field
For art personnel, the invention may be variously modified and varied.All within the spirits and principles of the present invention, any made by repair
Change, equivalent replacement, improvement etc., should all be included in the protection scope of the present invention.
Claims (12)
1. a kind of antibacterial dental implant, which is characterized in that including：
Dental implant ontology；
Differential arc oxidation film layer is arranged on the surface of the dental implant ontology；And
Nanometer antibacterial function material is supported on the differential arc oxidation film layer.
2. antibacterial dental implant according to claim 1, which is characterized in that the thickness of the differential arc oxidation film layer be 2~
15 μm, preferably 3~10 μm；The aperture of the differential arc oxidation film layer mesoporous is 2~10 μm, preferably 2~5 μm；The differential of the arc
The porosity of oxidation film layer is 5~20%, preferably 8~20%；It is preferred that the active element in the differential arc oxidation film layer includes
Ca and P.
3. antibacterial dental implant according to claim 1, which is characterized in that the nanometer antibacterial function material includes nanometer
Silver, the preferably described nanometer antibacterial function material includes nano silver and Nano-Zinc.
4. antibacterial dental implant according to claim 1, which is characterized in that the dental implant ontology is titanium-base alloy sheet
Body, the titanium-base alloy ontology are selected from pure titanium, Ti-6Al-4V, Ti-6Al-17Nb, Ti-13Nb-13Zr and Ti-5Zr-3Mo-
One kind in 15Nb.
5. a kind of preparation method of antibacterial dental implant, which is characterized in that the preparation method includes：
Step S1 carries out differential arc oxidation, with the growth in situ differential arc oxidation on the dental implant ontology to dental implant ontology
Film layer；
Step S2, to carrying out PIC method in plasma immersion ion injection by the dental implant ontology of the differential arc oxidation, with
Nanometer antibacterial function material is loaded on the differential arc oxidation film layer.
6. preparation method according to claim 5, which is characterized in that the PIC method in plasma immersion ion of the step S2 is noted
Enter the implementation of using plasma plasma immersion ion implantation equipment, and controls the true of the PIC method in plasma immersion ion injection device
The vacuum degree of empty room is 5 × 10-3~8 × 10-3Pa, injecting voltage are -50~-30KV, and injection length is 1~3h, preferably described
The element of step S2 injections is silver ion and/or zinc ion.
7. preparation method according to claim 6, which is characterized in that the vacuum degree is 5.5 × 10-3~6.5 × 10- 3Pa, the injecting voltage are -35~-45KV, and the injection length is 1.5~2.5h.
8. preparation method according to claim 5, which is characterized in that in electrolyte used by the differential arc oxidation, calcium
The concentration of element is denoted as m mol/L, and the concentration of P elements is denoted as n mol/L, as 0.01≤m ＜ 0.2, (0.1m+0.025)≤
N ＜ 0.05；As 0.2≤m≤0.6, when 0.075≤n≤m/0.875, preferably 0.4 ＜ m≤0.6,0.25≤n≤m/0.875；
It is preferred that calcium source is selected from one kind of calcium acetate, calcium chloride, calcium dihydrogen phosphate, calcium glycerophosphate, calcium citrate, calcium lactate and calcium oxide
Or it is several；More preferable phosphorus source is in sodium glycero-phosphate, sodium dihydrogen phosphate, disodium hydrogen phosphate, calgon and polyphosphate sodium
One or more.
9. preparation method according to claim 8, which is characterized in that the electrolyte further includes EDTA-2Na and silicic acid
Sodium adjusts the electrolyte ph between 11~14 preferably by sodium hydroxide or potassium hydroxide.
10. preparation method according to claim 8, which is characterized in that the differential arc oxidation of the step S1 is using power supply
Voltage is 50~500V, and the output pulse frequency of the power supply is 100~1000Hz, and the pulse width of the power supply is 8~500
The peak point current of μ s, the power supply are 0~300A, and oxidization time is 3~30min.
11. preparation method according to claim 5, which is characterized in that the preparation method is gone back before the step S1
Include to the dental implant ontology carry out blasting treatment process, the abrasive material used during the preferably described blasting treatment for
The grain size of SiC or schmigel, the further preferred abrasive material is 50~300 μm；It is preferred that the sandblasting of the process of the blasting treatment
Distance is 10~15cm, and compression pressure is 2~10bar, and injecting time is 5~60s.
12. preparation method according to claim 5, which is characterized in that the dental implant ontology is titanium-base alloy ontology,
The titanium-base alloy ontology is selected from pure titanium, Ti-6Al-4V, Ti-6Al-17Nb, Ti-13Nb-13Zr and Ti-5Zr-3Mo-15Nb
In one kind；It is preferred that the dental implant ontology is obtained by increases material manufacturing technology, the increases material manufacturing technology is molten for electron beam
Melt manufacturing technology and selective laser sintering.
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| CN110180020A (en) * | 2019-05-29 | 2019-08-30 | 中国科学院上海硅酸盐研究所 | A kind of N doping titanium oxide coating and its preparation method and application |
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