CN103654979A - Dental implant and surface treatment method thereof - Google Patents
Dental implant and surface treatment method thereof Download PDFInfo
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- CN103654979A CN103654979A CN201310591134.0A CN201310591134A CN103654979A CN 103654979 A CN103654979 A CN 103654979A CN 201310591134 A CN201310591134 A CN 201310591134A CN 103654979 A CN103654979 A CN 103654979A
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Abstract
The invention discloses a dental implant and a surface treatment method thereof. The surface treatment method for the dental implant comprises the following steps of dental implant cleaning, sandblasting, surface acid etching, surface nanocrystallization processing, soaking, calcinating, and cleaning and the like, so that the dental implant adopting a micron and nanometer mixed structure and having the visible-light catalytic activity through nitrogen doping is obtained. The dental implant achieves preferable hydrophilia, protein adsorption capacity and good biological activity.
Description
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Technical field
The present invention relates to field of biomedicine technology, be specifically related to a kind of dentistry implant and surface treatment method thereof.
Background technology
Dentistry implant refers to that a class is with in surgical operation implantation jawbone, in order to the fixing medical apparatus and instruments of supporting artificial tooth; Its fixing means can be worn gum, and a part for tooth implant is exposed to outside gingiva as foundation pile; Or be embedded in completely under gingiva, only as supporting dismountable dental case.As required, the variform such as that tooth implant can be made is cylindric, foliaceous and helical form, can be formed or be composited by previous materials by different materials such as metal, pottery, polymer or natural materials.
Dentistry implant surface treatment method mainly contains at present, the methods such as sandblast acid etching, laser treatment, differential arc oxidation, and the surface that these methods are made is all surfaces of micron level.
Chinese patent application CN101919741A discloses a kind of tooth implant and preparation method of nanometer multi-grade micro-surface structure, and its step is as follows: 1), after the depassivation film of titanium dental implant surface, be placed in respectively acetone, and 95% ethanol, deionized water for ultrasonic is cleaned, dry; 2) configuration electrolyte: hydrofluoric acid concentration: 0.1-10mol/L, concentration of hydrochloric acid: 0.3-17mol/L; 3) setting of electrode: anode is titanium tooth pure titanium implant, and negative electrode is platinized platinum; 4) processing parameter: solution temperature 10-50 ℃, processing time 1-10min, electric current density 100-1000mA/cm2; 5) titanium dental implant of step 1) being processed is placed in electrolyte process after, be placed in respectively acetone, 95% ethanol, in deionized water, excusing from death is cleaned, dry; Make test specimen surface have the surface of micron-nanometer micro structure concurrently.The tooth implant obtaining by the method has micron-nanometer multi micro structure concurrently, has solved surface texture and has been combined hypodynamic problem with base; But because implantation body is saved in last clinical use from being fabricated into, conventionally have the spacer segment time, along with the prolongation dental implant surface of holding time is just larger by the chance of hydrocarbon pollution in air, the biologic activity of tooth implant is just lower; Have that research surface is new processes without the implantation body its ratio of bone contact (BIC) polluting can reach more than 90% aging pure titanium implant BIC only less than 60%, and can reach 100% BIC after ultraviolet (UV) irradiates, this is because of UV irradiation TiO
2there is photocatalytic effect, generate the photohole electron pair with strong redox ability, by TiO
2the Hydrocarbon degraded of surface contamination makes it have the BIC higher than the pure titanium implant of new processing, but UV is inconvenient in clinical use, and protection sternly can not injure medical personnel and patient around, also can produce the harmful gass such as ozone.
Summary of the invention
In order to overcome the deficiencies in the prior art, the object of the present invention is to provide a kind of dentistry implant and surface treatment method thereof, obtain and a kind ofly there is surface for micron/nano mixed structure and by nitrogen, adulterate and there is the tooth implant of visible light catalysis activity, make tooth implant obtain better hydrophilic, protein adsorption ability, has better biologic activity.
Another object of the present invention is to provide a kind of dentistry implant, there is surface for micron/nano mixed structure, visible light catalysis activity and biologic activity.
For addressing the above problem, the technical solution adopted in the present invention is as follows:
A surface treatment method for dentistry implant, its concrete steps are as follows:
1) pure-titanium tooth implantation cleans: pure-titanium tooth implantation is passed through to acetone, dehydrated alcohol, deionized water ultrasonic cleaning, natural drying successively;
2) blasting treatment: the tooth implant after step (1) is processed, under 0.4-0.5MPa air pressure, be take the alumina particle blasting treatment of diameter as 100-150 μ m;
3) surperficial acid etching: configure the bisgallic acid solution of hydrochloric acid and sulphuric acid, by step 2) tooth implant after blasting treatment is immersed in completely in bisgallic acid and carries out acid etching, obtains the tooth implant of acid etching;
4) dental implant surface nanorize is processed: 0.5% the Fluohydric acid. of take is electrolyte, and the tooth implant after step 3) acid etching is anode, and platinized platinum is negative electrode, power supply is D.C. regulated power supply, voltage is 10 ~ 20V, and solution temperature is room temperature, tooth implant is placed in to electrolyte Anodic Oxidation and processes;
5) soak: the tooth implant after step 4) is processed is immersed in the ammonia of 1mol/L;
6) calcining: the tooth implant after step 5) is processed is placed in Muffle furnace to be calcined, and disconnected power down makes tooth implant naturally cool to room temperature in stove behind source;
7) clean: the tooth implant after step 6) is processed takes out, and passes through successively subsequently acetone, dehydrated alcohol, each ultrasonic cleaning of deionized water, natural drying.
In such scheme, as a kind of concrete embodiment, step 2) during blasting treatment, described nozzle distance tooth implant 0.5-1.5cm, nozzle evenly sprays 20-40 second perpendicular to tooth implant, makes dental implant surface form uniform one-level hole; Pass through successively subsequently acetone, dehydrated alcohol, deionized water ultrasonic cleaning, natural drying.
In such scheme, as a kind of concrete embodiment, described bisgallic acid solution is with 18%HCl solution and 49%H
2sO
4solution mixes with volume ratio 1:1.
In such scheme, as a kind of concrete embodiment, the acid etching of step 3) is acid etching 20-40 minute at 50-70 ℃, take out subsequently the tooth implant of acid etching, with deionized water, rinse well immediately, pass through successively subsequently acetone, dehydrated alcohol, deionized water ultrasonic cleaning, natural drying.
In such scheme, as a kind of concrete embodiment, step 4) oxidation processes was taken out tooth implant after 20 minutes, rinsed well immediately with deionized water, passed through successively subsequently acetone, dehydrated alcohol, deionized water ultrasonic cleaning, natural drying.
In such scheme, as a kind of concrete embodiment, in step 6), the temperature of Muffle furnace is 400-500 ℃.
In such scheme, as a kind of concrete embodiment, wherein, successively through the time of acetone, dehydrated alcohol, the deionized water ultrasonic cleaning 10-20 minute that respectively does for oneself.
A dentistry implant, is that the surface of pure-titanium tooth implantation is processed through above-mentioned surface treatment method, and its surface is that the one-level hole of 10-30 micron and nanotube that diameter is 30-100 nanometer form by diameter.
Compared to existing technology, beneficial effect of the present invention is:
1. surface treatment method of the present invention is by obtaining the structure of nanotube on micron order surface by anodizing on the basis on sandblast aciding acquisition micron order surface, and can realize the control to nanotube diameter by controlling anodised voltage, at dental implant surface, not only retain micrometer structure but also there is nanostructured like this;
2. semiconductor light-catalyst is N-shaped semi-conducting material (the current TiO of thinking mostly
2use the most extensive) all there is the special band structure that is different from metal or megohmite insulant, at valence band (ValenceBand, VB) and between conduction band (ConductionBand, CB), have a forbidden band (ForbiddenBand, BandGap); Because semi-conductive light absorption threshold value and band gap have the relation of K=1240/Eg (eV), therefore the absorbing wavelength threshold value of conventional wide band gap semiconducter is mostly at ultraviolet region, when photon energy absorbs the rayed quasiconductor of threshold value higher than quasiconductor, semi-conductive valence band electronics generation band-to-band transition, from valence band, transit to conduction band, thereby produce light induced electron (e-) and hole (h+); The dissolved oxygen trapped electron that is now adsorbed on nano grain surface forms superoxide anion, and hole is oxidized to hydroxyl free radical by the hydroxide ion and the water that are adsorbed on catalyst surface, and superoxide anion and hydroxyl free radical have very strong oxidisability, can be by most oxidation operations to end product CO
2and H
2o, even also can thoroughly decompose some inorganic matters.Surface treatment method of the present invention is soaked in pure titanium implant in ammonia, then is placed on calcining in Muffle furnace, and nitrogen is doped to TiO
2in, at dental implant surface, form the N-TiO with visible light catalysis activity
2, reaching and only need radiation of visible light can excite photohole-electron pair, the Hydrocarbon of the surface contamination of degrading, makes tooth implant obtain better hydrophilic, and protein adsorption ability, has better biologic activity.
Below in conjunction with the drawings and specific embodiments, the present invention is described in further detail.
Accompanying drawing explanation
Fig. 1 is that dentistry implant of the present invention amplifies the electron micrograph of 1000 times;
Fig. 2 is that dentistry implant of the present invention amplifies the electron micrograph of 10000 times;
Fig. 3 is that dentistry implant of the present invention amplifies the electron micrograph of 100000 times.
The specific embodiment
Embodiment 1
A dentistry implant, process by the following method on its surface:
1) pure-titanium tooth implantation cleans: pure-titanium tooth implantation is passed through to acetone, dehydrated alcohol, each ultrasonic cleaning of deionized water 15 minutes successively, natural drying;
2) blasting treatment: the tooth implant after step 1) is processed be take the alumina particle of diameter as 120 μ m under 0.45MPa air pressure, nozzle distance pure titanium implant 1cm, nozzle evenly sprays 30 seconds perpendicular to tooth implant, makes dental implant surface have uniform one-level hole; Pass through successively subsequently acetone, dehydrated alcohol, each ultrasonic cleaning of deionized water 15 minutes, natural drying;
3) surperficial acid etching: configure 18%HCL, 49%H2SO4 with deionized water the hydrochloric acid sulphuric acid configuring is mixed with volume ratio 1:1, by step 2) tooth implant after processing is immersed in bisgallic acid completely, at 60 ℃, acid etching is 30 minutes, take out subsequently the tooth implant after acid etching, use immediately a large amount of deionized water rinsings, pass through successively subsequently acetone, dehydrated alcohol, each ultrasonic cleaning of deionized water 15 minutes, natural drying;
4) Surface Nanocrystalline: with the Fluohydric acid. of deionized water configuration 0.5%; The tooth implant of take after acid etching is anode, and platinized platinum is negative electrode, and power supply is D.C. regulated power supply, and voltage is 10V, and solution temperature is room temperature, tooth implant is placed in to electrolyte Anodic Oxidation and processes 20 minutes; Take out subsequently tooth implant, use immediately a large amount of deionized water rinsings, pass through successively subsequently acetone, dehydrated alcohol, each ultrasonic cleaning of deionized water 15 minutes, natural drying;
5) with the ammonia of deionized water configuration 1mol/L, the tooth implant after step 4) is processed soaks 24 hours in the ammonia of 1mol/L;
6) tooth implant after step 5) is processed is placed in Muffle furnace 450 ℃ of calcinings 2 hours, and disconnected power down source makes tooth implant in stove, naturally cool to room temperature subsequently;
7) tooth implant after step 6) is processed takes out, and passes through successively subsequently acetone, dehydrated alcohol, each ultrasonic cleaning of deionized water 15 minutes, natural drying.
It is the nanotube of 30nm left and right that the surface of the tooth implant finally obtaining forms one-level hole and the diameter that diameter is 10 microns of left and right.
Embodiment 2
A dentistry implant, process by the following method on its surface:
1) pure-titanium tooth implantation cleans: pure-titanium tooth implantation is passed through to acetone, dehydrated alcohol, each ultrasonic cleaning of deionized water 10 minutes successively, natural drying;
2) blasting treatment: the tooth implant after step 1) is processed be take the alumina particle of diameter as 100 μ m under 0.45MPa air pressure, nozzle distance tooth implant 0.5cm, nozzle evenly sprays 20 seconds perpendicular to tooth implant, makes dental implant surface have uniform one-level hole; Pass through successively subsequently acetone, dehydrated alcohol, each ultrasonic cleaning of deionized water 10 minutes, natural drying;
3) pure titanium implant surface acid etching: configure 18%HCl, 49%H with deionized water
2sO
4the hydrochloric acid sulphuric acid configuring is mixed with volume ratio 1:1, by step 2) tooth implant after processing is immersed in bisgallic acid completely, at 40 ℃, acid etching is 40 minutes, take out subsequently the tooth implant after acid etching, use immediately a large amount of deionized water rinsings, pass through successively subsequently acetone, dehydrated alcohol, each ultrasonic cleaning of deionized water 10 minutes, natural drying;
4) Surface Nanocrystalline: with the Fluohydric acid. of deionized water configuration 0.5%; The tooth implant of take after acid etching is anode, and platinized platinum is negative electrode, and power supply is D.C. regulated power supply, and voltage is 15V, and solution temperature is room temperature, tooth implant is placed in to electrolyte Anodic Oxidation and processes 20 minutes; Take out subsequently tooth implant, use immediately a large amount of deionized water rinsings, pass through successively subsequently acetone, dehydrated alcohol, each ultrasonic cleaning of deionized water 15 minutes, natural drying;
5) with the ammonia of deionized water configuration 1mol/L, the tooth implant after step 4) is processed soaks 20 hours in the ammonia of 1mol/L;
6) tooth implant after step 5) is processed is placed in Muffle furnace 400 ℃ of calcinings 4 hours, and disconnected power down source makes tooth implant in stove, naturally cool to room temperature subsequently;
7) tooth implant after step 6) is processed takes out, and passes through successively subsequently acetone, dehydrated alcohol, each ultrasonic cleaning of deionized water 10 minutes, natural drying.
It is the nanotube of 50nm left and right that the surface of the tooth implant finally obtaining forms one-level hole and the diameter that diameter is 20 microns of left and right.
Embodiment 3
A dentistry implant, process by the following method on its surface:
1) pure-titanium tooth implantation cleans: pure-titanium tooth implantation is passed through to acetone, dehydrated alcohol, each ultrasonic cleaning of deionized water 20 minutes successively, natural drying;
2) blasting treatment: the tooth implant after step 1) is processed be take the alumina particle of diameter as 150 μ m under 0.45MPa air pressure, nozzle distance tooth implant 1.5cm, nozzle evenly sprays 40 seconds perpendicular to tooth implant, makes dental implant surface have uniform one-level hole; Pass through successively subsequently acetone, dehydrated alcohol, each ultrasonic cleaning of deionized water 20 minutes, natural drying;
3) surperficial acid etching: configure 18%HCL, 49%H2SO4 with deionized water the hydrochloric acid sulphuric acid configuring is mixed with volume ratio 1:1, by step 2) tooth implant after processing is immersed in bisgallic acid completely, at 70 ℃, acid etching is 20 minutes, take out subsequently the tooth implant after acid etching, use immediately a large amount of deionized water rinsings, pass through successively subsequently acetone, dehydrated alcohol, each ultrasonic cleaning of deionized water 20 minutes, natural drying;
4) dental implant surface nanorize is processed: with the Fluohydric acid. of deionized water configuration 0.5%; The tooth implant of take after acid etching is anode, and platinized platinum is negative electrode, and power supply is D.C. regulated power supply, and voltage is 20V, and solution temperature is room temperature, tooth implant is placed in to electrolyte Anodic Oxidation and processes 40 minutes; Take out subsequently tooth implant, use immediately a large amount of deionized water rinsings, pass through successively subsequently acetone, dehydrated alcohol, each ultrasonic cleaning of deionized water 20 minutes, natural drying;
5) with the ammonia of deionized water configuration 1mol/L, the tooth implant after step 4) is processed soaks 28 hours in the ammonia of 1mol/L;
6) tooth implant after step 5) is processed is placed in Muffle furnace 500 ℃ of calcinings 2 hours, and disconnected power down source makes tooth implant in stove, naturally cool to room temperature subsequently;
7) tooth implant after step 6) is processed takes out, and passes through successively subsequently acetone, dehydrated alcohol, each ultrasonic cleaning of deionized water 20 minutes, natural drying.
It is the nanotube of 80nm left and right that the surface of the tooth implant finally obtaining forms one-level hole and the diameter that diameter is 30 microns of left and right.
Above-mentioned embodiment is only the preferred embodiment of the present invention; can not limit the scope of protection of the invention with this, the variation of any unsubstantiality that those skilled in the art does on basis of the present invention and replacement all belong to the present invention's scope required for protection.
Claims (8)
1. a surface treatment method for dentistry implant, is characterized in that its concrete steps are as follows:
1) pure-titanium tooth implantation cleans: pure-titanium tooth implantation is passed through to acetone, dehydrated alcohol, deionized water ultrasonic cleaning, natural drying successively;
2) blasting treatment: the tooth implant after step 1) is processed, under 0.4-0.5MPa air pressure, be take the alumina particle blasting treatment of diameter as 100-150 μ m;
3) surperficial acid etching: configure the bisgallic acid solution of hydrochloric acid and sulphuric acid, by step 2) tooth implant after blasting treatment is immersed in completely in bisgallic acid and carries out acid etching, obtains the tooth implant of acid etching;
4) Surface Nanocrystalline: 0.5% the Fluohydric acid. of take is electrolyte, and the tooth implant after step 3) acid etching is anode, and platinized platinum is negative electrode, power supply is D.C. regulated power supply, voltage is 10 ~ 20V, and solution temperature is room temperature, tooth implant is placed in to electrolyte Anodic Oxidation and processes;
5) soak: the tooth implant after step 4) is processed is immersed in the ammonia of 1mol/L;
6) calcining: the tooth implant after step 5) is processed is placed in Muffle furnace to be calcined, and disconnected power down makes tooth implant naturally cool to room temperature in stove behind source;
7) clean: the tooth implant after step 6) is processed takes out, and passes through successively subsequently acetone, dehydrated alcohol, each ultrasonic cleaning of deionized water, natural drying.
2. surface treatment method according to claim 1, it is characterized in that: step 2) during blasting treatment, described nozzle distance tooth implant 0.5-1.5cm, nozzle evenly sprays 20-40 second perpendicular to tooth implant, makes dental implant surface form uniform one-level hole; Pass through successively subsequently acetone, dehydrated alcohol, deionized water ultrasonic cleaning, natural drying.
3. surface treatment method according to claim 1, is characterized in that: described bisgallic acid solution is with 18%HCl solution and 49%H
2sO
4solution mixes with volume ratio 1:1.
4. surface treatment method according to claim 1, it is characterized in that: the acid etching of step 3) is acid etching 20-40 minute at 50-70 ℃, take out subsequently the tooth implant of acid etching, with deionized water, rinse well immediately, pass through successively subsequently acetone, dehydrated alcohol, deionized water ultrasonic cleaning, natural drying.
5. surface treatment method according to claim 1, is characterized in that: step 4) oxidation processes was taken out tooth implant after 20 minutes, rinses well immediately with deionized water, passes through successively subsequently acetone, dehydrated alcohol, deionized water ultrasonic cleaning, natural drying.
6. surface treatment method according to claim 1, is characterized in that: in step 6), the temperature of Muffle furnace is 400-500 ℃.
7. according to the surface treatment method described in claim 1-6 any one, it is characterized in that: wherein, successively through the time of acetone, dehydrated alcohol, the deionized water ultrasonic cleaning 10-20 minute that respectively does for oneself.
8. a dentistry implant, is characterized in that: be that the surface of pure-titanium tooth implantation is processed through surface treatment method claimed in claim 1, its surface is that the one-level hole of 10-30 micron and nanotube that diameter is 30-100 nanometer form by diameter.
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