CN102921037B - Method for preparing multistage micron structure on titanium implant surface - Google Patents
Method for preparing multistage micron structure on titanium implant surface Download PDFInfo
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- CN102921037B CN102921037B CN201210431965.7A CN201210431965A CN102921037B CN 102921037 B CN102921037 B CN 102921037B CN 201210431965 A CN201210431965 A CN 201210431965A CN 102921037 B CN102921037 B CN 102921037B
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- 229910052719 titanium Inorganic materials 0.000 title claims abstract description 101
- 239000010936 titanium Substances 0.000 title claims abstract description 101
- 239000007943 implant Substances 0.000 title claims abstract description 100
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 title claims abstract description 99
- 238000000034 method Methods 0.000 title claims abstract description 37
- 239000002253 acid Substances 0.000 claims abstract description 48
- 238000005530 etching Methods 0.000 claims abstract description 40
- 238000004140 cleaning Methods 0.000 claims abstract description 21
- 238000010438 heat treatment Methods 0.000 claims abstract description 21
- 239000000243 solution Substances 0.000 claims abstract description 14
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims abstract description 10
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims abstract description 10
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- 238000005498 polishing Methods 0.000 claims abstract description 10
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- 238000005554 pickling Methods 0.000 claims description 36
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 28
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 28
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 28
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 28
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 27
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- 229910021641 deionized water Inorganic materials 0.000 claims description 21
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- 238000005422 blasting Methods 0.000 claims description 13
- 239000004576 sand Substances 0.000 claims description 9
- QGTQTQBVAMFOGO-UHFFFAOYSA-N 1,1,2,2,3,3,4,4,5,5,6,6,7,7,8,8,8-heptadecafluorooctane-1-sulfonic acid;potassium Chemical compound [K].OS(=O)(=O)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)F QGTQTQBVAMFOGO-UHFFFAOYSA-N 0.000 claims description 7
- 244000137852 Petrea volubilis Species 0.000 claims description 7
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 7
- 239000007864 aqueous solution Substances 0.000 claims description 7
- 239000000919 ceramic Substances 0.000 claims description 7
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- 239000000470 constituent Substances 0.000 claims description 2
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- 210000000988 bone and bone Anatomy 0.000 abstract description 7
- 238000005488 sandblasting Methods 0.000 abstract description 7
- 238000003912 environmental pollution Methods 0.000 abstract description 3
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 abstract 2
- 238000001816 cooling Methods 0.000 abstract 1
- 238000007598 dipping method Methods 0.000 abstract 1
- 210000000963 osteoblast Anatomy 0.000 abstract 1
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- 150000001875 compounds Chemical class 0.000 description 1
- 238000002316 cosmetic surgery Methods 0.000 description 1
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- 150000002500 ions Chemical class 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 239000003595 mist Substances 0.000 description 1
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- CCEKAJIANROZEO-UHFFFAOYSA-N sulfluramid Chemical group CCNS(=O)(=O)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)F CCEKAJIANROZEO-UHFFFAOYSA-N 0.000 description 1
- 238000010301 surface-oxidation reaction Methods 0.000 description 1
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Abstract
The invention discloses a method for preparing a multistage micron structure on a titanium implant surface and relates to a titanium implant. The method includes polishing the titanium implant surface, performing oil removing treatment, and cleaning; subjecting the titanium implant which is subjected to the oil treatment and cleaning to acid dipping treatment in a mixed solution containing a nitric acid, a hydrofluoric acid and hydrogen peroxide; subjecting the titanium implant surface to sand blasting treatment; cleaning the titanium implant which is subjected to the sand blasting treatment; subjecting the cleaned titanium implant to acid etching post-treatment in an acid etching solution; and subjecting the titanium implant to heat treatment and cooling the titanium implant to the normal temperature to obtain the titanium implant with the surface in the multistage micron structure. According to the method for preparing the multistage micron structure on the titanium implant surface, the contact area between the titanium implant and bone tissues is increased, osteoblast ingrowth is facilitated, and thereby the forming of bone closure is facilitated; processing devices are easy to obtain, the operation process is simple, the environmental pollution is small, and the industrialization is easy to achieve; and the appearance is abundant, and the hydrophilic performance is excellent.
Description
Technical field
The present invention relates to a kind of titanium implant, especially relate to a kind of method of preparing multistage micron active surface on titanium implant surface.
Background technology
Titanium and alloy thereof are due to its good mechanical property, as high strength, low elastic modulus, elastic modelling quantity and bone approach, can effectively suppress stress shielding, avoid producing local bone resorption, surface has good chemical stability and biocompatibility simultaneously, it is widely used, as artificial bone, artificial joint, nail, tooth titanium implant etc. in fields such as plastic surgery, dentistry.Clinical research shows, and to titanium implant, the short-term load after implant into body and long-term stability have vital effect to surface morphology and composition.At present, business-like product on market at home and abroad, is 1～3 μ m as Nobel Replace adopts differential arc oxidation can obtain diameter, the volcano type porous pattern of height 2～5 μ m, be beneficial to the growth of osseous tissue, but its requirement to equipment is higher, cost of equipment is expensive; The SLA that Straumann releases adopts sandblast acid etching, and equipment cost etc. are all lower, but the surface of its formation depression is more shallow, visible a large amount of sharpened edge after pattern amplifies, it is easily corroded in body fluid environment, cause ion to reveal, after implantation, have potential hazard.From the viewpoint of the actual effect of cost and application etc., how under the relatively simple condition of operating equipment, technique, to prepare structure and enrich, be conducive to the excellence surface that osseous tissue grows into and will have positive meaning.
Chinese patent CN200510062209.1 open a kind of " having the method for bioactivity, porous structure in the preparation of pure-titanium tooth implantation surface ", under employing corundum sandblast 4bar pressure, the method for sandblast and Fluohydric acid., nitric acid and sulphuric acid, hydrochloric acid double acid-etching is constructed the micron order pit that diameter is 10～30 μ m and 0.2 μ m.But the hydrochloric acid that it adopts and the concentration of sulphuric acid are all larger, under higher temperature, must bring a large amount of volatilizations of hydrochloric acid, cause environmental pollution, double acid-etching cost complicated operation simultaneously, cost is higher.Chinese patent CN200910248898.3 open " a kind of method of preparing loose structure on pure-titanium tooth implantation surface ", the method is a kind of method that obtains porous through the sandblast of bulky grain corundum by sulphuric acid, twice double acid-etching of hydrochloric acid, its heating-up temperature is 40～70 ℃, temperature is not high make in the volatilization of hydrochloric acid relatively less, but only can produce because the surface depression that surface forms is hit in sandblast.
Because losing in surperficial pickling solution, metatitanic acid in most of document and patent contains hydrochloric acid, while carrying out acid etching under higher temperature, easily produce a large amount of volatilizations, can produce very large corrosion to the plant and equipment of producing, also the healthy of operator caused damage.Based on multiple aspect, consider simultaneously, if not merely adopt single particle size, adopt the sand grains effects on surface that mixes particle diameter to process, can obtain the more compound pattern of horn of plenty of pattern, when forming sandblast depression, can form on surface darker wormhole, thereby form the special even multistage micron order structure and morphology compared with deep holes that has, significant to the practical application of product to increase considerably the contact area of titanium implant and tissue and to improve the sealed intensity of machinery.Simultaneously by the generation that can reduce sharpened edge in acid corrosion process that adds of other materials.
Summary of the invention
The object of the present invention is to provide a kind of titanium implant surface to prepare the method for multistage micrometer structure.
The present invention includes following steps:
1) by after titanium implant surface polishing, then carry out oil removal treatment, clean;
2) titanium implant by oil removal treatment and after cleaning carries out pickling processes in the mixed solution containing nitric acid, Fluohydric acid., hydrogen peroxide;
3) titanium implant surface is carried out to blasting treatment;
4) titanium implant after blasting treatment is cleaned;
5) titanium implant after cleaning is placed in to the post processing of pickling solution acid etching;
6) by after titanium implant heat treatment, be cooled to room temperature, obtain the titanium implant of surface for multistage micrometer structure.
In step 1), described polishing can adopt sand paper or grinder buffing; Described cleaning can be passed through difference ultrasonic cleaning 10～15min in acetone, ethanol, deionized water successively;
In step 2) in, the aqueous solution that the pickle of described pickling processes can be 10%～20% nitric acid, 2%～5% Fluohydric acid., 1%～3% hydrogen peroxide by mass fraction forms, and the temperature of pickling processes can be 20～30 ℃, and the time of pickling processes can be 30s～2min.
In step 3), described blasting treatment can adopt ceramic sand, and its constituent is ZrO
2, SiO
2and Al
2o
3deng mixture, sandblast particle diameter can be 80～180 orders, and (m), blasting pressure can be 5～8bar to 180～80 μ, and sandblast distance can be 0.5～2cm.
In step 4), the condition of described cleaning can be passed through acetone, ethanol, deionized water ultrasonic cleaning 10～15min respectively successively.
In step 5), the composition of described pickling solution can be sulphuric acid, hydrochloric acid, nitric acid, ethylene glycol, acid fog inhibitor and water, wherein the mass fraction of sulphuric acid is 15%～40%, the mass fraction of hydrochloric acid is 1%～8%, and the mass fraction of nitric acid is 1%～5%, and the mass fraction of ethylene glycol is 0.2%～5%, the content of acid fog inhibitor is 0.02～0.08g/L, all the other are deionized water, and acid etching temperature can be 50～80 ℃, and etching time can be 20～60min; Described acid fog inhibitor can adopt perfluoro octyl sulfonic acid potassium etc.
In step 6), described heat-treating methods can be titanium implant is placed in to Muffle furnace or tube furnace heat treatment, and heat treated temperature can be 400～550 ℃, and the heat treated time can be 2～3h.
Compared with prior art, beneficial effect of the present invention is:
1) adopt and mix the sandblast of particle diameter sand grains and construct a kind of special even multistage micron order pattern compared with deep holes that has at flat surface, appearance structure is horn of plenty more, the diameter of its one-level micron depression is about 10～20 μ m, the diameter of secondary micron hole is about 1～8 μ m, thereby increases considerably the contact area of titanium implant and tissue and improve the sealed intensity of machinery.
2) adopt formation and the generation of acid fog inhibitor acid mist can suppress in a large number acid etching solution-treated titanium implant time, significantly improved production operation environment, and process equipment is easy to get, operating procedure is simple, and environmental pollution is little, is beneficial to and realizes commercial production.
3) than the sandblast acid etching surface of conventional process, it is without sharpened edge, and has the surface of multistage micron order activity, and contact angle reduces, and hydrophilicity is more excellent.
4) pickling solution of the present invention is different from other pickling solutions, by adding other one-tenth, assign to be suppressed at a large amount of acid mists that under higher temperature, the volatilization due to hydrochloric acid forms, thereby significantly improve the environment of production operation, reduce the hydrochloric acid air pollution causing of volatilizing simultaneously, this also will have great importance.And to carrying out surface activation process by high-temperature heating in the multistage micron of gained surface, at surface oxidation, generate the titanium dioxide thin layer of the crystal type of thin layer, its contact angle is significantly reduced, be beneficial to the biomineralization at material surface after implantation, thereby the short-term load and the bone that are more conducive to realize titanium implant merge simultaneously.
Accompanying drawing explanation
Fig. 1 is the surface sweeping electron microscope picture (amplification is 1000) of Nobel Replace titanium implant surface.In Fig. 1, scale is 10 μ m.
Fig. 2 is the surface sweeping electron microscope picture (amplification is 5000) of Nobel Replace titanium implant surface.In Fig. 2, scale is 5 μ m.
Fig. 3 is the surface sweeping electron microscope picture (amplification is 1000) of titanium implant surface after Straumann SLA pickling.In Fig. 3, scale is 10 μ m.
Fig. 4 is the surface sweeping electron microscope picture (amplification is 5000) of titanium implant surface after Straumann SLA pickling.In Fig. 4, scale is 5 μ m.
Fig. 5 is the scanning electron microscope diagram of titanium implant surface (amplification is 1000) after pickling in embodiment 1.In Fig. 5, scale is 10 μ m.
Fig. 6 is the scanning electron microscope diagram of titanium implant surface (amplification is 5000) after pickling in embodiment 1.In Fig. 6, scale is 5 μ m.
Fig. 7 is the scanning electron microscope diagram of titanium implant surface (amplification is 1000) after sandblast in embodiment 1.In Fig. 7, scale is 10 μ m.
Fig. 8 is the scanning electron microscope diagram of titanium implant surface (amplification is 5000) after sandblast in embodiment 1.In Fig. 8, scale is 5 μ m.
Fig. 9 is the scanning electron microscope diagram of titanium implant surface (amplification is 1000) after sandblast acid etching in embodiment 1.In Fig. 9, scale is 10 μ m.
Figure 10 is the scanning electron microscope diagram of titanium implant surface (amplification is 5000) after sandblast acid etching in embodiment 1.In Figure 10, scale is 5 μ m.
Figure 11 is the scanning electron microscope diagram of titanium implant surface (amplification is 1000) after sandblast acid etching heat treatment in embodiment 1.In Figure 11, scale is 10 μ m.
Figure 12 is the scanning electron microscope diagram of titanium implant surface (amplification is 5000) after sandblast acid etching heat treatment in embodiment 1.In Figure 12, scale is 5 μ m.
Figure 13 is the static contact angle microscope figure of titanium implant surface water after pickling in embodiment 1.
Figure 14 is the static contact angle microscope figure of titanium implant surface water after sandblast acid etching in embodiment 1.
Figure 15 is the static contact angle microscope figure of titanium implant surface water after sandblast acid etching heat treatment in embodiment 1.
Figure 16 is titanium implant surface XRD figure after sandblast acid etching heat treatment in embodiment 1.
Figure 17 is under embodiment 1 condition after pickling, after sandblast acid etching, the XPS figure of heat treatment rear surface.In Figure 17, abscissa is Binding Energy, and vertical coordinate is intensity I ntensity; After curve a is heat treatment, after curve b is acid etching, after curve c is pickling.
The specific embodiment
The present invention is further illustrated in connection with accompanying drawing for following examples.
Fig. 1 and 2 provides the surface sweeping electron microscope picture of Nobel Replace titanium implant surface, and Fig. 3 and 4 provides the surface sweeping electron microscope picture of titanium implant surface after Straumann SLA pickling.
Embodiment 1
(1) with sand paper or grinder buffing titanium implant surface, then by difference ultrasonic cleaning 10min in the titanium implant of polishing successively process acetone, ethanol, deionized water;
(2), after cleaning, titanium implant is being 10%HN0 containing mass fraction
3, 2%HF, 1%H
2o
2aqueous solution in, pickling 2min;
(3) after pickling, titanium implant surface is 5bar at pressure, after adopting 80 orders to mix at 1: 1 with 180 object ceramic sand in the sandblasting machine for 0.5cm, carries out blasting treatment;
(4) to titanium implant after sandblast, again successively through difference ultrasonic cleaning 10min in acetone, ethanol, deionized water;
(5) sample after sandblast cleaning is placed in containing mass fraction 15%H
2sO
4, 8%HCl, 1%HNO
3, 0.2% ethylene glycol, 0.2g/L perfluoro octyl sulfonic acid potassium, in all the other solution that are deionized water, acid etching temperature 50 C, etching time is controlled at 60min;
(6), after large water gaging rinses, titanium implant is placed in heat treatment 2h at 400 ℃, tube furnace, cools to room temperature with the furnace.
In embodiment 1 after pickling the scanning electron microscope diagram of titanium implant surface referring to Fig. 5 and 6; In embodiment 1 after sandblast the scanning electron microscope diagram of titanium implant surface referring to Fig. 7 and 8; In embodiment 1 after sandblast acid etching the scanning electron microscope diagram of titanium implant surface referring to Fig. 9 and 10; In embodiment 1 after sandblast acid etching heat treatment the scanning electron microscope diagram of titanium implant surface referring to pickling in Figure 11 and 12 embodiment 1 after the static contact angle microscope figure of titanium implant surface water referring to Figure 13; In embodiment 1 after sandblast acid etching the static contact angle microscope figure of titanium implant surface water referring to Figure 14; In embodiment 1 after sandblast acid etching heat treatment the static contact angle microscope figure of titanium implant surface water referring to Figure 15; In embodiment 1 after sandblast acid etching heat treatment titanium implant surface XRD figure referring to Figure 16; Under embodiment 1 condition after pickling, after sandblast acid etching, the XPS figure of heat treatment rear surface is referring to Figure 17.
(1) with sand paper or grinder buffing titanium implant surface, then by difference ultrasonic cleaning 12min in the titanium implant of polishing successively process acetone, ethanol, deionized water;
(2) after cleaning, titanium implant is placed at containing mass fraction 12%HN0
3, 2%HF, 1%H
2o
2aqueous solution in, pickling 2min;
(3) after pickling, implant surface is 6bar at pressure, and distance is carried out blasting treatment after adopting 90 orders to mix at 2: 1 with 150 object ceramic sand in the inherent sandblasting machine of 0.5cm scope;
(4) to titanium implant after sandblast, again successively through difference ultrasonic cleaning 12min in acetone, ethanol, deionized water;
(5) sample after sandblast cleaning is placed in containing mass fraction 20%H
2sO
4, 6%HCl, 2%HNO
3, 1% ethylene glycol, 0.03g/L perfluoro octyl sulfonic acid potassium, in all the other solution that are deionized water, acid etching temperature 60 C, etching time is controlled at 50min;
(6), after large water gaging rinses, titanium implant is placed in heat treatment 2h at 450 ℃, tube furnace, cools to room temperature with the furnace.
(1) with sand paper or grinder buffing titanium implant surface, then by difference ultrasonic cleaning 15min in the titanium implant of polishing successively process acetone, ethanol, deionized water;
(2), after cleaning, titanium implant is containing mass fraction 15%HN0
3, 3%HF, 2%H
2o
2aqueous solution in, pickling 1min;
(3) after pickling, titanium implant surface is 7bar at pressure, and distance is carried out blasting treatment after adopting 100 orders to mix at 1: 1 with 160 object ceramic sand in the inherent sandblasting machine of 1cm scope;
(4) to titanium implant after sandblast, again successively through difference ultrasonic cleaning 15min in acetone, ethanol, deionized water;
(5) sample after sandblast cleaning is placed in to mass fraction 25%H
2sO
4, 5%HCl, 3%HNO
3, 2% ethylene glycol, 0.05g/L perfluoro octyl sulfonic acid potassium, in all the other solution that are deionized water, acid etching temperature 60 C, etching time is controlled at 40min;
(6), after large water gaging rinses, titanium implant is placed in heat treatment 3h at 500 ℃, tube furnace, cools to room temperature with the furnace.
(1) with sand paper or grinder buffing titanium implant surface, then by difference ultrasonic cleaning 12min in the titanium implant of polishing successively process acetone, ethanol, deionized water;
(2) after cleaning, titanium implant is placed at containing mass fraction 18%HN0
3, 3%HF, 2%H
2o
2aqueous solution in, pickling 1min;
(3) after pickling, titanium implant surface is 7bar at pressure, and distance is carried out blasting treatment after adopting 120 orders to mix at 1: 1 with 150 object ceramic sand in the inherent sandblasting machine of 1cm scope;
(4) to titanium implant after sandblast, again successively through difference ultrasonic cleaning 12min in acetone, ethanol, deionized water;
(5) sample after sandblast cleaning is placed in containing mass fraction 30%H
2sO
4, 3%HCl, 4%HNO
3, 3% ethylene glycol, 0.06g/L perfluoro octyl sulfonic acid potassium, in all the other solution that are deionized water, acid etching temperature 70 C, etching time is controlled at 30min;
(6), after large water gaging rinses, titanium implant is placed in heat treatment 3h at 500 ℃, tube furnace, cools to room temperature with the furnace.
(1) with sand paper or grinder buffing titanium implant surface, then by difference ultrasonic cleaning 12min in the titanium implant of polishing successively process acetone, ethanol, deionized water;
(2) after cleaning, titanium implant is placed at containing mass fraction 20%HN0
3, 5%HF, 3%H
2o
2aqueous solution in, pickling 30s;
(3) after pickling, titanium implant surface is 8bar at pressure, and distance is for adopting 150 object ceramic sand to carry out blasting treatment in the inherent sandblasting machine of 2cm scope;
(4) to titanium implant after sandblast, again successively through difference ultrasonic cleaning 12min in acetone, ethanol, deionized water;
(5) sample after sandblast cleaning is placed in containing mass fraction 40%H
2sO
4, 1%HCl, 5%HNO
3, 5% ethylene glycol, 0.08g/L perfluoro octyl sulfonic acid potassium, in all the other solution that are deionized water, 80 ℃ of acid etching temperature, etching time is controlled at 20min;
(6), after large water gaging rinses, titanium implant is placed in heat treatment 3h at 550 ℃, tube furnace, cools to room temperature with the furnace.
Claims (4)
1. titanium implant surface is prepared a method for multistage micrometer structure, it is characterized in that comprising the following steps:
1) by after titanium implant surface polishing, then carry out oil removal treatment, clean;
2) titanium implant by oil removal treatment and after cleaning carries out pickling processes in the mixed solution containing nitric acid, Fluohydric acid., hydrogen peroxide; The aqueous solution that the pickle of described pickling processes is 10%～20% nitric acid, 2%～5% Fluohydric acid., 1%～3% hydrogen peroxide by mass fraction forms; The temperature of described pickling processes is 20～30 ℃, and the time of pickling processes is 30s～2min;
3) titanium implant surface is carried out to blasting treatment; Described blasting treatment is to adopt ceramic sand, and its constituent is ZrO
2, SiO
2and Al
2o
3mixture; Sandblast particle diameter is 80～180 orders, and blasting pressure is 5～8bar, and sandblast distance is 0.5～2cm;
4) titanium implant after blasting treatment is cleaned;
5) titanium implant after cleaning is placed in to the post processing of pickling solution acid etching; The composition of described pickling solution is sulphuric acid, hydrochloric acid, nitric acid, ethylene glycol, acid fog inhibitor and water, wherein the mass fraction of sulphuric acid is 15%～40%, the mass fraction of hydrochloric acid is 1%～8%, the mass fraction of nitric acid is 1%～5%, the mass fraction of ethylene glycol is 0.2%～5%, the content of acid fog inhibitor is 0.02～0.08g/L, and all the other are deionized water; The temperature of described acid etching is 50～80 ℃, and the time of acid etching is 20～60min; Described acid fog inhibitor adopts perfluoro octyl sulfonic acid potassium;
6) by after titanium implant heat treatment, be cooled to room temperature, obtain the titanium implant of surface for multistage micrometer structure, heat treated temperature is 400～550 ℃, and the heat treated time is 2～3h.
2. a kind of titanium implant surface as claimed in claim 1 is prepared the method for multistage micrometer structure, it is characterized in that in step 1), and described polishing is to adopt sand paper or grinder buffing.
3. a kind of titanium implant surface as claimed in claim 1 is prepared the method for multistage micrometer structure, it is characterized in that in step 1), and described cleaning is successively through difference ultrasonic cleaning 10～15min in acetone, ethanol, deionized water; In step 4), the condition of described cleaning is successively through acetone, ethanol, deionized water ultrasonic cleaning 10～15min respectively.
4. a kind of titanium implant surface as claimed in claim 1 is prepared the method for multistage micrometer structure, it is characterized in that in step 6), and described heat-treating methods is for to be placed in Muffle furnace or tube furnace heat treatment by titanium implant.
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|---|---|---|---|
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| CN103087718B (en) * | 2013-01-16 | 2014-12-31 | 四川大学 | Etching solution for performing wet etching on lanthanum nickelate film and ferroelectric film/lanthanum nickelate composite film and preparation method thereof |
| CN103388173B (en) * | 2013-07-26 | 2016-09-28 | 厦门大学 | Method for constructing micro-nano ordered structure on titanium and titanium alloy surface |
| CN104083801B (en) * | 2014-07-25 | 2017-05-10 | 林野 | Method for providing hydrophily for roughened surface of dental implant |
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