CN105030353A - Preparation method of dental implant of multistage nano morphologic structure - Google Patents
Preparation method of dental implant of multistage nano morphologic structure Download PDFInfo
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- CN105030353A CN105030353A CN201510404988.2A CN201510404988A CN105030353A CN 105030353 A CN105030353 A CN 105030353A CN 201510404988 A CN201510404988 A CN 201510404988A CN 105030353 A CN105030353 A CN 105030353A
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Abstract
The invention relates to a preparation method of a dental implant of a multistage nano morphologic structure. The preparation method includes: at 24 to 90 DEG C, submerging a titanium-based implant with a titanate nanotube array on the surface into deionized water for the purpose of growth and cultivation so as to obtain the titanium-based implant with the multistage nano morphologic structure. An anodic oxide coating of nanotube morphology is prepared on the outer surface of an implant base by means of an anodizing process, the nanotube morphology is a tubular structure having a nano-level pore size; by means of submerging the implant into the deionized water, the multistage nano coating having mass nano needle structures attached to the surface is prepared based on the nanotubes; the coating rarely drops due to external forces. The implant of the nano-nano multi-stage nanostructure has the advantages that peripheral biological activity of the implant can be greatly improved and the implant can combine better with peripheral bone.
Description
Technical field
The present invention relates to dentistry implant, be specifically related to the preparation method of multi-stage nano appearance structure dentistry implant.
Background technology
Dentistry planting technology has become one of important restorative procedure of defect of dentition or disappearance, but due to the biological activity of implantation body still undesirable, there is the problems such as knitting is bad at Osseointegrated implants interface.Therefore, the coating being prepared by implant surface to high bioactivity for prolongation tool significance in its in service life.
Human body natural's tissue is assembled by nanoscale building blocks, therefore should have better biological activity from bionic angle nanostructured.Titanium dioxide (TiO
2) nanotube (NT) preparation technology simple and also it prepare by electrochemical treatments, be applicable to being applied to complex-shaped implant surface.The anodic oxidation nano-tube array coating of prior art report has been widely used in the surface modification of implantation body.But the environment in organism is very complicated, the structure dimension in osseous tissue from a few nanometer to hundreds of nanoscale building blocks not etc., simple TiO
2-NT structure can not simulate bioactive demand in body.
Summary of the invention
For defect or the deficiency of prior art, the object of the present invention is to provide a kind of preparation method of dentistry implant of multi-stage nano appearance structure.
For this reason, the preparation method of the dentistry implant of multi-stage nano appearance structure provided by the invention comprises:
Under 24 DEG C of-90 DEG C of conditions, be that the titanio implantation body of Nano tube array of titanium dioxide is immersed in grown cultures in deionized water by surface, prepare the titanio implantation body of multi-stage nano appearance structure.
Described cultivation duration is 3h-3d.
The titanio implantation body of described multi-stage nano appearance structure is that Titanium base surface-borne has Nano tube array of titanium dioxide, and Nano tube array of titanium dioxide generates many needling structures.
Described titanio implantation body and water with magnitude relation be: the water consumption of long 10mm × wide 10mm × thick 1mm titanium sheet is 0.3-1ml.
Dentistry implant of the present invention, adopt anode oxidation process to have the anodized coating of nanotube pattern in implantation body's outer surface of matrix preparation, nanotopography is tubular structure, and aperture is nanoscale; Adopt the technique preparation surface attachment based on nanotube being immersed in deionized water to have the multi-stage nano coating of a large amount of nanometer needling structure, this coating can not come off easily because of External Force Acting.
The implantation body of nano-nano multi-level nano-structure prepared by the present invention, can increase substantially bone regeneration around implant biologic activity, can be combined with surrounding bone better.
Accompanying drawing explanation
Below in conjunction with the drawings and specific embodiments, the present invention is described in further detail.
Fig. 1 is scanning electron microscope (SEM) the photo figure of dentistry implant anodizing morphology, and wherein (a) is the anodizing morphology figure before not soaking; B multi-stage nano coating morphology figure that () is embodiment 2; C multi-stage nano coating morphology figure that () is embodiment 4; D multi-stage nano coating morphology figure that () is embodiment 1; E () is the schematic diagram of nanotube composite Nano acupuncture multi-stage nano pattern implantation body preparation process.
Fig. 2 is X-ray diffraction analysis (XRD) figure before and after the dentistry implant anodizing morphology of embodiment 4 soaks.
Fig. 3 is scanning electron microscope (SEM) the photo figure of nanotube composite Nano pin time thorn multi-stage nano pattern dentistry implant cultured cell pattern after 1 day;
Detailed description of the invention
Surface of the present invention is that the titanio implantation body of Nano tube array of titanium dioxide adopts conventional method preparation.
Inventor is at implant surface TiO
2on-NT architecture basics.Defined the multi-level nano-structure of nanoneedle time composite nano tube array by the mode of water environment submergence, from bionics angle, it can simulate the structure of different Nano grade better, has good application prospect and important clinical meaning.
Below the specific embodiment that inventor provides, to be further explained explanation to technical scheme of the present invention.
Embodiment 1:
1) select pure titanium to be processed into dentistry implant matrix, after the polishing of dentistry implant matrix surface, use acetone, dehydrated alcohol and deionized water ultrasonic cleaning successively each 5 minutes, dry up stand-by;
2) anode oxidation process electrolyte is configured: ethylene glycol is solvent, and solute is the NH of 0.5% mass fraction
4f, the CH of 5% volume fraction
3oH, and 5% volume fraction deionized water;
3) anode oxidation process is adopted to prepare Nano tube array of titanium dioxide coating at implantation body's outer surface of matrix: graphite carbon rod is negative electrode, dentistry implant matrix is as anode, put into step 2) electrolyte that configures, concrete technology parameter is: supply frequency 50Hz ± 2Hz, voltage is 40V, processing time 1h, reaction temperature is room temperature;
4) after prepared by implantation body's matrix surface Nano tube array of titanium dioxide coating, circulating water cleaning 30s;
5) the dentistry implant matrix of anodic oxidation is immersed in deionized water, be placed in 24 porocyte culture plates (the corresponding 0.3ml deionized water of 10 × 10 × 1mm surface area pure titanium implant), the 24 porocyte culture plates being loaded with implantation body are placed in constant-temperature incubation case, wherein, temperature is 90 DEG C, and soak time is 3h; Last dry standing under room temperature, leave standstill after taking out dentistry implant, obtain the dentistry implant of multi-stage nano pattern coating.
Embodiment 2:
1) select pure titanium to be processed into dentistry implant matrix, after the polishing of dentistry implant matrix surface, use acetone, dehydrated alcohol and deionized water ultrasonic cleaning successively each 5 minutes, dry up stand-by;
2) anode oxidation process electrolyte is configured: ethylene glycol is solvent, and solute is the NH of 0.5% mass fraction
4f, the CH of 5% volume fraction
3oH, and 5% volume fraction deionized water;
3) anode oxidation process is adopted to prepare Nano tube array of titanium dioxide coating at implantation body's outer surface of matrix: graphite carbon rod is negative electrode, dentistry implant matrix is as anode, put into step 2) electrolyte that configures, concrete technology parameter is: supply frequency 50Hz ± 2Hz, voltage is 40V, processing time 1h, reaction temperature is room temperature;
4) after prepared by implantation body's matrix surface Nano tube array of titanium dioxide coating, circulating water cleaning 30s;
5) the dentistry implant matrix of anodic oxidation is immersed in deionized water, be placed in 24 porocyte culture plates (the corresponding 0.5ml deionized water of 10 × 10 × 1mm surface area pure titanium implant), the 24 porocyte culture plates being loaded with implantation body are placed in constant temperature culture incubator, wherein, temperature is 24 DEG C, and soak time is 3d; Last dry standing under room temperature, leave standstill after taking out dentistry implant, obtain the dentistry implant of multi-stage nano pattern coating.
Embodiment 3:
1) select pure titanium to be processed into dentistry implant matrix, after the polishing of dentistry implant matrix surface, use acetone, dehydrated alcohol and deionized water ultrasonic cleaning successively each 5 minutes, dry up stand-by;
2) anode oxidation process electrolyte is configured: ethylene glycol is solvent, and solute is the NH of 0.5% mass fraction
4f, the CH of 5% volume fraction
3oH, and 5% volume fraction deionized water;
3) anode oxidation process is adopted to prepare Nano tube array of titanium dioxide coating at implantation body's outer surface of matrix: graphite carbon rod is negative electrode, dentistry implant matrix is as anode, put into step 2) electrolyte that configures, concrete technology parameter is: supply frequency 50Hz ± 2Hz, voltage is 40V, processing time 1h, reaction temperature is room temperature;
4) after prepared by implantation body's matrix surface Nano tube array of titanium dioxide coating, circulating water cleaning 30s;
5) the dentistry implant matrix of anodic oxidation is immersed in deionized water, be placed in 24 porocyte culture plates (the corresponding 0.5ml deionized water of 10 × 10 × 1mm surface area pure titanium implant), the 24 porocyte culture plates being loaded with implantation body are placed in constant temperature culture incubator, wherein, temperature is 57 DEG C, and soak time is 12h; Last dry standing under room temperature, leave standstill after taking out dentistry implant, obtain the dentistry implant of multi-stage nano pattern coating.
Embodiment 4:
1) select pure titanium to be processed into dentistry implant matrix, after the polishing of dentistry implant matrix surface, use acetone, dehydrated alcohol and deionized water ultrasonic cleaning successively each 5 minutes, dry up stand-by;
2) anode oxidation process electrolyte is configured: ethylene glycol is solvent, and solute is the NH of 0.5% mass fraction
4f, the CH of 5% volume fraction
3oH, and 5% volume fraction deionized water;
3) anode oxidation process is adopted to prepare Nano tube array of titanium dioxide coating at implantation body's outer surface of matrix: graphite carbon rod is negative electrode, dentistry implant matrix is as anode, put into step 2) electrolyte that configures, concrete technology parameter is: supply frequency 50Hz ± 2Hz, voltage is 40V, processing time 1h, reaction temperature is room temperature;
4) after prepared by implantation body's matrix surface Nano tube array of titanium dioxide coating, circulating water cleaning 30s;
5) the dentistry implant matrix of anodic oxidation is immersed in deionized water, be placed in 24 porocyte culture plates (the corresponding 1.0ml deionized water of 10 × 10 × 1mm surface area pure titanium implant), the 24 porocyte culture plates being loaded with implantation body are placed in constant temperature culture incubator, wherein, temperature is 37 DEG C, and soak time is 1d; Last dry standing under room temperature, leave standstill after taking out dentistry implant, obtain the dentistry implant of multi-stage nano pattern coating.
Select example 4, the dentistry implant of multi-stage nano pattern coating be placed in 24 porocyte culture plates, get 1 week P of Rats 1 generation mesenchymal stem cells MSCs (BMSCs) with 2 × 10
4the density in/ml, 1ml/ hole is inoculated in surface of test piece.
The dentistry implant of the nanotube composite Nano pin time multi-level nano-structure prepared with embodiment 4, and in conjunction with relevant drawings, the present invention is further described.
With reference to Fig. 1, for surface sweeping Electronic Speculum (SEM) photo of front and back pattern before and after implantation body's matrix anode oxidized surface submergence, microscopic appearance in comparison diagram 1 (a) before submergence, visible in deionized water after submergence certain hour, nanostructured surface forms the large stylet spline structure of a large amount of 8-15nm.
Fig. 2 is that implantation body's matrix anode oxidized surface is immersed in X-ray diffractogram before and after deionized water (XRD), and after as can be seen from the figure soaking, the inner nanometer needling structure of anodised implantation body produces the change along with crystalline phase.
Fig. 3 is that the multi-stage nano coating implant surface of embodiment 4 has cultivated the scanning electron microscopic picture of mescenchymal stem cell after 1 day, visible cell can normally in material surface field planting, sprawl, cell stretches out a large amount of pseudopodium in the gap of multi-stage nano coating, illustrates that multi-stage nano coating implantation body contributes to cell field planting and stretching, extension.
Other embodiments prepare dentistry implant, have similar results.Namely deionized water soaks the multi-stage nano tubular construction that anodised nanostructured defines nanotube composite Nano thorn, and this structure has facilitation effect for cell field planting and stretching, extension.
Claims (4)
1. the preparation method of a multi-stage nano appearance structure dentistry implant, it is characterized in that, preparation method comprises: under 24 DEG C of-90 DEG C of conditions, be that the titanio implantation body of Nano tube array of titanium dioxide is immersed in grown cultures in deionized water by surface, prepare the titanio implantation body of multi-stage nano appearance structure.
2. the preparation method of the dentistry implant of multi-stage nano appearance structure according to claim 1, is characterized in that, described cultivation duration is 3h-3d.
3. the preparation method of the dentistry implant of multi-stage nano appearance structure according to claim 1, it is characterized in that, the titanio implantation body of described multi-stage nano appearance structure is that Titanium base surface-borne has Nano tube array of titanium dioxide, and Nano tube array of titanium dioxide generates many needling structures.
4. the preparation method of the dentistry implant of multi-stage nano appearance structure according to claim 1, is characterized in that, described titanio implantation body and water with magnitude relation be: the water consumption of long 10mm × wide 10mm × thick 1mm titanium sheet is 0.3-1ml.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106618765A (en) * | 2016-12-23 | 2017-05-10 | 大连三生科技发展有限公司 | Antibacterial peptide layer for dental implants |
| CN107233619A (en) * | 2017-07-14 | 2017-10-10 | 中国人民解放军第四军医大学 | A kind of Porous titanium bone implant material of functionalization and preparation method thereof |
| CN107551316A (en) * | 2017-09-11 | 2018-01-09 | 佘雨辰 | Imitation biochemistry mixes the preparation method of chlorine nanotube boundling pattern layer dentistry implant |
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| CN102560597A (en) * | 2012-01-05 | 2012-07-11 | 哈尔滨工业大学 | Method for preparing high bioactivity titanium dioxide coating containing nano-crystalline grains |
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Cited By (3)
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| CN106618765A (en) * | 2016-12-23 | 2017-05-10 | 大连三生科技发展有限公司 | Antibacterial peptide layer for dental implants |
| CN107233619A (en) * | 2017-07-14 | 2017-10-10 | 中国人民解放军第四军医大学 | A kind of Porous titanium bone implant material of functionalization and preparation method thereof |
| CN107551316A (en) * | 2017-09-11 | 2018-01-09 | 佘雨辰 | Imitation biochemistry mixes the preparation method of chlorine nanotube boundling pattern layer dentistry implant |
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Application publication date: 20151111 |