CN104645413A - Dental implant and preparation method thereof - Google Patents
Dental implant and preparation method thereof Download PDFInfo
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- CN104645413A CN104645413A CN201510016985.1A CN201510016985A CN104645413A CN 104645413 A CN104645413 A CN 104645413A CN 201510016985 A CN201510016985 A CN 201510016985A CN 104645413 A CN104645413 A CN 104645413A
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Abstract
The invention relates to a dental implant and preparation method thereof. The related dental implant is provided with an anode oxidizing coating with nanotopography, and a cobalt element efficiently promoting blood vessel differentiation is loaded on a nano tube coating; the related method comprises the following steps of: immersing a dental implant base body of which the external surface is a titanium dioxide nano tube array coating, into a cobalt acetate-containing solution; under appropriate reaction conditions, loading the cobalt element on the nano tube coating, thus obtaining the dental implant loaded with cobalt element. According to the invention, a cobalt-loaded mixture is loaded on the anode oxidizing coating through a hydrothermal crystallization process, hydrothermal crystals of the cobalt-loaded mixture can be evenly distributed inside or outside the pores of the anode oxidizing coating, cannot fall off easily under the action of an external force, and also cannot change nanotopography of the anode oxidizing coating too much.
Description
Technical field
The present invention relates to dentistry implant material, particularly a kind of dentistry implant being loaded with cobalt element and preparation method thereof.
Background technology
Along with planting technology development, dentistry implant has been widely used in the reparation of clinical defect of dentition and disappearance patient.But titanium or titanium alloy in implantable bone after, the bad synosteosis of bone regeneration around implant may be there is, finally cause the failure that implantation body implants.The inevitable destruction simultaneously causing osseous tissue in the process of implant implantable bone tissue, this destruction comprises the successional destruction of bone, hemorrhage, the fracture being interpreted as a kind of artificial manufacture can be similar to, the osseous tissue healing that " fracture " is occurred together afterwards, the formation of defect area area of new bone will directly affect implantation body and osseointegration intensity, this process is subject to the impact of many factors, comprise the pattern of osteoblastic activity, implantation body, blood supply etc.Wherein blood supply has very important impact for the sclerotin healing of bone regeneration around implant, bone remodeling, and the good blood supply of bone regeneration around implant both can supply oxygen, various nutrient substance to damage field, the metabolic waste of tissue can also be got rid of in time simultaneously.So we consider to improve implantation body be implanted to power from promotion skeletonization with promote into blood vessel two aspect and start with.Now, in order to promote local skeletonization, existing multiple implant surface pattern occurs and is applied to clinical, mainly adopts the technology such as anodic oxidation, differential arc oxidation, the spraying of titanium slurry or sandblasting acid etching to improve implant surface pattern.Anodic oxidation is as the implant surface treatment technology of wherein a kind of comparative maturity in wide clinical application, and its implant surface has nano tubular structure, can improve synosteosis speed.
In order to improve into vessel patency, having been reported now the scientific research report mainly facilitating the blood vessel differentiation factor to be loaded into implant surface, mainly containing the vascular endothelial cell factor (VEGF), oxygen deficient induction factor 1 (HIF-1 α) etc.But after said method exists cytokine transformation in various degree, activity reduces, the release of cytokines time is shorter, can not promote into the problems such as blood vessel more lastingly.Its a kind of loading method is loaded in poly-dopamine coating by VEGF (vascular endothelial cell growth factor), and be wrapped in pure titanium surface.Another kind method, is immersed in implantation body's matrix in biotic factor VEGF exactly.VEGF in said method is active cannot be ensured after transformation; Above-mentioned steps is loaded down with trivial details in addition, first needs to adopt the more unstable coating etc. of multi-step preparation, then could mix with the albumen such as VEGF and load afterwards; Above-mentioned loading method can not promote titanium surface osteogenetic process simultaneously in addition, does not consider that other somatomedin are for Osseointegrated implants and the facilitation becoming blood vessel simultaneously.Cobalt element has been widely studied the generation of induction ischaemia environment, then promotes HIF-1 α, then produces the change of a series of adaptation anaerobic environment, comprising the generation promoting local environment new vessels.
Summary of the invention
One object of the present invention is to provide a kind of dentistry implant, this dentistry implant is the anodized coating with nanotopography, nanotube coatings is loaded with efficiently facilitates blood vessel differentiation material-cobalt element, cobalt element has been proved to be can induce local cells to secrete HIF-1 α, thus further inducing cell is to the adaptation of anaerobic environment, comprising the generation promoting local new vessels.Promote while the present invention can improve synosteosis speed more rapidly that local becomes vascular process, thus improve synestotic quality.
Another object of the present invention is the preparation method providing above-mentioned dentistry implant.
The method provided comprises: be that the dentistry implant matrix of Nano tube array of titanium dioxide coating is immersed in containing in cobalt acetate solution by outer surface, under suitable reaction condition, cobalt element is loaded on nanotube coatings, obtains the dentistry implant being loaded with cobalt element.
Further, preparation method of the present invention comprises:
Outer surface is that the dentistry implant matrix of Nano tube array of titanium dioxide coating is immersed in and is mounted with in the politef High Temperature High Pressure hydro-thermal still of cobalt acetate solution by step 1;
Step 2, is placed in low-temperature sintering stove by the politef High Temperature High Pressure hydro-thermal still of step 1, adopts hydrothermal crystallisation methods to be loaded on nanotube coatings by cobalt element, obtains the dentistry implant being loaded with cobalt element.
Optionally, in described cobalt acetate solution, cobaltous acetate concentration is 0.01-0.1M.
Optionally, described hydrothermal crystallisation methods temperature is 200 DEG C, and heating rate is 5-10 DEG C/min, and packing density is 40%, and the hydrothermal crystallization time is 1-3h.
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 hydrothermal crystallization technique will carry cobalt mixture and be loaded into anodized coating, carry in hole that cobalt mixture hydrothermal crystallization thing can be uniformly distributed in anodized coating and outside hole, can not come off easily because of External Force Acting, and the nanotopography of anodized coating can not be changed egregiously.
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 not carrying cobalt element; B () is for loading the anodizing morphology figure after cobalt element 3h.
Fig. 2 is Energy Dispersive X-ray detector (EDX) figure that dentistry implant anodizing morphology carries cobalt element, and wherein (a) is the EDX energy spectrogram not carrying cobalt element; B () is for loading the EDX energy spectrogram after cobalt element 3h;
Fig. 3 is that dentistry implant anodizing morphology carries the scanning electron microscope of cultured cell after 7 days (SEM) photo figure after cobalt element;
Fig. 4 is the block diagram that different disposal surface cultivates that Rat Mesenchymal Stem Cells (MSCs) is correlated with into blood vessel gene expression for 14 days afterwards by reverse transcription quantitative PCR (qRT-PCR) detection, wherein CP is Tissue Culture Plate surface, PT is the pure titanium surface of the pure titanium of polishing, NT is the titanium implant surface not loading cobalt element after anodic oxidation, and NT-Co is the titanium implant surface loading cobalt element after anodic oxidation; Wherein (a) is the expression of HIF-1 α gene; B () is the expression of VEGF gene; ## represents compared to CP group diversity p<0.01.
Detailed description of the invention
Although the healing after the implantation of implantation body greatly depends on the foundation of blood vessel network, but article more attention is in the past implantation body's different-shape and adds the impact of loading on the osteogenetic process of surrounding, good vascularization itself can play the healing of acceleration bone regeneration around implant to realize the effect of more good bone union process, because bone itself is a kind of tissue of very vascular, it highly depends on the supply of blood, blood can bring nutrient substance, take away the refuse that metabolism produces simultaneously, this process and how much angiopoietic, the distance etc. of blood vessel and tissue distance has direct relation.If more than 150 μm-200 μm, (limit of diffusion of oxygen and nutrient substance) cannot ensure to obtain enough nutrition the nearest blood vessel distance of tissue distance, so be necessary for freshman bone tissue's new vessels.
The very important mechanism of the promotion vascularization function of cobalt is exactly that the anaerobic environment of cobalt induction makes HIF-1 alpha molecule raise, and the existence of cobalt can cause the environment of cell peripheral formation hypoxia inducible.Hypoxia inducible factor enhances the toleration of cell to oxygen deprivation stress by the expression of target gene, and the HIF-1 α that histology's aspect raises causes increasing of erythrocyte output and local to become the reinforcement of blood vessel, and then the supply of local blood obtains reinforcement.The HIF-1 α that the aspect of individual cells raises embodies the adaptation of cell for anaerobic environment.The toxicity mechanism of cobalt also may be realized by HIF-1 α.Cobalt ion directly can suppress proline hydroxylase (PHD), oxygen dependence hydroxylase, HIF-α aspartyl hydroxylase (FIH); above-mentioned three kinds of materials all have adjusted the degraded of HIFs or active reduction, and the existence of cobalt ion makes HIF degraded minimizing, transcriptional activity strengthens.Therefore, by the suppression of PHD and the FIH-1 hydroxylase activity effect to dependence oxygen, the HIFa degraded of hypoxia, cobalt ion blocking-up PHD-HIFa-VHL and p300 and CAD, in conjunction with two paths, make HIF protein content and transcriptional activity occur to reverse fast respectively.The regulation and control of HIF proteins downstream promote into the gene of blood vessel in a large number, and cobalt element greatly have stimulated local environment by the path of HIF albumen and produces new vessels.
Nano tube structure that anodic oxidation is formed is carried out on titanium surface perhaps can simulated in vivo environment preferably, the TiO2 nanotube caliber that anodic oxidation is formed is by different voltage, different electrolyte quota can change in hundreds of nanometer range tens, the size of applicable different tissues combination can be screened with this, the interface contacted in body due to cell is nano level structure, as recessed by 50 ~ 200nm size of the basement membrane of various tissue, prominent, hole and fibrous, the average mineral granularity of woven bone is 10 ~ 50nm, lamellar bone is made up of the inorganic mineral particles of diameter 2 ~ 5nm and long 20 ~ 50nm, organic principle type i collagen main in bone is wide is 0.5nm, the long triple helix structure for 300nm.TiO
2nanotube can the size of collagen fibril and arrangement in analog bone tissue, and it is close with the elastic modelling quantity of osseous tissue, better biological activity may be obtained, so carry out anodic oxidation formation nano tube structure at titanium implant surface to serve optimum facilitation for the rear synosteosis of implantation.
Dentistry implant matrix of the present invention is the implantation body's matrix used in prior art, as: the pure titanium titanium sheet that adopts represent pure titanium implant system the most common clinically.
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 the electrolyte of previous step configuration, 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, each 5min has been cleaned successively with acetone, dehydrated alcohol and deionized water;
5) configure hydrothermal crystallization mother solution: 1g cobaltous acetate powder is joined 40ml deionized water, form the cobalt acetate solution of 0.1M, fully stir with Glass rod, obtain the hydrothermal crystallization mother solution containing cobalt element;
6) the dentistry implant matrix of anodic oxidation is immersed in the hydrothermal crystallization mother solution containing cobalt element, is placed in high pressure water heating kettle, tighten lid mouth, water heating kettle is positioned in low-temperature sintering stove and heats; Adopt the method for hydrothermal crystallization that cobalt element is loaded into anodized coating, wherein, temperature is 200 DEG C, and heating rate is 10 DEG C/min, and the hydro-thermal time is 1h; Last in room temperature borehole cooling, leave standstill after taking out dentistry implant, the dentistry implant of cobalt element must be loaded with.
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 the electrolyte of previous step configuration, 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, each 5min has been cleaned successively with acetone, dehydrated alcohol and deionized water;
5) configure hydrothermal crystallization mother solution: 1g cobaltous acetate powder is joined 40ml deionized water, form the cobalt acetate solution of 0.1M, fully stir with Glass rod, obtain the hydrothermal crystallization mother solution containing cobalt element;
6) the dentistry implant matrix of anodic oxidation is immersed in the hydrothermal crystallization mother solution containing cobalt element, is placed in high pressure water heating kettle, tightens and withdraw the previous remark, water heating kettle is positioned in low-temperature sintering stove and heats; Adopt the method for hydrothermal crystallization that cobalt element is loaded into anodized coating, wherein, temperature is 200 DEG C, and heating rate is 10 DEG C/min, and the hydro-thermal time is 2h; Last in room temperature borehole cooling, leave standstill after taking out dentistry implant, the dentistry implant of cobalt element must be loaded with.
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 the electrolyte of previous step configuration, 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, each 5min has been cleaned successively with acetone, dehydrated alcohol and deionized water;
5) configure hydrothermal crystallization mother solution: 1g cobaltous acetate powder is joined 40ml deionized water, form the cobalt acetate solution of 0.1M, fully stir with Glass rod, obtain the hydrothermal crystallization mother solution containing cobalt element;
6) the dentistry implant matrix of anodic oxidation is immersed in the hydrothermal crystallization mother solution containing cobalt element, is placed in high pressure water heating kettle, tighten lid mouth, water heating kettle is positioned in low-temperature sintering stove and heats; Adopt the method for hydrothermal crystallization that cobalt element is loaded into anodized coating, wherein, temperature is 200 DEG C, and heating rate is 10 DEG C/min, and the hydro-thermal time is 3h; Last in room temperature borehole cooling, leave standstill after taking out dentistry implant, the dentistry implant of cobalt element must be loaded with.
With the dentistry implant being loaded with cobalt element prepared by embodiment 3, and in conjunction with relevant drawings, the present invention is further described.With reference to Fig. 1, for implantation body's matrix anode oxidized surface loads surface sweeping Electronic Speculum (SEM) photo of pattern before and after cobalt element, the microscopic appearance before cobalt element is not carried in comparison diagram 1 (a), visible Fig. 1 (b) is after hydro-thermal loads, and nanostructured surface covers one deck cobalt granule.Fig. 2 is Energy Dispersive X-ray (EDX) the energy spectrogram that implantation body's matrix anode oxidized surface loads pattern before and after cobalt element, as can be seen from the figure after cobalt element hydro-thermal loads, anodised implant surface occurs for cobalt element peak value really, proves that cobalt element is deposited on implant surface.The implant surface loaded in Fig. 3 after cobalt element has cultivated the scanning electron microscopic picture of mescenchymal stem cell after 7 days, visible load cobalt element after cellularity is not obviously affected, cell can normally in material surface field planting, sprawl.The cell HIF-1 Alpha of different disposal front and rear surfaces and the expression of VEGF gene is contrasted in Fig. 4.Tissue Culture Plate surface (CP), pure titanium surface (PT), the expression that HIF-1 α with VEGF of nano-array topographical surface cell is correlated with into blood vessel gene does not have notable difference, and after loading cobalt element, the HIF-1 α of titanium implant and the expression of VEGF related gene are obviously raised.Describe titanium implant after loading cobalt element and have obvious facilitation for the HIF-1 α of superficial cell and the expression of VEGF related gene.This formation for osseous tissue healing rear in the process of implant implantable bone tissue, defect area area of new bone has direct impact.Be first section herein load inorganic metal element by implant surface and realize facilitating the titanium implant of blood vessel object.
Other embodiments prepare dentistry implant, have similar results.Namely, after cobalt element hydro-thermal loads, still remain with complete nano tube structure while that anodised nanostructured surface having one deck cobalt granule to cover, and truly have the deposition of cobalt element.Load the expression that titanium implant after cobalt element is correlated with into blood vessel gene for HIF-1 α with VEGF of superficial cell and have obvious facilitation.
Claims (5)
1. a dentistry implant, is characterized in that, the outer surface of described dentistry implant is Nano tube array of titanium dioxide coating, and described nanotube coatings is loaded with facilitates angiogenic substance, described in facilitate blood vessel differentiation material to be cobalt element.
2. the preparation method of a dentistry implant, it is characterized in that, method comprises: be that the dentistry implant matrix of Nano tube array of titanium dioxide coating is immersed in containing in cobalt acetate solution by outer surface, under suitable reaction condition, cobalt element is loaded on nanotube coatings, obtains the dentistry implant being loaded with cobalt element.
3. the preparation method of dentistry implant as claimed in claim 2, is characterized in that, comprising:
Outer surface is that the dentistry implant matrix of Nano tube array of titanium dioxide coating is immersed in and is mounted with in the politef High Temperature High Pressure hydro-thermal still of cobalt acetate solution by step 1;
Step 2, is placed in low-temperature sintering stove by the politef High Temperature High Pressure hydro-thermal still of step 1, adopts hydrothermal crystallisation methods to be loaded on nanotube coatings by cobalt element, obtains the dentistry implant being loaded with cobalt element.
4. the preparation method of dentistry implant as claimed in claim 3, it is characterized in that, in described cobalt acetate solution, cobaltous acetate concentration is 0.01-0.1M.
5. the preparation method of dentistry implant as claimed in claim 3, it is characterized in that, described hydrothermal crystallisation methods temperature is 200 DEG C, and heating rate is 5-10 DEG C/min, and packing density is 40%, and the hydrothermal crystallization time is 1-3h.
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Cited By (4)
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| CN105597157A (en) * | 2015-12-28 | 2016-05-25 | 宝鸡文理学院 | Coating capable of promoting vascularization and anti-infection bioactivity and preparing method and application thereof |
| CN107019571A (en) * | 2017-06-02 | 2017-08-08 | 南方医科大学 | A kind of method that selective laser melting prepares dentistry implant |
| CN109692051A (en) * | 2018-12-12 | 2019-04-30 | 佛山市安齿生物科技有限公司 | A kind of cobalt carried titanium dioxide film layer and preparation method thereof |
| CN113186579A (en) * | 2021-04-20 | 2021-07-30 | 北京科技大学 | Titanium alloy oral cavity restoration body surface whitening self-cleaning coating and preparation method thereof |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105597157A (en) * | 2015-12-28 | 2016-05-25 | 宝鸡文理学院 | Coating capable of promoting vascularization and anti-infection bioactivity and preparing method and application thereof |
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| CN107019571A (en) * | 2017-06-02 | 2017-08-08 | 南方医科大学 | A kind of method that selective laser melting prepares dentistry implant |
| CN109692051A (en) * | 2018-12-12 | 2019-04-30 | 佛山市安齿生物科技有限公司 | A kind of cobalt carried titanium dioxide film layer and preparation method thereof |
| CN113186579A (en) * | 2021-04-20 | 2021-07-30 | 北京科技大学 | Titanium alloy oral cavity restoration body surface whitening self-cleaning coating and preparation method thereof |
| CN113186579B (en) * | 2021-04-20 | 2024-02-27 | 北京科技大学 | Titanium alloy oral cavity restoration surface whitening self-cleaning coating and preparation method thereof |
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