CN104645413B - A kind of dentistry implant and preparation method thereof - Google Patents
A kind of dentistry implant and preparation method thereof Download PDFInfo
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- CN104645413B CN104645413B CN201510016985.1A CN201510016985A CN104645413B CN 104645413 B CN104645413 B CN 104645413B CN 201510016985 A CN201510016985 A CN 201510016985A CN 104645413 B CN104645413 B CN 104645413B
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Abstract
The present invention relates to a kind of dentistry implant and preparation method thereof, involved dentistry implant is the anodized coating with nanotopography, nanotube coatings is loaded with efficiently facilitates blood vessel differentiation material cobalt element, involved method includes that the dentistry implant matrix by outer surface is Nano tube array of titanium dioxide coating is immersed in containing in cobalt acetate solution, under suitable reaction condition, cobalt element is loaded on nanotube coatings, it is thus achieved that be loaded with the dentistry implant of cobalt element.The present invention uses hydrothermal crystallization technique that load cobalt mixture is loaded into anodized coating, carry outside in cobalt mixture hydrothermal crystallization thing may be uniformly distributed in the hole of anodized coating and hole, will not come off easily because of External Force Acting, and the nanotopography of anodized coating will not be changed egregiously.
Description
Technical field
The present invention relates to dentistry implant material, particularly to a kind of dentistry implant being loaded with cobalt element and
Preparation method.
Background technology
Along with planting technology develops, dentistry implant is widely used to defect of dentition and the disappearance patient of clinic
Reparation.But titanium or titanium alloy is after implanting in bone, it is possible that the bad bone of bone regeneration around implant
In conjunction with, ultimately result in the failure that implantation body implants.Implant necessarily also results in during implanting osseous tissue
The destruction of osseous tissue, this destruction includes the successional destruction of bone, hemorrhage, can approximate and be interpreted as a kind of people
For the fracture manufactured, the osseous tissue that " fracture " is occurred together afterwards heals, the formation of defect area area of new bone will be straight
Connecing and affect implantation body and osseointegration intensity, this process is affected by various factors, including osteoblastic work
Property, the pattern of implantation body, blood supply etc..Wherein blood supply for bone regeneration around implant sclerotin healing,
Bone remodeling has critically important impact, and the good blood supply of bone regeneration around implant both can be to damage field supply
Oxygen, various nutrient substance, can also get rid of the metabolic waste of tissue simultaneously in time.So it is contemplated that carrying
High implantation body is implanted to power from promoting that skeletonization is started with in terms of promoting into blood vessel two.Now, in order to promote office
Portion's skeletonization, existing multiple implant surface pattern occurs and is applied to clinic, mainly use anodic oxidation,
The technology such as the slurry spraying of differential arc oxidation, titanium or sandblasting acid etching are to improve implant surface pattern.Anodic oxidation conduct
The implant surface treatment technology of one of which comparative maturity is in wide clinical application, and its implant surface has
There is nano tubular structure, synosteosis speed can be improved.
In order to improve into vessel patency, have been reported now and mainly facilitate the blood vessel differentiation factor to be loaded into plantation
The scientific research report of surface, mainly has the vascular endothelial cell factor (VEGF), oxygen deficient induction factor 1 (HIF-1
α) etc..But when there is activity reduction, release of cytokines after cytokine is transformed in various degree in said method
Between shorter, can not more persistently promote into the problems such as blood vessel.Its a kind of loading method is by VEGF (blood
Endothelial cell somatomedin) load in poly-dopamine coating, and it is wrapped in pure titanium surface.Another kind side
Method, it is simply that implantation body's matrix is immersed in biotic factor VEGF.VEGF activity warp in said method
Cannot ensure after crossing transformation;Additionally above-mentioned steps is loaded down with trivial details, it is necessary first to use multi-step preparation more unstable
Coatings etc., then could load after mixing with the albumen such as VEGF;The most above-mentioned loading method can not be simultaneously
Promote titanium surface osteogenetic process, do not consider simultaneously other somatomedin for Osseointegrated implants with become blood vessel
Facilitation.Cobalt element has been widely studied the generation of induction ischaemia environment, then promotes HIF-1
α, produces the change of a series of adaptation anaerobic environment then, including promoting local environment new vessels
Generate.
Summary of the invention
It is an object of the present invention to provide a kind of dentistry implant, this dentistry implant is for having nanometer shape
The anodized coating of looks, nanotube coatings is loaded with efficiently facilitates blood vessel differentiation material cobalt element, cobalt unit
Element has been proved to induce local cells to secrete HIF-1 α, thus inducing cell is to anoxia ring further
The adaptation in border, including the generation promoting local new vessels.The present invention can improve bone more rapidly
Promote while association rate that local becomes vascular process, thus improve synestotic quality.
Further object is that the preparation method that above-mentioned dentistry implant is provided.
The method provided includes: by the dentistry implant base that outer surface is Nano tube array of titanium dioxide coating
Body is immersed in containing in cobalt acetate solution, under suitable reaction condition, cobalt element is loaded into nanotube and is coated with
On layer, it is thus achieved that be loaded with the dentistry implant of cobalt element.
Further, the preparation method of the present invention includes:
Step 1, is immersed in dress by the dentistry implant matrix that outer surface is Nano tube array of titanium dioxide coating
It is loaded with in the politef High Temperature High Pressure hydro-thermal still of cobalt acetate solution;
Step 2, is placed in the politef High Temperature High Pressure hydro-thermal still of step 1 in low-temperature sintering stove, uses
Cobalt element is loaded on nanotube coatings by hydrothermal crystallisation methods, it is thus achieved that be loaded with the dentistry implant of 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, packing density
Being 40%, the hydrothermal crystallization time is 1-3h.
The dentistry implant of the present invention, uses anode oxidation process to have in implantation body's outer surface of matrix preparation and receives
The anodized coating of mitron pattern, nanotopography is tubular structure, and aperture is nanoscale;Employing hydro-thermal is tied
Load cobalt mixture is loaded into anodized coating by brilliant technique, and carrying cobalt mixture hydrothermal crystallization thing can uniformly divide
In being distributed in the hole of anodized coating and outside hole, will not come off easily because of External Force Acting, and will not be excessive
Ground changes the nanotopography of anodized coating.
Accompanying drawing explanation
With detailed description of the invention, the present invention is described in further detail below in conjunction with the accompanying drawings.
Fig. 1 is scanning electron microscope (SEM) the photo figure of dentistry implant anodizing morphology, wherein (a)
For not carrying the anodizing morphology figure of cobalt element;B () is the anodizing morphology figure after loading cobalt element 3h.
Fig. 2 is the Energy Dispersive X-ray detector that dentistry implant anodizing morphology carries cobalt element
(EDX) figure, wherein (a) is the EDX energy spectrogram not carrying cobalt element;B () is for loading cobalt element 3h
After EDX can spectrogram;
Fig. 3 is to cultivate cell scanning electron microscope after 7 days after dentistry implant anodizing morphology carries cobalt element
(SEM) photo figure;
Fig. 4 is that reverse transcription was passed through after 14 days in different disposal surface cultivation Rat Mesenchymal Stem Cells (MSCs)
The block diagram of blood vessel gene expression is correlated with in quantitative PCR (qRT-PCR) detection, and wherein CP is cell training
Supporting plate surface, PT is polishing pure titanium pure titanium surface, and NT is the titanium plantation not loading cobalt element after anodic oxidation
Surface, NT-Co is the titanium implant surface loading cobalt element after anodic oxidation;Wherein (a) is HIF-1
The expression of α gene;B () is the expression of VEGF gene;## represents poor compared to CP group
Opposite sex p < 0.01.
Detailed description of the invention
Although the healing after the implantation of implantation body depend heavilys on the foundation of blood vessel network, but conventional literary composition
Chapter more attention is implantation body's different-shape and the load impact on the osteogenetic process of surrounding, good
Vascularization itself can play the healing accelerating bone regeneration around implant to realize the best bone union process
Effect because bone itself is the tissue of a kind of very vascular, it is highly dependent on the supply of blood, blood
Liquid can bring nutrient substance, takes away the refuse that metabolism produces simultaneously, this process with angiopoietic how much,
The distance etc. of blood vessel and tissue distance has direct relation.If the nearest blood vessel distance of tissue distance exceedes
150 μm-200 μm (oxygen and the limit of diffusion of nutrient substance) will be unable to ensure to obtain enough nutrition,
So being necessary for freshman bone tissue's new vessels.
The critically important mechanism of the promotion vascularization function of cobalt is exactly that the anaerobic environment of cobalt induction makes HIF-1 alpha molecule
Raising, the existence of cobalt can cause cell peripheral to form the environment of hypoxia inducible.Hypoxia inducible factor passes through target
The expression of gene enhances the cell toleration to oxygen deprivation stress, and the HIF-1 α that histology's aspect raises causes
Increasing and the reinforcement of local one-tenth blood vessel of erythrocyte yield, and then the supply of local blood is added
By force.The HIF-1 α raised in the aspect of individual cells embodies the cell adaptation for anaerobic environment.Cobalt
Toxicity mechanism realizes possibly by HIF-1 α.Cobalt ion can directly suppress proline hydroxylase
(PHD), oxygen dependence hydroxylase, HIF-α aspartyl hydroxylase (FIH), above-mentioned three kinds of materials
The degraded or the activity that all have adjusted HIFs reduce, and the existence of cobalt ion makes HIF degraded reduce, transcriptional activity
Strengthen.Therefore, by the suppression to PHD and the FIH-1 hydroxylase activity effect relying on oxygen, hypoxia, cobalt
Ion blocks the HIFa degraded of PHD-HIFa-VHL and is combined two paths with p300 with CAD, makes respectively
There is quickly reversion in HIF protein content and transcriptional activity.The regulation and control of HIF proteins downstream promote into blood vessel in a large number
Gene, cobalt element greatly have stimulated local environment by the path of HIF albumen and produces new vessels.
Titanium surface carry out the formed nano tube structure of anodic oxidation perhaps can preferable simulated in vivo environment, sun
The TiO2 nanotube caliber that pole oxidation is formed can be tens by different voltage, different electrolyte quota
Change in hundreds of nanometer range, can screen, with this, the size that applicable different tissues combines, owing to cell exists
The interface contacted in body is nano level structure, if the basement membrane of various tissues is by 50~200nm
Recessed, prominent, the hole of size and fiber composition, the average mineral granularity of woven bone is 10~50nm, lamellar bone by
Diameter 2~5nm and the inorganic mineral particles composition of long 20~50nm, organic principle I type main in bone
Collagen is the triple helix structure of a width of 0.5nm, a length of 300nm.TiO2Nanotube can analog bone group
Knit the size and arrangement of middle collagen fibril, and close with the elastic modelling quantity of osseous tissue, may obtain more preferably
Biological activity, so titanium implant surface carry out anodic oxidation formed nano tube structure for implant after bone
In conjunction with serving optimum facilitation.
The dentistry implant matrix of the present invention be in prior art use implantation body's matrix, as: use
Pure titanium titanium sheet represents the most most commonly seen pure titanium implant system.
The following is the specific embodiment that inventor provides, so that technical scheme to be further explained
Bright.
Embodiment 1:
1) select pure titanium to be processed into dentistry implant matrix, after the polishing of dentistry implant matrix surface, use successively
Each 5 minutes of acetone, dehydrated alcohol and deionized water ultrasonic cleaning, dry up stand-by;
2) configuration anode oxidation process electrolyte: ethylene glycol is solvent, and solute is 0.5% mass fraction
NH4F, the CH of 5% volume fraction3OH, and 5% volume fraction deionized water;
3) anode oxidation process is used to prepare Nano tube array of titanium dioxide coating at implantation body's outer surface of matrix:
Graphite carbon rod is negative electrode, and dentistry implant matrix, as anode, puts into the electrolyte of previous step configuration,
Concrete technology parameter is: supply frequency 50Hz ± 2Hz, and voltage is 40V, processes time 1h, reaction temperature
For room temperature;
4) after prepared by implantation body's matrix surface Nano tube array of titanium dioxide coating, by acetone, anhydrous second
Alcohol and deionized water clean each 5min successively;
5) configuration hydrothermal crystallization mother solution: 1g cobaltous acetate powder joins 40ml deionized water, forms 0.1M
Cobalt acetate solution, be sufficiently stirred for 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,
It is placed in high pressure water heating kettle, tightens lid mouth, water heating kettle is positioned in low-temperature sintering stove heating;Use hydro-thermal
Cobalt element is loaded into anodized coating by the method for crystallization, and wherein, temperature is 200 DEG C, and heating rate is
10 DEG C/min, the hydro-thermal time is 1h;Finally lower the temperature at room temperature, stand after taking out dentistry implant, to obtain final product
It is loaded with the dentistry implant of cobalt element.
Embodiment 2:
1) select pure titanium to be processed into dentistry implant matrix, after the polishing of dentistry implant matrix surface, use successively
Each 5 minutes of acetone, dehydrated alcohol and deionized water ultrasonic cleaning, dry up stand-by;
2) configuration anode oxidation process electrolyte: ethylene glycol is solvent, and solute is 0.5% mass fraction
NH4F, the CH of 5% volume fraction3OH, and 5% volume fraction deionized water;
3) anode oxidation process is used to prepare Nano tube array of titanium dioxide coating at implantation body's outer surface of matrix:
Graphite carbon rod is negative electrode, and dentistry implant matrix, as anode, puts into the electrolyte of previous step configuration,
Concrete technology parameter is: supply frequency 50Hz ± 2Hz, and voltage is 40V, processes time 1h, reaction temperature
For room temperature;
4) after prepared by implantation body's matrix surface Nano tube array of titanium dioxide coating, by acetone, anhydrous second
Alcohol and deionized water clean each 5min successively;
5) configuration hydrothermal crystallization mother solution: 1g cobaltous acetate powder joins 40ml deionized water, forms 0.1M
Cobalt acetate solution, be sufficiently stirred for 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,
It is placed in high pressure water heating kettle, tightens and withdraw the previous remark, water heating kettle is positioned in low-temperature sintering stove heating;Use hydro-thermal
Cobalt element is loaded into anodized coating by the method for crystallization, and wherein, temperature is 200 DEG C, and heating rate is
10 DEG C/min, the hydro-thermal time is 2h;Finally lower the temperature at room temperature, stand, i.e. 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 successively
Each 5 minutes of acetone, dehydrated alcohol and deionized water ultrasonic cleaning, dry up stand-by;
2) configuration anode oxidation process electrolyte: ethylene glycol is solvent, and solute is 0.5% mass fraction
NH4F, the CH of 5% volume fraction3OH, and 5% volume fraction deionized water;
3) anode oxidation process is used to prepare Nano tube array of titanium dioxide coating at implantation body's outer surface of matrix:
Graphite carbon rod is negative electrode, and dentistry implant matrix, as anode, puts into the electrolyte of previous step configuration,
Concrete technology parameter is: supply frequency 50Hz ± 2Hz, and voltage is 40V, processes time 1h, reaction temperature
For room temperature;
4) after prepared by implantation body's matrix surface Nano tube array of titanium dioxide coating, by acetone, anhydrous second
Alcohol and deionized water clean each 5min successively;
5) configuration hydrothermal crystallization mother solution: 1g cobaltous acetate powder joins 40ml deionized water, forms 0.1M
Cobalt acetate solution, be sufficiently stirred for 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,
It is placed in high pressure water heating kettle, tightens lid mouth, water heating kettle is positioned in low-temperature sintering stove heating;Use hydro-thermal
Cobalt element is loaded into anodized coating by the method for crystallization, and wherein, temperature is 200 DEG C, and heating rate is
10 DEG C/min, the hydro-thermal time is 3h;Finally lower the temperature at room temperature, stand, i.e. after taking out dentistry implant
The dentistry implant of cobalt element must be loaded with.
With the dentistry implant being loaded with cobalt element of embodiment 3 preparation, and combine relevant drawings to the present invention
It is further described.With reference to Fig. 1, for pattern before and after implantation body's matrix anode oxidized surface loading cobalt element
Surface sweeping Electronic Speculum (SEM) photo, comparison diagram 1 (a) does not carries the microscopic appearance before cobalt element, it is seen that figure
1 (b), after hydro-thermal loads, nanostructured surface covers one layer of cobalt granule.Fig. 2 is implantation body's matrix sun
Energy Dispersive X-ray (EDX) the energy spectrogram of pattern before and after the oxidized surface loading cobalt element of pole, from figure
Can be seen that anodised implant surface goes out for cobalt element peak value really after cobalt element hydro-thermal loads
Existing, it was demonstrated that cobalt element is deposited on implant surface.Fig. 3 loads the implant surface after cobalt element cultivate
Mescenchymal stem cell scanning electron microscopic picture after 7 days, it is seen that load unobvious to cellularity shadow after cobalt element
Ring, cell can normally in material surface field planting, sprawl.Fig. 4 contrasts the thin of different disposal front and rear surfaces
Born of the same parents HIF-1 α and the expression of VEGF gene.Tissue Culture Plate surface (CP), pure titanium surface (PT), receive
HIF-1 α with VEGF of rice array topographical surface cell is correlated with into the expression of blood vessel gene does not has notable difference
Property, and after loading cobalt element, the HIF-1 α of titanium implant and the expression of VEGF related gene are substantially raised.
Illustrate loading titanium implant after cobalt element for the HIF-1 α of superficial cell and VEGF related gene
Expression has obvious facilitation.This heals for rear osseous tissue during implant implantation osseous tissue, lacks
The formation damaging region area of new bone has directly impact.It is first herein and is loaded by implant surface inorganic
Metallic element and realize facilitating the titanium implant of blood vessel purpose.
Other embodiments prepare dentistry implant, have similar results.After i.e. cobalt element hydro-thermal loads, anodic oxygen
The nanostructured surface changed has one layer of cobalt granule still to remain with complete nano tube structure while of covering, and truly has
The deposition of cobalt element.After loading cobalt element, titanium implant is relevant for HIF-1 α with VEGF of superficial cell
The expression becoming blood vessel gene has obvious facilitation.
Claims (3)
1. the preparation method of a dentistry implant, it is characterised in that method includes:
Step 1, is immersed in dress by the dentistry implant matrix that outer surface is Nano tube array of titanium dioxide coating
It is loaded with in the politef High Temperature High Pressure hydro-thermal still of cobalt acetate solution;
Step 2, is placed in the politef High Temperature High Pressure hydro-thermal still of step 1 in low-temperature sintering stove, uses
Cobalt element is loaded on nanotube coatings by hydrothermal crystallisation methods, it is thus achieved that be loaded with the dentistry implant of cobalt element.
2. the preparation method of dentistry implant as claimed in claim 1, it is characterised in that described acetic acid
In cobalt liquor, cobaltous acetate concentration is 0.01-0.1M.
3. the preparation method of dentistry implant as claimed in claim 1, it is characterised in that described hydro-thermal
Crystallization process temperature is 200 DEG C, and heating rate is 5-10 DEG C/min, and packing density is 40%, the hydrothermal crystallization time
For 1-3h.
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CN105597157B (en) * | 2015-12-28 | 2018-07-27 | 周建宏 | One kind can promote vascularization and anti-infection bio active coating and its preparation method and application |
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 |
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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