CN1237952C - Biologically active artificial teeth root and its preparation method - Google Patents
Biologically active artificial teeth root and its preparation method Download PDFInfo
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- CN1237952C CN1237952C CN 200410013918 CN200410013918A CN1237952C CN 1237952 C CN1237952 C CN 1237952C CN 200410013918 CN200410013918 CN 200410013918 CN 200410013918 A CN200410013918 A CN 200410013918A CN 1237952 C CN1237952 C CN 1237952C
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Abstract
The present invention relates to a bioactive artificial teeth root and a preparation method thereof. On the surface of the bioactive artificial teeth root, a porous Ca-P bioactive ceramic coating layer prepared with a bionic method, and bone morphogenetic protein (BMP) are arranged. The bioactive artificial teeth root has the composition that a double-layer porous Ca-P bioactive ceramic coating layer is arranged on the surface of a radical body of a metal tooth, and bone morphogenetic protein is compounded on the surface of the porous Ca-P bioactive ceramic coating layer. The preparation method has the steps that pure titanium or titanium alloy are adopted to process artificial tooth roots of which the surfaces are activated, the artificial tooth roots are then bionically deposited, and porous Ca-P bioactive ceramic coating layers each of which is composed of a compact calcium phosphate amorphous underlayer and a porous bone-like apatite crystal phase surface layer in sequence on the surfaces of the artificial tooth roots; the artificial tooth roots of which the surfaces are provided with porous Ca-P bioactive ceramic coating layers are soaked in mixed solution composed of bone morphogenetic protein and phosphate-buffered saline.
Description
Technical field
The present invention relates to a kind of artificial tooth root with bioactivity and preparation method thereof, particularly relate to a kind of surface and have the porous calcium phosphorus bioactive ceramic coating of biomimetic method preparation and artificial tooth root material of bone morphogenetic protein (BMP) and preparation method thereof, belong to technical field of biomedical materials.
Background technology
Canine implant can recover to lack the function of natural permanent teeth, and this just makes that the anodontia patient that can't repair with traditional method can obtain basic treatment, improves the quality of living.Normally used artificial tooth root is a metal material, because of it is a bio-inert material, combines with not forming firm physiology between the dental bed osseous tissue, after implantation, usually can become flexible, and causes artificial tooth root displacement failure.Adopt process for modifying surface to prepare biological coating (film) at the artificial tooth root metal base surface, can reduce the stripping of harmful metal ion under the human body environment, improve its biocompatibility and biological activity, make that forming firm physiology between artificial tooth root and the dental bed osseous tissue combines.The main inanimate matter of dental tissue is a calcium phosphorus phase, so calcium phosphate, hydroxyapatite, mixes CO
3 2-The bioactive layer of Ca-P ceramic phase compositions such as ionic osteoid apatite or OCP is to improve surface-active desirable selection of artificial tooth root.In addition, at artificial tooth root surface recombination bone morphogenetic protein (BMP), can significantly improve the ability of implantation initial stage artificial tooth root spatial induction skeletonization.
In the common method of artificial tooth root surface preparation calcium phosphate bioceramic coating is plasma spraying technology or based on the complex method of plasma spraying technology.Chinese patent ZL03113841.1 " induced osteogenesis artificial tooth root with bioactivity implantation body's material and manufacture method thereof " discloses a kind of complex method based on plasma spraying technology, promptly earlier at artificial tooth root surface plasma sprayed biological glass ceramics gradient coating, at the further compound BMP of coating surface, basic fibroblast growth factor or transforming growth factor, prepared artificial tooth root has good induced osteogenesis effect then.But this artificial tooth root surface biological glass ceramics gradient coating is that high temperature forms under the condition that differs greatly with the human body environment, and its composition and structure and biological osteolith differ greatly, and cause the instability of artificial tooth root long-term behaviour.
Summary of the invention
Technical problem: the objective of the invention is at the above-mentioned deficiency of artificial tooth root material, propose a kind of its surperficial BMP and prolong deenergized period, help artificial tooth root with bioactivity of giving full play to of BMP induced osteogenesis effect and preparation method thereof.
Technical scheme: the composition of artificial tooth root with bioactivity of the present invention is to be provided with one deck at metal root of the tooth matrix surface to have double-deck porous calcium phosphorus bioactive ceramic coating, surface at porous calcium phosphorus bioactive ceramic coating also is compounded with bone morphogenetic protein, the porous calcium phosphorus bioactive ceramic coating of being addressed is made up of calcium phosphate amorphous underlayer that contacts with metallic matrix and osteoid apatite crystalline phase surface layer, wherein, calcium phosphate amorphous underlayer thickness is 1-10 μ m; Osteoid apatite crystalline phase surface layer thickness is 10-100 μ m.
The method of preparation is:
1) at first select for use pure titanium or titanium alloy to process artificial tooth root;
2) artificial tooth root is carried out surface activation process, go on foot bionical deposition processes by two then, obtain the porous calcium phosphorus bioactive ceramic coating of forming successively by fine and close calcium phosphate amorphous underlayer and porous osteolith stone crystalline phase surface layer on the artificial tooth root surface;
3) surface is immersed in the mixed solution that bone morphogenetic protein and phosphate buffered saline(PBS) form by the artificial tooth root of porous calcium phosphorus bioactive ceramic coating, bone morphogenetic protein concentration is 0.1-50mg/L, 20-40 ℃ was soaked 5-15 hour down, slowly stirred once in middle every 1-2 hour, take out, get final product artificial tooth root with bioactivity material of the present invention.
It is the ebullient H of 10-60% that surface activation process adopts concentration
2O
2Aqueous solution, the processing time is 10-90 minute, take out flushing after, be immersed in temperature again and be 30-80 ℃, concentration and be in the NaOH aqueous solution of 1-10M 6-48 hour.
Two steps, bionical deposition processes comprised the steps:
1) the bionical calcifying solution A of preparation: bionical calcifying solution A presses the active constituent content of ionometer:
Sodium ion 500-850mM, magnesium ion 4.5-6.0mM, calcium ion 10.0-13.5mM, chloride ion 500-800mM, phosphoric acid hydrogen radical ion 4.0-6.0mM, bicarbonate ion 15.0-30.0mM;
2) the bionical calcifying solution B of preparation: bionical calcifying solution B presses the active constituent content of ionometer:
Sodium ion 100.0-180.0mM, potassium ion 4.0-5.5mM, magnesium ion 3.0-4.5mM, calcium ion 2.0-3.5mM, chloride ion 80.0-150.0mM, phosphoric acid hydrogen radical ion 0.5-1.5mM, bicarbonate ion 6.5-12.0mM, sulfate ion 0.5-1.0mM;
3) the bionical deposition processes of calcium phosphate amorphous underlayer: the artificial tooth root immersion temperature that surface activation process is crossed is among the 10-30 ℃ of bionical calcifying solution A, under stirring condition, take out after bionical deposition processes 12-36 hour, clean, drying, artificial tooth root material surface obtain the calcium phosphate amorphous layer of thickness 1-10 μ m;
4) the bionical deposition processes of osteoid apatite crystalline phase surface layer: the artificial tooth root immersion temperature that the surface is had the calcium phosphate amorphous layer is among the 30-50 ℃ of bionical calcifying solution B, took out in bionical deposition processes 12-144 hour, clean, drying, further deposit thickness is 10-100 μ m, porous osteoid apatite crystalline phase layer on the artificial tooth root surface phosphoric acid calcium amorphous layer.
Beneficial effect:
(1) artificial tooth root with bioactivity of the present invention has one deck to adopt bionic method being similar to the porous calcium phosphorus bioactive ceramic coating for preparing under the physiological environment at metal base surface, its surface further is compounded with bone morphogenetic protein (BMP), this artificial tooth root material has good biological activity and induced osteogenesis effect, can form firm physiology with the dental bed osseous tissue in a short time and combine.
(2) artificial tooth root porous surface Ca-P ceramic coating and metallic matrix bond strength height, and has an ideal double-decker: the calcium phosphate amorphous underlayer densification that contacts with the metal surface, can suppress that toxic metals is ionic in the metallic matrix separates out, and can be used as the deposition growing that " nucleus basal plane " promotes osteoid apatite crystalline phase surface layer; Osteoid apatite crystalline phase surface layer porous, thickness is 10-100 μ m, has good biological activity, also is the ideal carrier of BMP simultaneously, helps giving full play to of BMP induced osteogenesis effect.
This artificial tooth root with bioactivity has one deck to adopt bionic method being similar to the double-deck porous calcium phosphorus bioactive ceramic coating that has for preparing under the physiological environment at metal base surface, and its surface further is compounded with bone morphogenetic protein (BMP).Porous calcium phosphorus ceramic coating and metallic matrix bond strength height, form by calcium phosphate amorphous underlayer that contacts with the metal surface and osteoid apatite crystalline phase surface layer, the densification of calcium phosphate amorphous underlayer, thickness are 1-10 μ m, can suppress that toxic metals is ionic in the metallic matrix separates out; Osteoid apatite crystalline phase surface layer porous, thickness is 10-100 μ m, has good biological activity, also is the ideal carrier of BMP simultaneously.The compound common employing solution dipping method of artificial tooth root and BMP, BMP can deeply be penetrated in the porous osteoid apatite crystalline phase layer by capillarity, and the amount of carrying of artificial tooth root surface BMP is improved greatly.Behind the artificial tooth root implant into body, its surperficial BMP prolongs deenergized period, helps giving full play to of BMP induced osteogenesis effect.
The instantiation mode
Embodiment 1
(1) at first select for use pure titanium to process artificial tooth root;
(2) artificial tooth root surface activation process: after artificial tooth root used acetone, 70% ethanol, distilled water ultrasonic cleaning successively, adopting concentration was 20% ebullient H
2O
2Aqueous solution is handled, and the processing time is 45 minutes, take out flushing after, be immersed in temperature again and be in 30-50 ℃, the NaOH aqueous solution of 4M after 24-36 hour, take out distilled water flushing, 70 ℃ of dryings.
(3) the bionical deposition processes of calcium phosphate amorphous underlayer: the artificial tooth root immersion temperature that surface activation process is crossed is that bionical calcifying solution A is among 20 ℃ of bionical calcifying solution A by the active constituent content of ionometer: sodium ion 610mM, magnesium ion 4.5mM, calcium ion 12.5mM, chloride ion 610.0mM, phosphoric acid hydrogen radical ion 5.0mM, bicarbonate ion 18.0mM.Bionical calcifying solution A employing magnetic stirring apparatus stirs, takes out after bionical deposition processes 12-24 hour, and the distilled water ultrasonic cleaning, drying at room temperature, the artificial tooth root surface obtains the calcium phosphate amorphous layer of thickness 1.5-2.0 μ m, densification.
(4) the bionical deposition processes of osteoid apatite crystalline phase surface layer: the artificial tooth root immersion temperature that the surface is had the calcium phosphate amorphous layer is that bionical calcifying solution B presses the active constituent content of ionometer among 30 ℃ of bionical calcifying solution B: sodium ion 120.0mM, potassium ion 5.0mM, magnesium ion 3.5mM, calcium ion 2.5mM, chloride ion 120.0mM, phosphoric acid hydrogen radical ion 1.0mM, bicarbonate ion 11.0mM, sulfate ion 0.5mM.Took out in bionical deposition processes 12-36 hour, the distilled water ultrasonic cleaning, drying at room temperature, further deposit thickness is 15-20 μ m, porous osteoid apatite crystalline phase surface layer on the artificial tooth root surface phosphoric acid calcium amorphous underlayer.
(5) surface being immersed in bone morphogenetic protein and concentration by the artificial tooth root of porous calcium phosphorus bioactive ceramic coating is in the mixed solution formed of the phosphate buffered saline(PBS) of 0.1mol/L, bone morphogenetic protein concentration is 0.1-50mg/L, 20-40 ℃ was soaked 5-15 hour down, slowly stirred once, and took out in middle every 1-2 hour;
(6) with above-mentioned taking-up artificial tooth root with ethanol drip washing after, vacuum drying, the sterilization aseptic preservation in back, standby, get final product artificial tooth root with bioactivity of the present invention.
Embodiment 2
(1) at first select for use the Ti6Al4V alloy to process artificial tooth root;
(2) artificial tooth root surface activation process: after artificial tooth root used acetone, 70% ethanol, distilled water ultrasonic cleaning successively, adopting concentration was 30% ebullient H
2O
2Aqueous solution is handled, and the processing time is 90 minutes, take out flushing after, be immersed in temperature again and be 60-70 ℃, concentration and be in the NaOH aqueous solution of 8M 24-36 hour, take out distilled water flushing, 70 ℃ of dryings.
(3) the bionical deposition processes of calcium phosphate amorphous underlayer: the artificial tooth root immersion temperature that surface activation process is crossed is that bionical calcifying solution A is among 30 ℃ of bionical calcifying solution A by the active constituent content of ionometer: sodium ion 610mM, magnesium ion 4.5mM, calcium ion 12.5mM, chloride ion 610.0mM, phosphoric acid hydrogen radical ion 5.0mM, bicarbonate ion 18.0mM.Bionical calcifying solution A employing magnetic stirring apparatus stirs, takes out after bionical deposition processes 24-36 hour, and the distilled water ultrasonic cleaning, drying at room temperature, the artificial tooth root surface obtains the calcium phosphate amorphous layer of thickness 7.5-9.0 μ m, densification.
(4) the bionical deposition processes of osteoid apatite crystalline phase surface layer: the artificial tooth root immersion temperature that the surface is had the calcium phosphate amorphous layer is that bionical calcifying solution B presses the active constituent content of ionometer among 50 ℃ of molten B of bionical calcification: sodium ion 120.0mM, potassium ion 5.0mM, magnesium ion 3.5mM, calcium ion 2.5mM, chloride ion 120.0mM, phosphoric acid hydrogen radical ion 1.0mM, bicarbonate ion 11.0mM, sulfate ion 0.5mM.Took out in bionical deposition processes 72-144 hour, the distilled water ultrasonic cleaning, drying at room temperature, further deposit thickness is 60-80 μ m, porous osteoid apatite crystalline phase surface layer on the artificial tooth root surface phosphoric acid calcium amorphous underlayer.
(5) surface being immersed in bone morphogenetic protein and concentration by the artificial tooth root of porous calcium phosphorus bioactive ceramic coating is in the mixed solution formed of the phosphate buffered saline(PBS) of 0.1mol/L, bone morphogenetic protein concentration is 0.1-50mg/L, 20-40 ℃ was soaked 5-15 hour down, slowly stirred once, and took out in middle every 1-2 hour;
(6) with above-mentioned taking-up artificial tooth root with ethanol drip washing after, vacuum drying, the sterilization aseptic preservation in back, standby, get final product artificial tooth root with bioactivity of the present invention.
Embodiment 3
(1) at first select for use the Ti6Al4V alloy to process artificial tooth root;
(2) artificial tooth root surface activation process: after artificial tooth root used acetone, 70% ethanol, distilled water ultrasonic cleaning successively, adopting concentration was 30% ebullient H
2O
2Aqueous solution is handled, and the processing time is 90 minutes, take out flushing after, be immersed in temperature again and be 60-70 ℃, concentration and be in the NaOH aqueous solution of 8M 24-36 hour, take out distilled water flushing, 70 ℃ of dryings.
(3) the bionical deposition processes of calcium phosphate amorphous underlayer: the artificial tooth root immersion temperature that surface activation process is crossed is that bionical calcifying solution A is among 30 ℃ of bionical calcifying solution A by the active constituent content of ionometer: sodium ion 610mM, magnesium ion 4.5mM, calcium ion 12.5mM, chloride ion 610.0mM, phosphoric acid hydrogen radical ion 5.0mM, bicarbonate ion 18.0mM.Bionical calcifying solution A employing magnetic stirring apparatus stirs, takes out after bionical deposition processes 24-36 hour, and the distilled water ultrasonic cleaning, drying at room temperature, the artificial tooth root surface obtains the calcium phosphate amorphous layer of thickness 7.5-9.0 μ m, densification.
(4) the bionical deposition processes of osteoid apatite crystalline phase surface layer: the artificial tooth root immersion temperature that the surface is had the calcium phosphate amorphous layer is that bionical calcifying solution B presses the active constituent content of ionometer among 50 ℃ of molten B of bionical calcification: sodium ion 120.0mM, potassium ion 5.0mM, magnesium ion 3.5mM, calcium ion 2.5mM, chloride ion 120.0mM, phosphoric acid hydrogen radical ion 1.0mM, bicarbonate ion 11.0mM, sulfate ion 0.5mM.Took out in bionical deposition processes 48-64 hour, the distilled water ultrasonic cleaning, drying at room temperature, further deposit thickness is 40-50 μ m, porous osteoid apatite crystalline phase surface layer on the artificial tooth root surface phosphoric acid calcium amorphous underlayer.
(5) surface being immersed in bone morphogenetic protein and concentration by the artificial tooth root of porous calcium phosphorus bioactive ceramic coating is in the mixed solution formed of the phosphate buffered saline(PBS) of 0.1mol/L, bone morphogenetic protein concentration is 0.1-50mg/L, 20-40 ℃ was soaked 5-15 hour down, slowly stirred once, and took out in middle every 1-2 hour;
(6) with above-mentioned taking-up artificial tooth root with ethanol drip washing after, vacuum drying, the sterilization aseptic preservation in back, standby, get final product artificial tooth root with bioactivity of the present invention.
Obviously, the above embodiment of the present invention only is in order to clearly demonstrate example of the present invention, and is not to be qualification to embodiments of the present invention.For those of ordinary skill in the field; also can make other changes in different forms on the basis of the above description; here need not also can't give all embodiments exhaustive, and these belong to conspicuous variation or the change that spirit of the present invention amplified out and still are in protection scope of the present invention.
Claims (4)
1. artificial tooth root with bioactivity, it is characterized in that, the composition of this artificial tooth root with bioactivity is to be provided with one deck at metal root of the tooth matrix surface to have double-deck porous calcium phosphorus bioactive ceramic coating, surface at porous calcium phosphorus bioactive ceramic coating also is compounded with bone morphogenetic protein, the porous calcium phosphorus bioactive ceramic coating of being addressed is made up of calcium phosphate amorphous underlayer that contacts with metallic matrix and osteoid apatite crystalline phase surface layer, wherein, calcium phosphate amorphous underlayer thickness is 1-10 μ m; Osteoid apatite crystalline phase surface layer thickness is 10-100 μ m.
2. the preparation method of an artificial tooth root with bioactivity as claimed in claim 1 is characterized in that the method for preparing is:
1) at first select for use pure titanium or titanium alloy to process artificial tooth root;
2) artificial tooth root is carried out surface activation process, go on foot bionical deposition processes by two then, obtain the porous calcium phosphorus bioactive ceramic coating of forming successively by fine and close calcium phosphate amorphous underlayer and porous osteolith stone crystalline phase surface layer on the artificial tooth root surface;
3) surface is immersed in the mixed solution that bone morphogenetic protein and phosphate buffered saline(PBS) form by the artificial tooth root of porous calcium phosphorus bioactive ceramic coating, bone morphogenetic protein concentration is 0.1-50mg/L, 20-40 ℃ was soaked 5-15 hour down, slowly stirred once in middle every 1-2 hour, take out, get final product artificial tooth root with bioactivity.
3. the preparation method of artificial tooth root with bioactivity as claimed in claim 2 is characterized in that it is the ebullient H of 10-60% that surface activation process adopts concentration
2O
2Aqueous solution, the processing time is 10-90 minute, take out flushing after, be immersed in temperature again and be 30-80 ℃, concentration and be in the NaOH aqueous solution of 1-10M 6-48 hour.
4. the preparation method of artificial tooth root with bioactivity as claimed in claim 2 is characterized in that bionical deposition processes of two steps comprises the steps:
1) the bionical calcifying solution A of preparation: bionical calcifying solution A presses the active constituent content of ionometer:
Sodium ion 500-850mM, magnesium ion 4.5-6.0mM, calcium ion 10.0-13.5mM, chloride ion 500-800mM, phosphoric acid hydrogen radical ion 4.0-6.0mM, bicarbonate ion 15.0-30.0mM;
2) the bionical calcifying solution B of preparation: bionical calcifying solution B presses the active constituent content of ionometer:
Sodium ion 100.0-180.0mM, potassium ion 4.0-5.5mM, magnesium ion 3.0-4.5mM, calcium ion 2.0-3.5mM, chloride ion 80.0-150.0mM, phosphoric acid hydrogen radical ion 0.5-1.5mM, bicarbonate ion 6.5-12.0mM, sulfate ion 0.5-1.0mM;
3) the bionical deposition processes of calcium phosphate amorphous underlayer: the artificial tooth root immersion temperature that surface activation process is crossed is among the 10-30 ℃ of bionical calcifying solution A, under stirring condition, take out after bionical deposition processes 12-36 hour, clean, drying, artificial tooth root material surface obtain the calcium phosphate amorphous layer of thickness 1-10 μ m;
4) the bionical deposition processes of osteoid apatite crystalline phase surface layer: the artificial tooth root material immersion temperature that the surface is had the calcium phosphate amorphous layer is among the 30-50 ℃ of bionical calcifying solution B, took out in bionical deposition processes 12-144 hour, clean, drying, further deposit thickness is 10-100 μ m, porous osteoid apatite crystalline phase layer on the artificial tooth root material surface calcium phosphate amorphous layer.
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| CN 200410013918 CN1237952C (en) | 2004-01-16 | 2004-01-16 | Biologically active artificial teeth root and its preparation method |
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| CN1237952C true CN1237952C (en) | 2006-01-25 |
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| CN101766538B (en) * | 2009-12-31 | 2012-02-22 | 东南大学 | Rare earth element cerium slow-release type artificial tooth root based on nanometer tube array surface |
| CN101766840B (en) * | 2009-12-31 | 2012-10-24 | 东南大学 | Antibacterial functionalized artificial joint with silver-loaded nanotube array surface |
| CN101766839B (en) * | 2009-12-31 | 2012-10-24 | 东南大学 | Silver-loaded antibacterial artificial joint and preparation method thereof |
| CN101744666B (en) * | 2010-01-01 | 2012-02-22 | 东南大学 | Artificial tooth root with slow release function of trace element of selenium and preparation method thereof |
| CN101732762B (en) * | 2010-01-01 | 2013-04-03 | 东南大学 | Bioactive artificial joint capable of slowly releasing trace element selenium |
| CN101766540B (en) * | 2010-01-01 | 2011-12-14 | 东南大学 | Antibacterial artificial tooth root with bioactivity and preparation method thereof |
| EP2359873A1 (en) * | 2010-02-12 | 2011-08-24 | Straumann Holding AG | Process for preparing a body having an osteointegrative surface |
| CN101791435B (en) * | 2010-03-26 | 2012-11-21 | 浙江大学 | Method of collagen modification of medical metal implant surface |
| JP6039814B2 (en) * | 2012-09-26 | 2016-12-07 | ストラウマン ホールディング アーゲー | Dental implant or abutment comprising a ceramic body coated with a monomolecular phosphate layer |
| CN106333753B (en) * | 2016-08-23 | 2019-07-02 | 天津医科大学口腔医院 | The dental implant and preparation method thereof of individuation bionic |
| CN111282019B (en) * | 2020-01-20 | 2021-07-16 | 浙江大学 | Medical titanium implant and preparation method thereof |
| CN115382010B (en) * | 2021-05-19 | 2023-06-06 | 北京荷月顺畅生物科技有限公司 | Bionic bone material and preparation method thereof |
| CN115382016B (en) * | 2021-05-19 | 2023-06-23 | 北京荷月顺畅生物科技有限公司 | Bionic bone material for resisting cancer, medicinal composition containing bionic bone material and preparation method of medicinal composition |
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