CN1181803C - Induction ossified bio-active artificial tooth root implant material and preparing method thereof - Google Patents
Induction ossified bio-active artificial tooth root implant material and preparing method thereof Download PDFInfo
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- CN1181803C CN1181803C CNB031138411A CN03113841A CN1181803C CN 1181803 C CN1181803 C CN 1181803C CN B031138411 A CNB031138411 A CN B031138411A CN 03113841 A CN03113841 A CN 03113841A CN 1181803 C CN1181803 C CN 1181803C
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Abstract
The present invention relates to an artificial tooth root implant with bioactivity, particularly to an artificial tooth root implant material capable of inducing the bioactive gradient coating layer of osteogenesis, and a preparation method thereof. The present invention adopts a plasma spraying technique which is under the fully automatic control of net energy, and a bioactive coating layer of which the ingredient and the structure are in continuous gradient change is coated on the surface of a metal base with superior biocompatibility. The constituents and the quality percentage content thereof of the coating layer comprise 30 to 80% of hydroxyapatite nanometer powder, 5 to 20% of bioactive glass nanometer powder, 5 to 20% of alumina nanometer powder, and 10 to 40% of titanium oxide nanometer powder. Bone morphogenetic protein, basic fibroblast growth factors or transforming growth factors (beta) are arranged on the surface of the gradient coating layer. The artificial tooth root implant of the present invention has favorable osteogenesis induction and bioactivity, and the adhesive strength between the coating layer of the artificial tooth root implant material and the metal base, which meets the requirements of clinical application.
Description
Technical field
The present invention relates to artificial tooth root with bioactivity implantation body, specifically be meant induced osteogenesis bio-active gradient coating artificial tooth root implantation body material and preparation method thereof.
Background technology
Because the tooth excalation that a variety of causes causes or whole disappearance have directly influenced the healthy and attractive in appearance of people, modern artificial tooth's planting technology makes the mistake tooth replantation become possibility.Canine implant can recover to lack the repertoire of natural permanent teeth and the state of similar natural permanent teeth, and a large amount of anodontia patients that can't repair with traditional method are treated at all.Clinical practice at present tooth root planting body the most widely is to be made by pure titanium of metal or titanium alloy, this class implantation body has excellent biological compatibility and excellent mechanical property and processing characteristics, but because the metal tooth implant belongs to bio-inert material, dental bed and artificial tooth root can not form biological combination, be easy to infect, become flexible, late result is poor.Hydroxyapatite coating layer manual tooth planting body material has good biological activity and biocompatibility, yet the bond strength of hydroxyapatite coating layer and metallic matrix is low, under the corrosion function of stress and biofluid, coating comes off easily, dissolves and corrodes, cause implantation body's biological activity to reduce, shorten service life, even infect.Chinese patent ZL97119791.1 " preparation method of artificial joint with bio-active gradient coating " discloses a kind of in metal base surface bio-active gradient coating preparation methods, effectively improve the bond strength between coating and metallic matrix, improved artificial tooth's function and user mode.But still there are some unsolved technical problems in such material, mainly is that material itself does not have the induced osteogenesis function, behind material implantable bioartificial body, needs the long time to form stable biology with organism and combines.Therefore exist early stage set time length might cause the bone regeneration around implant tissue infection, problems such as biological activity reduction.
Summary of the invention
The objective of the invention is the problem that exists at present artificial tooth root implantation body material, bio-active gradient coating artificial tooth root implantation body material of a kind of induced osteogenesis and preparation method thereof is provided, thereby make implantation body's material produce biological the combination with tissue in a short time, and form an integral body, solve the early stage fixation problem and the late result problem of tooth root planting body material.
Purpose of the present invention can realize by following measure:
A kind of induced osteogenesis artificial tooth root with bioactivity implantation body material is characterized in that:
(1) be matrix with the good metal of biocompatibility, metal base surface prepares bioactivity coatings;
(2) on the structure from densification to porous, be the bio-active gradient coating that continuous gradient changes from biological stability to biological activity on the composition, its coating layer thickness is that the porosity of 80～100 μ m, face coat is 20～30%;
(3) composition of gradient coating and quality percentage composition thereof are hydroxyapatite nano-powder 30～80%, bioactive glass nano powder 5～20%, nanometer alumina powder 5～20% and TiOx nano powder body 10～40%;
(4) the gradient coating surface-assembled bone morphogenetic protein is arranged or/and basic fibroblast growth factor or/and transforming growth factor.
A kind of induced osteogenesis artificial tooth root with bioactivity implantation body preparation methods, comprise the plasma spraying technology that adopts full-automatic net energy control, the metal base surface good at biocompatibility prepares bio-active gradient coating, the composition and the structure that it is characterized in that bioactivity coatings all are the continuous gradient variation, and the bioactivity coatings surface-assembled has bioactie agent, and concrete steps are as follows:
The preparation of step 1, bio-active gradient coating
(1) composition of gradient coating and quality percentage composition adjusting range thereof are as follows:
Hydroxyapatite nano-powder 30～80%
Bioactive glass nano powder 5～20%
Nanometer alumina powder 5～20%
TiOx nano powder body 10～40%
With the metal prostheses is substrate, and the rule of coating composition distribution gradient is from inside to outside:
Hydroxyapatite nano-powder 30～80% is progressively and increases progressively
Bioactive glass nano powder 20～5% is progressively and successively decreases
Nanometer alumina powder 20～5% is progressively and successively decreases
TiOx nano powder body 40～10% is progressively and successively decreases
(2) particle size range of above-mentioned nano-powder is 30～80nm, and need carry out conventional surface activation process;
(3) according to the prescription and the requirement of above-mentioned gradient coating material, accurately control the conveying capacity and the plasma spray coating process parameter of various nano-powders, gradient coating thickness is that the porosity of 80～100 μ m, face coat is 20～30%; The plasma spray coating process parameter is as follows: main gas: argon 70～90scfh, inferior gas: hydrogen 5～10scfh, spraying current: 400～600A, spray voltage: 40～60V, spray distance: 100～150mm;
Step 2, assembling bioactie agent
(1) a kind of in bone morphogenetic protein, basic fibroblast growth factor or the transforming growth factor or two kinds or three kinds of bioactie agents are dissolved in solvent, make the concentration that contains bioactie agent in the corresponding solution be: bone morphogenetic protein 0～500 μ g/L, basic fibroblast growth factor 0～10 μ g/L, or transforming growth factor 0～50 μ g/L; When three kinds of bioactie agents are that bone morphogenetic protein, basic fibroblast growth factor, transforming growth factor are dissolved in solvent simultaneously, make in the solution concentration range of bioactie agent as follows: bone morphogenetic protein 100～500 μ g/L, basic fibroblast growth factor 2～10 μ g/L, transforminggrowthfactor-0～50 μ g/L.
(2) will contain bioactie agent solution places 30～37 ℃ calorstat low-speed oscillation after 5～10 minutes, the prepared bio-active gradient coating material of step 1 is immersed in this solution, kept 2～8 hours, take out the vacuum draw lyophilization then, select epoxyethane fumigation sterilization 3～5 hours for use, the artificial tooth root with bioactivity implantation body material that obtains having the induced osteogenesis function.
The present invention compared with prior art has following advantage:
1, loose structure on bio-active gradient coating surface (porosity of face coat is 20～30%) and bioactive ingredients help forming synostosis between implant and osseous tissue, can be used as the carrier and the support of various biotic factors, active somatic cell simultaneously.
2, the bio-active gradient coating surface-assembled has bioactie agent, have induced osteogenesis function and biological activity, can be at short notice produce with gums biologically combine, tissue and cell effect, the metabolism of promotion material participant soma, it is fast that the patient recovers.
3, bio-active gradient coating have on the structure from densification to porous, on the composition from Biostatic to bioactive pair of gradient coating feature.The compact texture of coating bottom and biological stability composition have obviously improved bond strength and tooth implant antibody liquid solvability in the Human Physiology environment of bioactivity coatings and metallic matrix, help stoping the corrosion of body fluid simultaneously, solved the late result problem that tooth root planting body material is faced metallic matrix.
4, the prepared induced osteogenesis artificial tooth root with bioactivity implantation body material of the present invention has good induced osteogenesis function, biological activity and biocompatibility, implantation body can form firm biology with dental bed in the short time and combine, and steady in a long-term the existence, satisfy the clinical practice requirement.
The specific embodiment
Embodiment 1
Select for use root of the tooth that the pure titanium of metal processes a collection of Canis familiaris L. as matrix material, adopt the Praxair4550 plasma spraying equipment to prepare bio-active gradient coating.Utilize biological package technique that bone morphogenetic protein is assembled in the gradient coating surface then, make material have induced osteogenesis function and good biological activity.Its concrete preparation process is as follows:
The preparation of the first step, bio-active gradient coating
Particle size range is carried out conventional surface activation process respectively at hydroxyapatite, bioactivity glass, aluminium oxide and the titanium oxide powder of 30～80nm, to satisfy the plasma spray coating process requirement.Being continuous gradient from biological stability to biological activity on the composition of bio-active gradient coating changes.Promptly be substrate with the metal prostheses, the composition of coating and quality percentage composition Changing Pattern thereof are as follows from inside to outside:
Hydroxyapatite nano-powder 40%～80% progressively increases progressively successively;
Bioactive glass nano powder 15%～5% progressively successively decreases successively;
Nanometer alumina powder 20%～5% progressively successively decreases successively;
TiOx nano powder body 25%～10% progressively successively decreases successively.
In the bio-active gradient coating preparation process, adopt the plasma spraying technology of full-automatic net energy control,, accurately control the conveying capacity and the plasma spray coating process parameter of various nano-powders according to the component requirement of above-mentioned gradient coating.Gradient coating thickness is that the porosity of about 100 μ m, face coat is 30%.The plasma spray coating process parameter is as follows: main gas: argon 70scfh; Inferior gas: hydrogen 5scfh; Spraying current: 400A; Spray voltage: 40V; Spray distance: 150mm.
Second step, assembling bioactie agent
(1) configuration contains the solution of bioactie agent
A, with 450 μ g bone morphogenetic proteins with the dissolving of 0.2g/dL guanidine hydrochloride solution after, guanidine hydrochloride is removed in the water dialysis, vibration shakes up and is configured to the bone morphogenetic protein suspension 1.5L that concentration is 300 μ g/L;
B, 12 μ g basic fibroblast growth factors are dissolved in deionized water after, vibration shakes up and is configured to the basic fibroblast growth factor suspension 1.5L that concentration is 8 μ g/L;
C, 45 μ g transforming growth factors are dissolved in deionized water after, vibration shakes up and is configured to the transforming growth factor suspension 1.5L that concentration is 30 μ g/L.
(2) above-mentioned a or b or c suspension are placed 37 ℃ calorstat low-speed oscillation after 5 minutes, the bio-active gradient coating material prepared step 1 immerses suspension, and under 37 ℃, constant temperature 2 hours takes out the vacuum draw lyophilization;
The 3rd step, artificial tooth root implantation body material that above-mentioned steps is prepared are standby after 3 hours with the epoxyethane fumigation sterilization.
Embodiment 2
Select for use root of the tooth that metal Ti 6Al7Nb processes a collection of Canis familiaris L. as matrix material, adopt the Praxair4550 plasma spraying equipment to prepare bio-active gradient coating.Utilize biological package technique that bone morphogenetic protein, transforming growth factor are assembled in the gradient coating surface then, make material have induced osteogenesis function and good biological activity.Its concrete preparation process is as follows:
The preparation of the first step, bio-active gradient coating
Particle size range is carried out conventional surface activation process respectively at hydroxyapatite, bioactivity glass, aluminium oxide and the titanium oxide powder of 30～80nm, to satisfy the plasma spray coating process requirement.Change from biological stability to bioactive continuous gradient on the composition of bio-active gradient coating.Promptly be substrate with the metal prostheses, the composition of coating and quality percentage composition degree Changing Pattern thereof are as follows from inside to outside:
Hydroxyapatite nano-powder 30%～65% progressively increases progressively successively
Bioactive glass nano powder 20%～10% progressively successively decreases successively
Nanometer alumina powder 10%～5% progressively successively decreases successively
TiOx nano powder body 40%～20% progressively successively decreases successively
In the bio-active gradient coating preparation process, adopt the plasma spraying technology of full-automatic net energy control,, accurately control the conveying capacity and the plasma spray coating process parameter of various nano-powders according to the component requirement of above-mentioned gradient coating.Gradient coating thickness is that the porosity of about 80 μ m, face coat is 20%.The plasma spray coating process parameter is as follows: main gas: argon 90scfh; Inferior gas: hydrogen 10scfh; Spraying current: 600A; Spray voltage: 55V; Spray distance: 100mm.
Second step, assembling bioactie agent
(1) 150 μ g bone morphogenetic proteins, 30 μ g transforming growth factors are added the vibration of 0.1mol/L phosphate buffered saline(PBS) and shake up, be configured to the suspension 1.5L of bone morphogenetic protein concentration 100 μ g/L, transforming growth factor concentration 20 μ g/L.
(2) above-mentioned suspension is placed 30 ℃ calorstat low-speed oscillation after 8 minutes, the bio-active gradient coating material prepared step 1 immerses suspension, and under 37 ℃, constant temperature took out the vacuum draw lyophilization after 5 hours;
The 3rd step, artificial tooth root implantation body material that step is prepared are standby after 3 hours with the epoxyethane fumigation sterilization.
Embodiment 3
Select for use root of the tooth that the pure titanium of metal processes a collection of Canis familiaris L. as matrix material, adopt the Praxair4550 plasma spraying equipment to prepare bio-active gradient coating.Utilize biological package technique that bone morphogenetic protein, basic fibroblast growth factor, transforming growth factor are assembled in the gradient coating surface then, make material have induced osteogenesis function and good biological activity.Its concrete preparation process is as follows:
The preparation of the first step, bio-active gradient coating
Particle size range is carried out conventional surface activation process respectively at hydroxyapatite, bioactivity glass, aluminium oxide and the titanium oxide powder of 30～80nm, to satisfy the plasma spray coating process requirement.Change from biological stability to bioactive continuous gradient on the composition of bio-active gradient coating.Promptly be substrate with the metal prostheses, the composition of coating and quality percentage composition Changing Pattern thereof are as follows from inside to outside:
Hydroxyapatite nano-powder 35%～70% progressively increases progressively successively
Bioactive glass nano powder 20%～15% progressively successively decreases successively
Nanometer alumina powder 15%～5% progressively successively decreases successively
TiOx nano powder body 30%～10% progressively successively decreases successively
In the bio-active gradient coating preparation process, adopt the plasma spraying technology of full-automatic net energy control,, accurately control the conveying capacity and the plasma spray coating process parameter of various nano-powders according to the component requirement of above-mentioned gradient coating.Gradient coating thickness is that the porosity of about 90 μ m, face coat is 25%.The plasma spray coating process parameter is as follows: main gas: argon 82scfh; Inferior gas: hydrogen 8scfh; Spraying current: 480A; Spray voltage: 50V; Spray distance: 120mm.
Second step, assembling bioactie agent
(1) 750 bone morphogenetic proteins, 75 μ g transforming growth factors are added the vibration of 0.1mol/L phosphate buffered saline(PBS) and shake up, and then add the suspension 1.5L that 15 μ g basic fibroblast growth factors are configured to bone morphogenetic protein concentration 500 μ g/L, transforming growth factor concentration 50 μ g/L, basic fibroblast growth factor concentration 10 μ g/L.
(2) above-mentioned suspension is placed 30 ℃ calorstat low-speed oscillation after 10 minutes, the bio-active gradient coating material prepared step 1 immerses, and under 37 ℃, constant temperature took out the vacuum draw lyophilization after 8 hours;
The 3rd step, artificial tooth root implantation body material that step is prepared are standby after 5 hours with the epoxyethane fumigation sterilization.
Embodiment 4
Select for use root of the tooth that metal Ti 6Al7Nb processes a collection of Canis familiaris L. as matrix material, adopt the Praxair4550 plasma spraying equipment to prepare bio-active gradient coating.Utilize biological package technique with transforming growth factor then, basic fibroblast growth factor is assembled in the gradient coating surface, makes material have induced osteogenesis function and good biological activity.Its concrete preparation process is as follows:
The preparation of the first step, bio-active gradient coating
Particle size range is carried out conventional surface activation process respectively at hydroxyapatite, bioactivity glass, aluminium oxide and the titanium oxide powder of 30～80nm, to satisfy the plasma spray coating process requirement.Change from biological stability to bioactive continuous gradient on the composition of bio-active gradient coating.Promptly be substrate with the metal prostheses, the composition of coating and quality percentage composition graded rule thereof are as follows from inside to outside:
Hydroxyapatite nano-powder 30%～60% progressively increases progressively successively
Bioactive glass nano powder 20%～12% progressively successively decreases successively
Nanometer alumina powder 15%～8% progressively successively decreases successively
TiOx nano powder body 35%～20% progressively successively decreases successively
In the bio-active gradient coating preparation process, adopt the plasma spraying technology of full-automatic net energy control,, accurately control the conveying capacity and the plasma spray coating process parameter of various nano-powders according to the component requirement of above-mentioned gradient coating.Gradient coating thickness is that the porosity of about 78 μ m, face coat is 22%.The plasma spray coating process parameter is as follows: main gas: argon 85scfh; Inferior gas: hydrogen 10scfh; Spraying current: 580A; Spray voltage: 60V; Spray distance: 110mm.
Second step, assembling bioactie agent
(1) 15 μ g transforming growth factors, 3 μ g basic fibroblast growth factors are added deionized water solution vibration and shake up, be configured to transforming growth factor concentration 10 μ g/L, basic fibroblast growth suspension 1.5L because of concentration 2 μ g/L.
(2) above-mentioned suspension is placed 30 ℃ calorstat low-speed oscillation after 6 minutes, the bio-active gradient coating material prepared step 1 immerses, and under 37 ℃, constant temperature took out the vacuum draw lyophilization after 3 hours;
The 3rd step, artificial tooth root implantation body material that step is prepared are standby after 3 hours with the epoxyethane fumigation sterilization.
Claims (4)
1, a kind of induced osteogenesis artificial tooth root with bioactivity implantation body material is characterized in that:
(1) be matrix with the good metal of biocompatibility, metal base surface prepares bioactivity coatings;
(2) on the structure from densification to porous, be the bio-active gradient coating that continuous gradient changes from biological stability to biological activity on the composition, its coating layer thickness is that the porosity of 80～100 μ m, face coat is 20～30%;
(3) composition of gradient coating and quality percentage composition thereof are hydroxyapatite nano-powder 30～80%, bioactive glass nano powder 5～20%, nanometer alumina powder 5～20% and TiOx nano powder body 10～40%;
(4) the gradient coating surface-assembled bone morphogenetic protein is arranged or/and basic fibroblast growth factor or/and transforming growth factor.
2, a kind of induced osteogenesis artificial tooth root with bioactivity implantation body preparation methods, comprise the plasma spraying technology that adopts full-automatic net energy control, the metal base surface good at biocompatibility prepares bioactivity coatings, the composition and the structure that it is characterized in that bioactivity coatings all are the continuous gradient variation, and the bioactivity coatings surface-assembled has bioactie agent, and concrete steps are as follows:
The preparation of step 1, bio-active gradient coating
(1) composition of gradient coating and quality percentage composition adjusting range thereof are as follows:
Hydroxyapatite nano-powder 30～80%,
Bioactive glass nano powder 5～20%,
Nanometer alumina powder 5～20%,
TiOx nano powder body 10～40%;
(2) particle size range of above-mentioned nano-powder is 30～80nm, and need carry out conventional surface activation process;
(3) according to the prescription and the requirement of above-mentioned gradient coating material, accurately control the conveying capacity and the plasma spray coating process parameter of various nano-powders, gradient coating thickness is that the porosity of 80～100 μ m, face coat is 20～30%; The plasma spray coating process parameter is as follows: main gas: argon 70～90scfh, inferior gas: hydrogen 5～10scfh, spraying current: 400～600A, spray voltage: 30～60V, spray distance: 100～150mm;
Step 2, assembling bioactie agent
(1) a kind of in bone morphogenetic protein, basic fibroblast growth factor, the transforming growth factor or two kinds or three kinds of bioactie agents are dissolved in solvent, make the concentration range of bioactie agent in the corresponding solution as follows: bone morphogenetic protein 0～500 μ g/L, basic fibroblast growth factor 0～10 μ g/L, transforming growth factor 0～50 μ g/L;
(2) will contain bioactie agent solution places 30～37 ℃ calorstat low-speed oscillation after 5～10 minutes, the prepared bio-active gradient coating material of step 1 is immersed in this solution, kept 2～8 hours, take out vacuum draw lyophilization, sterilization then, obtain having the artificial tooth root with bioactivity implantation body material of induced osteogenesis function.
3, a kind of induced osteogenesis artificial tooth root with bioactivity according to claim 2 implantation body preparation methods is characterized in that with the metal prostheses being substrate, and the rule of coating composition distribution gradient is from inside to outside:
Hydroxyapatite nano-powder 30～80% is progressively and increases progressively;
Bioactive glass nano powder 20～5% is progressively and successively decreases;
Nanometer alumina powder 20～5% is progressively and successively decreases;
TiOx nano powder body 40～10% is progressively and successively decreases.
4, a kind of induced osteogenesis artificial tooth root with bioactivity according to claim 2 implantation body preparation methods, it is characterized in that working as three kinds of bioactie agents is that bone morphogenetic protein, basic fibroblast growth factor, transforming growth factor are dissolved in solvent simultaneously, make in the solution concentration range of bioactie agent as follows: bone morphogenetic protein 100～500 μ g/L, basic fibroblast growth factor 2～10 μ g/L, transforminggrowthfactor-0～50 μ g/L.
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Families Citing this family (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1325124C (en) * | 2003-11-21 | 2007-07-11 | 王岩 | Artificial biological prothesis, and its prepn. method |
| SE526749C2 (en) * | 2003-12-11 | 2005-11-01 | Nobel Biocare Ab | Dental implant device and method for its preparation |
| JP2005270371A (en) * | 2004-03-25 | 2005-10-06 | Gc Corp | Implant made of titanium or titanium alloy and its surface treating method |
| CN100353921C (en) * | 2005-07-28 | 2007-12-12 | 曹征旺 | Method for preparing implantation body possessing biological activity inside root of tooth |
| CN101878006B (en) * | 2007-11-28 | 2017-04-12 | 3M创新有限公司 | Digitally-painted dental articles |
| EP2227172B1 (en) | 2007-11-28 | 2018-04-18 | 3M Innovative Properties Company | Fabrication of dental articles using digitally-controlled reductive and digitally-controlled additive processes |
| CN101766840B (en) * | 2009-12-31 | 2012-10-24 | 东南大学 | Antibacterial functionalized artificial joint with silver-loaded nanotube array surface |
| 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 |
| CN102038556B (en) * | 2010-12-15 | 2013-07-31 | 中国人民解放军第四军医大学 | Bone stretching dental implant |
| CN112933292B (en) * | 2021-01-25 | 2021-10-12 | 天琪(广东)科技发展有限公司 | Modified dental implant and preparation method thereof |
| CN113636868B (en) * | 2021-08-19 | 2023-08-04 | 北京大学口腔医学院 | Surface coating method of zirconia ceramic implant material and application thereof |
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