CN102230206B - Surface treatment method of titanium implant suitable for bone growth - Google Patents
Surface treatment method of titanium implant suitable for bone growth Download PDFInfo
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- CN102230206B CN102230206B CN201110147488.7A CN201110147488A CN102230206B CN 102230206 B CN102230206 B CN 102230206B CN 201110147488 A CN201110147488 A CN 201110147488A CN 102230206 B CN102230206 B CN 102230206B
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Abstract
The invention discloses a surface treatment method of a titanium implant suitable for bone growth, preparing a film with multi-sized apertures suitable for bone growth on the surface of the titanium implant. The method comprises the following steps: putting the titanium implant in a silicate or phosphate electrolytic solution in an oxidation tank to join up with the power anode in parallel, connecting the power cathode with a stainless steel, controlling electrical parameters to prepare a TiO2 film, changing the electrolyte into soda ash, and controlling the electrical parameters to obtain a needed film. The treated titanium implant by the method disclosed in the invention fully satisfies the using requirement of human body, and can solve the problem of full growth of bone tissue on the surface of the titanium implant.
Description
Technical field
The invention belongs to titanium or titanium alloy implant surface treatment process technical field, be specifically related to a kind of surface treatment method of titanium implant that is suitable for bone growth.
Background technology
Due to the continuous improvement of social progress and medical conditions, people's life-span constantly extends, and therefore, exploitation can substitute those bio-medical materials that lost the tissue of physiological function and exercised its function and become more and more important.Planting body is a kind of as bio-medical material, is mainly used in substituting human body hard tissue damaged, disappearance, and exercises its function.Therefore, require it nontoxic, harmless, non-stimulated to human body, can stimulate the formation of new bone and fully grow on the surface of planting body.Titanium and titanium alloy are current most widely used planting body materials, and it has good mechanical mechanics and biocompatibility, but titanium and titanium alloy do not possess the induced osteogenesis cell in its epontic ability.How making after the titanium implanting to human body to be combined with bone forming is an emphasis of titanium implant surface modification.The form of implant surface is influential to the activity performance of biomaterial, porous surface can promote cell tissue and material surface adhere to and combine closely, porous surface has not only increased the contact area of planting body and surrounding tissue, and can preferentially attach scleroblast, make its activity obtain larger performance, and can make the newborn skeletonization porous surface of growing into.Research shows, more than the aperture that is suitable for the implant surface vesicular structure that osseous tissue will grow reaches 50uM.
Summary of the invention
The purpose of this invention is to provide a kind of surface treatment method of titanium implant that is suitable for bone growth, can generate in implant surface the ceramic layer of porous, its aperture, more than 50uM, has solved the problem that osseous tissue can not fully be grown in implant surface.
The technical solution adopted in the present invention is, a kind of surface treatment method of titanium implant that is suitable for bone growth, its operation steps is: first titanium implant is put into to silicate or the phosphoric acid salt electrolytic solution in oxidation trough and connect the positive pole that differential arc oxidation is controlled power supply, the negative pole of power supply connects stainless steel; Control power supply by differential arc oxidation titanium implant is applied to pulsed voltage 2 minutes, control voltage is 400V, and dutycycle is 8%, and frequency is 100HZ; Change silicate or phosphoric acid salt electrolytic solution into alkali lye again, control power supply by differential arc oxidation titanium implant is applied to pulsed voltage 1 minute, control voltage is 300V, and dutycycle is 20%, and frequency is 100HZ; By after above-mentioned steps in titanium implant surface growth in situ one deck porous and be suitable for the ceramic layer that osseous tissue is fully grown.
Wherein, the silicate electrolytic solution by weight with the cumulative volume ratio, by the water glass of 10～15g/L and the sodium carbonate of 3～8g/L, formed, solvent is distilled water.
Wherein, the phosphoric acid salt electrolytic solution for by weight with the cumulative volume ratio, by the sodium β-glycerophosphate of 8～20g/L and the lime acetate of 15～30g/L, solvent is distilled water.
Wherein, alkaline solution by weight with cumulative volume than being the potassium hydroxide of 20g/L, solvent is distilled water.
The invention has the beneficial effects as follows, because the present invention is by the control of the electrical parameter in the different time scope (voltage, dutycycle, frequency), regulate electrolyte prescription and the power supply output energy in two stages, thereby prepare the titanium implant surface of aperture more than 50uM, the titanium implant of processing through method disclosed by the invention has met the service requirements in human body fully, can solve the problem that osseous tissue is fully grown in implant surface.
The accompanying drawing explanation
Fig. 1 is the surface topography scanned photograph of titanium implant after the silicate electrolyte test in the embodiment of the present invention 1;
Fig. 2 is the preparation method that utilizes the embodiment of the present invention 1 to provide in the surface topography scanned photograph of the ceramic layer of the final growth of titanium implant surface (magnification be 80 *);
Fig. 3 is the preparation method that utilizes the embodiment of the present invention 1 to provide in the surface topography scanned photograph of the ceramic layer of the final growth of titanium implant surface (magnification be 650 *);
Fig. 4 is the ceramic layer XRD phase composition collection of illustrative plates prepared at titanium implant surface in the embodiment of the present invention 1;
Fig. 5 is the surface topography scanned photograph of titanium implant after the test of phosphoric acid salt electrolytic solution in the embodiment of the present invention 3;
Fig. 6 is the preparation method that utilizes the embodiment of the present invention 3 to provide in the surface topography scanned photograph of the ceramic layer of the final growth of titanium implant surface (magnification be 80 *);
Fig. 7 is the preparation method that utilizes the embodiment of the present invention 3 to provide in the surface topography scanned photograph of the ceramic layer of the final growth of titanium implant surface (magnification be 1200 *);
Fig. 8 is the ceramic layer XRD phase composition collection of illustrative plates prepared at titanium implant surface in the embodiment of the present invention 3.
Embodiment
Below in conjunction with the drawings and specific embodiments, the present invention is described in detail.
Embodiment 1
A kind of surface treatment method of titanium implant that is suitable for bone growth comprises the following steps:
First configuration silicate electrolytic solution in oxidation trough, the silicate electrolytic solution by weight with the cumulative volume ratio, by the water glass of 10g/L and the sodium carbonate of 8g/L, formed, its solvent is distilled water, the pH value of the electrolytic solution prepared is 10-12; Then titanium implant is immersed in the silicate electrolytic solution prepared, titanium implant connects the positive pole that differential arc oxidation is controlled power supply, the negative pole of power supply connects stainless steel plate, control power supply by differential arc oxidation titanium implant is applied to pulsed voltage 2 minutes, control voltage is 400V, dutycycle is 8%, and frequency is 100HZ.The titanium implant that is placed in the silicate electrolytic solution will form rapidly one deck titanium oxide ceramics layer as thin as a wafer in the moment of energising, under the highfield effect produced at voltage, weakness zone in the titanium oxide ceramics layer is punctured the formation discharge channel simultaneously, the silicate electrolytic solution is injected in discharge channel, simultaneously in high temperature action, the titanium of melting breaks away from and also enters into discharge channel from matrix, Plasma chemical reaction occurs subsequently in passage, the product TiO in reaction
2be deposited on the inwall and near surface porthole of discharge channel, cause like this formation the thickening gradually of the titanium oxide ceramics layer of porous.As shown in Figure 1, detect the microscopic appearance of titanium implant surface by scanning electronic microscope, the titanium oxide ceramics layer of titanium implant surface has been covered with the micropore that a large amount of diameters are 1～3uM, and it is formed that these holes are that titanium implant surface produces a large amount of micro-arc discharges.
Change the silicate electrolytic solution in oxidation trough into alkali lye again, alkali lye by weight with cumulative volume than being the potassium hydroxide of 20g/L, its solvent is distilled water; Control power supply by differential arc oxidation titanium implant is applied to pulsed voltage 1 minute, control voltage is 300V, and dutycycle is 20%, and frequency is 100HZ.
By above step in titanium implant surface growth in situ one deck porous and be suitable for the ceramic layer that osseous tissue is fully grown, as shown in Figure 2, the hole that to be covered with aperture be 50～100uM on the final ceramic layer surface formed, this is while due to electrolytic solution, being KOH, rete does not occur and thickens reaction in differential arc oxidation, but electrochemical dissolution occurs.Titanium implant has generated TiO in silicate electrolyte
2dielectric ceramic layer has formed " metal-insulator layer-electrolytic solution (titanium matrix-TiO when differential arc oxidation in KOH solution
2ceramic layer-alkali lye) " three-phase system, the ceramic layer of titanium implant surface is breakdown and the electric discharge arc light occurs, and KOH, under the effect of pressurization electric discharge, punctures place to TiO at arc light
2ceramic layer produces electrochemical dissolution, has caused surface topography as shown in Figure 2 to occur.As shown in Figure 3, it is that single micropore amplifies scanned photograph of 650 times, aperture be about 65uM be suitable for osteocyte within it section seek connections with growth.
Fig. 4 is the XRD phase composition collection of illustrative plates of the ceramic layer for preparing at titanium implant surface of the present embodiment, and figure can find out thus, and the composition of ceramic layer is TiO
2, have biocompatibility to human body without injury.
Embodiment 2
A kind of surface treatment method of titanium implant that is suitable for bone growth comprises the following steps:
First configuration silicate electrolytic solution in oxidation trough, the silicate electrolytic solution by weight with the cumulative volume ratio, by the water glass of 15g/L and the sodium carbonate of 3g/L, formed, its solvent is distilled water, the pH value of the electrolytic solution prepared is 10-12; Then titanium implant is immersed in the silicate electrolytic solution prepared, titanium implant connects the positive pole that differential arc oxidation is controlled power supply, the negative pole of power supply connects stainless steel plate, control power supply by differential arc oxidation titanium implant is applied to pulsed voltage 2 minutes, control voltage is 400V, dutycycle is 8%, and frequency is 100HZ.
Change the silicate electrolyte in oxidation trough into alkali lye again, alkali lye by weight with cumulative volume than being the potassium hydroxide of 20g/L, its solvent is distilled water; Control power supply by differential arc oxidation titanium implant is applied to pulsed voltage 1 minute, control voltage is 300V, and dutycycle is 20%, and frequency is 100HZ.
By above-mentioned steps in titanium implant surface growth in situ one deck porous and be suitable for the ceramic layer that osseous tissue is fully grown.
Embodiment 3
A kind of surface treatment method of titanium implant that is suitable for bone growth comprises the following steps:
First configuration phosphoric acid salt electrolytic solution in oxidation trough, the phosphoric acid salt electrolytic solution by weight with the cumulative volume ratio, by the sodium β-glycerophosphate of 8g/L and the lime acetate of 15g/L, formed, its solvent is distilled water, the pH value of the electrolytic solution prepared is 10-12; Then titanium implant is immersed in the phosphoric acid salt electrolytic solution prepared, titanium implant connects the positive pole that differential arc oxidation is controlled power supply, power cathode connects stainless steel plate, control power supply by differential arc oxidation titanium implant is applied to pulsed voltage 2 minutes, control voltage is 400V, dutycycle is 8%, and frequency is 100HZ.The titanium implant that is placed in the phosphoric acid salt electrolytic solution will form rapidly one deck titanium oxide ceramics layer as thin as a wafer in the moment of energising, under the highfield effect produced at voltage, weakness zone in the titanium oxide ceramics layer is punctured the formation discharge channel simultaneously, the phosphoric acid salt electrolytic solution is injected in discharge channel, simultaneously in high temperature action, the titanium of melting breaks away from and also enters into discharge channel from matrix, Plasma chemical reaction occurs subsequently in passage, the product TiO in reaction
2be deposited on the inwall and near surface porthole of discharge channel, cause like this formation the thickening gradually of the titanium oxide ceramics layer of porous.As shown in Figure 5, detect the microscopic appearance of titanium implant surface by scanning electronic microscope, the titanium oxide ceramics layer of titanium implant surface has been covered with the micropore that a large amount of diameters are 1～3uM, and it is formed that these holes are that titanium implant surface produces a large amount of micro-arc discharges.
Change the phosphoric acid salt electrolytic solution in oxidation trough into alkali lye again, alkali lye by weight with cumulative volume than being the potassium hydroxide of 20g/L, its solvent is distilled water; Control power supply by differential arc oxidation titanium implant is applied to pulsed voltage 1 minute, control voltage is 300V, and dutycycle is 20%, and frequency is 100HZ.
By above step in titanium implant surface growth in situ one deck porous and be suitable for the ceramic layer that osseous tissue is fully grown, as shown in Figure 6, the hole that to be covered with aperture be 50～100uM on the final ceramic layer surface formed, this is while due to electrolytic solution, being KOH, rete does not occur and thickens reaction in differential arc oxidation, but electrochemical dissolution occurs.Titanium implant has generated TiO in phosphoric acid salt electrolytic solution
2dielectric ceramic layer has formed " metal-insulator layer-electrolytic solution (titanium matrix-TiO when differential arc oxidation in KOH solution
2ceramic layer-alkali lye) " three-phase system, the ceramic layer of titanium implant surface is breakdown and the electric discharge arc light occurs, and KOH, under the effect of pressurization electric discharge, punctures place to TiO at arc light
2ceramic layer produces electrochemical dissolution, has caused surface topography as shown in Figure 6 to occur.As shown in Figure 7, it is that single micropore amplifies scanned photograph of 1200 times, aperture be about 65uM be suitable for osteocyte within it section seek connections with growth.
Fig. 8 is the XRD phase composition collection of illustrative plates of the ceramic layer for preparing at titanium implant surface of the present embodiment, and figure can find out thus, and the composition of ceramic layer is TiO
2, have biocompatibility to human body without injury.
Embodiment 4
A kind of surface treatment method of titanium implant that is suitable for bone growth comprises the following steps:
First configuration phosphoric acid salt electrolytic solution in oxidation trough, the phosphoric acid salt electrolytic solution by weight with the cumulative volume ratio, by the sodium β-glycerophosphate of 20g/L and the lime acetate of 30g/L, formed, its solvent is distilled water, the pH value of the electrolytic solution prepared is 10-12; Then titanium implant is immersed in the phosphoric acid salt electrolytic solution prepared, titanium implant connects the positive pole that differential arc oxidation is controlled power supply, power cathode connects stainless steel plate, control power supply by differential arc oxidation titanium implant is applied to pulsed voltage 2 minutes, control voltage is 400V, dutycycle is 8%, and frequency is 100HZ.
Change the phosphoric acid salt electrolytic solution in oxidation trough into alkali lye again, alkali lye by weight with cumulative volume than being the potassium hydroxide of 20g/L, its solvent is distilled water; Control power supply by differential arc oxidation titanium implant is applied to pulsed voltage 1 minute, control voltage is 300V, and dutycycle is 20%, and frequency is 100HZ.
By above step in titanium implant surface growth in situ one deck porous and be suitable for the ceramic layer that osseous tissue is fully grown.
Claims (2)
1. a surface treatment method of titanium implant that is suitable for bone growth, it is characterized in that, its operation steps is: first titanium implant is put into to silicate or the phosphoric acid salt electrolytic solution in oxidation trough and connect the positive pole that differential arc oxidation is controlled power supply, the negative pole of power supply connects stainless steel; Control power supply by differential arc oxidation titanium implant is applied to pulsed voltage 2 minutes, control voltage is 400V, and dutycycle is 8%, and frequency is 100HZ; Change silicate or phosphoric acid salt electrolytic solution into alkali lye again, control power supply by differential arc oxidation titanium implant is applied to pulsed voltage 1 minute, control voltage is 300V, and dutycycle is 20%, and frequency is 100HZ; By after above-mentioned steps in titanium implant surface growth in situ one deck porous and be suitable for the ceramic layer that osseous tissue is fully grown;
Described silicate electrolytic solution by weight with the cumulative volume ratio, by the water glass of 10～15g/L and the sodium carbonate of 3～8g/L, formed, solvent is distilled water; Described phosphoric acid salt electrolytic solution for by weight with the cumulative volume ratio, by the sodium β-glycerophosphate of 8～20g/L and the lime acetate of 15～30g/L, solvent is distilled water.
2. surface treatment method of titanium implant according to claim 1 is characterized in that: described alkaline solution for by weight with cumulative volume than being the potassium hydroxide of 20g/L, solvent is distilled water.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1147625C (en) * | 2002-03-01 | 2004-04-28 | 西安交通大学 | Porous nano titanium oxide base heterogeneous bioactive surface and its preparing process |
| CN100557087C (en) * | 2006-09-30 | 2009-11-04 | 中南大学 | Differential arc oxidation prepares K 2Ti 6O 13Coating and K 2Ti 6O 13The method of/HAp bioceramic film |
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| CN1147625C (en) * | 2002-03-01 | 2004-04-28 | 西安交通大学 | Porous nano titanium oxide base heterogeneous bioactive surface and its preparing process |
| CN100557087C (en) * | 2006-09-30 | 2009-11-04 | 中南大学 | Differential arc oxidation prepares K 2Ti 6O 13Coating and K 2Ti 6O 13The method of/HAp bioceramic film |
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