Zirconium oxide sand blasting implant surface treatment method

Abstract

The invention discloses a zirconium oxide sand blasting implant surface treatment method which comprises the following steps: carrying out sand blasting treatment on the implant surface by using crystallized zirconium oxide particles to form primary holes in the implant surface; then carrying out acid etching treatment on the implant with the first-level holes to form second-level holes in the surface of the implant, and respectively putting the implant with the second-level holes in absolute ethyl alcohol and deionized water for ultrasonic cleaning for 10 minutes; and finally, carrying out alkali heat treatment on the implant to finish the surface treatment of the implant. According to the method, zirconia particles with high biocompatibility and high strength after crystallization are used for carrying out sand blasting treatment on the implant, deeper first-level holes are formed, zirconia is helpful for osteogenesis, and sand blasting particle residues do not need to be worried about. The sand blasting particles do not need to be thoroughly removed through long-time acid etching, and the acid etching plays a role in removing the sand blasting particles while obtaining a secondary hole structure; the zirconia sand blasting implant is good in biocompatibility and has a growth promoting effect on MG63 osteoblastoma cells.

Description

Technical Field

[0001] The present invention relates to the technical field of implant surface treatment, and specifically to a treatment method for the surface of a zirconia-blasted implant. Background Art

[0002] The surface topography of dental implants is one of the important factors affecting bone bonding. It has been found that the bone bonding strength of titanium implants with a multi-level pore structure is greater than that of implants with a smooth surface. The existing sandblasting and acid etching surface treatment technology (SLA) uses large sandblasting particles to sandblast the surface of the implant to form primary pores; then strong acid etching is used to form secondary pores on the surface of the implant to further increase the surface roughness of the implant.

[0003] However, existing implants generally use alumina for sandblasting treatment. Because the hardness of alumina is relatively low, problems such as uneven pore structure, lack of multi-level pore structure, or residual sandblasting particles are likely to occur, and good bone bonding cannot be formed. Summary of the Invention

[0004] The purpose of the present invention is to overcome the deficiencies of the prior art and provide a treatment method for the surface of a zirconia-blasted implant. This method has a simple process, and the surface of the treated implant has good biocompatibility.

[0005] The technical solution for achieving the purpose of the present invention is as follows: A treatment method for the surface of a zirconia-blasted implant includes the following steps: 1) Use crystallized zirconia particles to sandblast the surface of the implant to form primary pores on the surface of the implant; 2) Acid-etch the implant with primary pores obtained in step 1) to form secondary pores on the surface of the implant, and ultrasonically clean the implant with secondary pores formed in absolute ethanol and deionized water for 10 minutes respectively; 3) After performing alkali heat treatment on the implant obtained in step 2), the surface treatment of the implant is completed.

[0006] In step 1), the crystallization is to crush spherical yttrium-stabilized zirconia with a particle size of 1-3 mm, filter it with 25-mesh and 50-mesh sieves to obtain irregular zirconia particles with a particle size of 0.3 mm - 0.7 mm, and then place the zirconia particles in a muffle furnace at 700 °C for heat preservation for 24 h to obtain stable m-ZrO2 particles.

[0007] The zirconia particles are amorphous zirconia particles, tetragonal zirconia particles, or cubic zirconia particles.

[0008] In step 1), for the sandblasting treatment, the treatment process is as follows: the angle between the spray gun and the implant is 30 - 60°, the distance between the muzzle of the gun and the implant is 5 - 12 mm, and the sandblasting time is 10 - 20 s; preferably, the angle between the spray gun and the implant is 45°, the distance between the muzzle of the gun and the implant is 8 mm, and the sandblasting time is 15 s.

[0009] In step 2), for the acid etching treatment, the implant is placed in an etching solution at 90 - 100 °C for 3 - 5 min; preferably, it is placed in an etching solution at 95 °C for 5 min.

[0010] The etching solution is at least one of HF, HNO3, H2SO4, and HCl solutions; preferably, the etching solution is a mixed solution of H2SO4, HCl, and water with a volume ratio of 1:1:2.

[0011] In step 3), for the alkali heat treatment, the implant is immersed in an alkali solution at 1 - 10 mol / L and 15 - 65 °C for 2 - 24 h; preferably, it is immersed in an alkali solution at 5 mol / L and 65 °C for 24 h.

[0012] The alkali solution is one of sodium hydroxide solution, sodium carbonate solution, or sodium bicarbonate solution.

[0013] A method for treating the surface of a zirconia sandblasted implant provided by the present invention. This method uses crystallized zirconia to perform sandblasting treatment on the implant surface. It can not only avoid the sandblasting particles remaining on the implant surface that are difficult to remove after sandblasting, but also form deeper and more uniform primary pores. After acid etching treatment, it can not only remove the zirconia on the implant surface, but also form secondary pores on the implant surface. The formation of primary pores and secondary pores increases the surface area of the implant and promotes the adhesion and differentiation of osteoblasts that adhere to the wall and grow on the implant surface; and after using zirconia to sandblast the implant surface, it has a growth promoting effect on MG63 osteosarcoma cells. Description of the Drawings

[0014] Figure 1 Scanning electron microscope image of the implant surface after treatment in Example 1; Figure 2 Scanning electron microscope image of the implant surface after treatment in Example 2; Figure 3 Scanning electron microscope image of the implant surface after treatment in Example 3; Figure 4 Energy spectrum diagram of the implant after treatment in Example 1; Figure 5 Energy spectrum diagram of the implant after treatment in Example 2; Figure 6 Energy spectrum diagram of the implant after treatment in Example 3. Embodiment

[0015] The following further elaborates on the content of the present invention in conjunction with the accompanying drawings and embodiments, but does not limit the present invention. Example

[0016] A method for treating the surface of a zirconia sandblasted implant includes the following steps: 1) Crush spherical yttria-stabilized zirconia with a particle size of 1 - 3 mm, filter it using 25-mesh and 50-mesh sieves to obtain irregular zirconia particles with a particle size of 0.3 mm - 0.7 mm. Then place the zirconia particles in a muffle furnace at 700 °C for heat preservation for 24 h to obtain stable m-ZrO2 particles; use the m-ZrO2 particles to perform sandblasting treatment on the implant surface to form primary holes on the implant surface; where the angle between the spray gun and the implant is 45°, the distance between the muzzle and the implant is 8 mm, and the sandblasting time is 15 s; 2) Place the implant with primary holes obtained in step 1) in a corrosion solution at 95 °C for 5 min to form secondary holes on the implant surface, and ultrasonically clean the implant with secondary holes formed in absolute ethanol and deionized water for 10 min respectively. The corrosion solution is a mixed solution of H2SO4, HCl, and water mixed evenly in a volume ratio of 1:1:2; 3) Immerse the implant obtained in step 2) in a 5 mol / L sodium hydroxide solution at 65 °C for 24 h, and then the surface treatment of the implant is completed.

[0017] Perform performance tests on the implant with the above surface treatment completed. The obtained SEM images and energy spectrum diagrams of the implant surface are respectively as Figure 1 and Figure 4 shown. Example

[0018] Use non-crystallized zirconia particles to perform sandblasting treatment on the implant surface, and then process the sandblasted implant according to the operations in steps 2) and 3) of Example 1. Perform performance tests on the processed implant. The obtained SEM images and energy spectrum diagrams of the implant surface are as Figure 2 and Figure 5 shown. Example

[0019] Use alumina particles to perform sandblasting treatment on the implant surface, and then process the sandblasted implant according to the operations in steps 2) and 3) of Example 1. Perform performance tests on the processed implant. The obtained SEM images and energy spectrum diagrams of the implant surface are as Figure 3 and Figure 6 shown.

[0020] According to the above performance test results, it can be seen that: Comparing Comparative Example 1 with Example 2, it can be seen that only the high-strength zirconia particles after crystallization can form first-level pores with larger sizes on the surface of the implant. These first-level pores are similar in size to human osteoblasts, which is beneficial for cell attachment.

[0021] 2. Comparing Comparative Example 1 with Example 3, it can be seen that for the implant sandblasted with ordinary alumina particles, after acid etching and cleaning, there are no obvious first-level pores on the surface, and energy spectrum analysis shows that there are still alumina sandblasting particles remaining on the surface of the implant, which may affect the bonding between the implant and bone.

Claims

1. A treatment method for the surface of a zirconia sandblasted implant, characterized in that, It includes the following steps: 1) Use the crystallized zirconia particles to perform sandblasting treatment on the surface of the implant, so that primary pores are formed on the surface of the implant; 2) Perform acid etching treatment on the implant with primary pores in step 1), so that secondary pores are formed on the surface of the implant, and the implants after the formation of secondary pores are respectively ultrasonically cleaned in absolute ethanol and deionized water for 10 min; 3) After performing alkali heat treatment on the implant obtained in step 2), the surface treatment of the implant is completed.

2. The treatment method for the surface of a zirconia sandblasted implant according to claim 1, characterized in that, In step 1), the crystallization is to crush spherical yttrium-stabilized zirconia with a particle size of 1-3 mm, filter it with 25-mesh and 50-mesh sieves, obtain irregular zirconia particles with a particle size of 0.3 mm-0.7 mm, and then place the zirconia particles in a muffle furnace at 700 °C for heating and heat preservation for 24 h to obtain stable m-ZrO2 particles; The zirconia particles are amorphous zirconia particles, tetragonal zirconia particles, or cubic zirconia particles.

3. The treatment method for the surface of a zirconia sandblasted implant according to claim 1, characterized in that, In step 1), the sandblasting treatment process is as follows: the angle between the spray gun and the implant is 30-60°, the distance between the nozzle and the implant is 5-12 mm, and the sandblasting time is 10-20 s.

4. The treatment method for the surface of a zirconia sandblasted implant according to claim 3, characterized in that, The angle between the spray gun and the implant is 45°, the distance between the nozzle and the implant is 8 mm, and the sandblasting time is 15 s.

5. The treatment method for the surface of a zirconia sandblasted implant according to claim 1, characterized in that, In step 2), the acid etching treatment is to immerse the implant in a corrosion solution at 90-100 °C for 3-5 min.

6. The treatment method for the surface of a zirconia sandblasted implant according to claim 5, characterized in that, The acid etching treatment is to immerse it in a corrosion solution at 95 °C for 5 min.

7. The treatment method for the surface of a zirconia sandblasted implant according to claim 1, characterized in that, The corrosion solution is at least one of HF, HNO3, H2SO4, and HCl solutions.

8. The treatment method for the surface of a zirconia sandblasted implant according to claim 7, characterized in that, The corrosion solution is a mixed solution of H2SO4, HCl, and water with a volume ratio of 1:1:

2.

9. The treatment method for the surface of a zirconia sandblasted implant according to claim 1, characterized in that, In step 3), the alkali heat treatment is to immerse the implant in an alkali solution with a concentration of 1-10 mol / L and a temperature of 15-65 °C for 2-24 h.

10. The treatment method for the surface of a zirconia sandblasted implant according to claim 9, characterized in that, The alkali heat treatment is to immerse it in an alkali solution with a concentration of 5 mol / L and a temperature of 65 °C for 24 h; The alkali solution is one of sodium hydroxide solution, sodium carbonate solution, or sodium bicarbonate solution.

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