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Method for preparing titanium dioxide layer with multi-level pore structure on surface of medicinal titanium

A technology of titanium dioxide and hierarchical pores, which is applied in the field of preparing a titanium dioxide layer with a hierarchical porous structure on the surface of medical titanium, can solve the problems of reducing the dissolution and release of metal titanium ions, insufficient coarsening, and small surface roughness, etc. The effect of new bone formation, simple preparation process, and easy operation

Inactive Publication Date: 2010-10-27
SICHUAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Various surface treatment methods have their own advantages and disadvantages, and there are few research literatures on the horizontal comparison of various methods
However, the outstanding advantage of the anodic oxidation method is that it can generate a titanium oxide layer on the surface in situ, which can effectively reduce the dissolution and release of metal titanium ions, and can treat implants with irregular shapes. The disadvantage is that the surface roughness Small, not coarse enough

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Example 1: A pure titanium sheet (TA2) with a size of 10×10×1mm was polished and polished with 400#, 600#, and 800# metallographic sandpaper successively, and then ultrasonically cleaned with acetone, absolute ethanol and deionized water for 5 minutes respectively ; In the 2M acetic acid electrolyte, the sample is anodized, using a slow uniform speed up-flow mode, that is, from 5mA / cm 2 Rise to 50mA / cm 2 Hold for 2min at each current density, with a step of 5mA / cm 2 , Co-anodized for 20min. . Then carry out secondary anodic oxidation treatment in 1M sodium acetate electrolyte, adopt constant voltage mode, preset voltage value is 150V, keep 2min after reaching preset voltage value. Under the scanning electron microscope, you can see the staggered groove-like porous structure at low magnification. The width of the groove is 20-30 microns. About 0.4 microns. X-ray diffraction analysis shows that the surface oxide film is composed of anatase and rutile titanium dioxide...

Embodiment 2

[0022] Embodiment 2: the pure titanium sheet (TA2) that diameter is 15mm is polished with 400#, 600#, 800# metallographic sandpaper successively, then with acetone, absolute ethanol, deionized water ultrasonic cleaning 5min respectively; In the acetic acid electrolyte, the sample was anodized, and the mode of slow uniform flow was adopted, that is, from 5mA / cm 2 Rise to 50mA / cm 2 Hold for 3min at each current density, with a step of 5mA / cm 2 , total anodizing for 30min. Then carry out secondary anodic oxidation treatment in 1M sulfuric acid electrolyte, adopt constant voltage mode, preset voltage value is 180V, keep 1min after reaching preset voltage value. Observation by scanning electron microscope, under low magnification, you can see the staggered groove-like porous structure, the groove width is 20-30 microns, and under high magnification, you can see the sub-micron microporous structure densely distributed on the entire surface, with a pore size of 0.8- 1.0 microns or...

Embodiment 3

[0023] Embodiment 3: The TA16V4 (TC4) whose size is 20×10×1mm is polished and polished with 400#, 600#, and 800# metallographic sandpaper successively, and then ultrasonically cleaned with acetone, absolute ethanol and deionized water for 5 minutes respectively; In 2M acetic acid electrolyte, the sample was anodized, and the mode of slow uniform flow was adopted, that is, from 5mA / cm 2 Rise to 50mA / cm 2 Hold for 2min at each current density, with a step of 5mA / cm 2 , Co-anodized for 20min. Then carry out secondary anodic oxidation treatment in 2M sodium acetate electrolyte, adopt constant voltage mode, preset voltage value is 200V, keep 1min after reaching preset voltage value. Scanning electron microscope observation, under low magnification, you can see the staggered groove-like porous structure, the groove width is 20-30 microns, and under high magnification, you can see the sub-micron microporous structure densely distributed on the entire surface, with a pore size of 0....

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Abstract

The invention relates to a method for preparing a titanium dioxide layer with a multi-level pore structure on the surface of medicinal titanium. The method provided by the invention comprises the following steps of: performing anode oxidation of a direct-current slow uniform-speed current raising mode on the medicinal titanium in acetic electrolyte, and performing secondary anode oxidation of a direct-current constant voltage mode in sulfuric acid or sodium acetate electrolyte to obtain the titanium dioxide layer with the multi-level pore structure, wherein the large-pore structure consists of staggered groove structures, the widths of grooves are 20 to 30 microns, the small-pore structure comprises submicron micropore structures densely distributed on the whole film, and the aperture is between dozens of and hundreds of microns. The method is simple and rapid, has simple and convenient operation, and is expected to become a surface modification method for medicinal titanium metal in the field of orthopedics, dentistry or plastic surgery.

Description

technical field [0001] The invention relates to the electrochemical surface modification treatment of medical titanium. A titanium dioxide layer with a multi-level porous structure is formed on the surface through a two-step anodic oxidation treatment process. It is expected to be used in the surface modification of titanium implants in orthopedics, dentistry or plastic surgery. Sexual field, improve the osseointegration ability of the implant. Background technique [0002] Commonly used metal biomedical materials include stainless steel, cobalt-based alloys, tantalum, titanium and titanium alloys. Among them, titanium and titanium alloys have good machinability, biocompatibility and strong corrosion resistance, so they are widely used as replacement materials for hard tissues in load-bearing parts such as joints and roots in clinical practice. For a long time, it has been believed that the good biocompatibility of titanium metal mainly comes from the oxide film on its surf...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C25D11/26A61L27/30A61L27/06A61L27/56
Inventor 尹光福廖晓明谢利姚亚东黄忠兵陈显春
Owner SICHUAN UNIV
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