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Process for preparing titanium-based hydroxylapatite/titanium oxide nanotube composite coating

A technology of titanium-based hydroxyapatite and titanium oxide nanotubes is applied in the coating, superimposed layer plating, metal material coating process, etc. The effect of bond strength

Inactive Publication Date: 2008-11-26
FUJIAN NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The above preparation methods have their own advantages and disadvantages, and have not been widely used clinically.

Method used

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  • Process for preparing titanium-based hydroxylapatite/titanium oxide nanotube composite coating

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] 1) Pretreatment: use pure titanium as the substrate, add 4% HF and 5mol / L HNO 3 Etched in the mixed acid solution for 30 seconds, then took it out, cleaned it with distilled water, and dried it at 80°C.

[0019] 2) Anodic oxidation: use pure titanium as the anode, platinum sheet as the cathode, control the distance between the cathode and anode to be 1cm, oxidize in a dimethyl sulfoxide solution containing 2% HF by mass percentage, voltage 60V, and oxidize in a water bath at 20°C for 24h. Then take it out, wash it with distilled water, and dry it at 80°C. The surface morphology observed by scanning electron microscope is shown in Fig. 1 in the accompanying drawings. The diameter of the nanotube is about 170nm, and the wall thickness of the tube is 30nm. From its cross-sectional view, it can be seen that the length of the nanotube tube is about 12 μm.

[0020] 3) Hydrothermal deposition: at 0.1mol / L CaCl 2 , 0.1mol / L NaH 2 PO 4 , In an aqueous solution of 0.2mol / L ...

Embodiment 2

[0022] 1) Pretreatment: use pure titanium as the substrate, add 4% HF and 5mol / L HNO 3 Etched in the mixed acid solution for 30 seconds, then took it out, cleaned it with distilled water, and dried it at 80°C.

[0023] 2) Anodic oxidation: use pure titanium as the anode, platinum sheet as the cathode, control the distance between the cathode and the anode to be 1cm, oxidize in a dimethyl sulfoxide solution containing 1% HF at a voltage of 20V, and oxidize in a water bath at 10°C for 2h. Then take it out, wash it with distilled water, and dry it at 80°C. The diameter of the titanium oxide nanotubes observed by the scanning electron microscope is about 100 nm, and the wall thickness of the tubes is 10 nm. From its cross-sectional view, it can be seen that the length of the nanotube tube is about 2 μm.

[0024] 3) Hydrothermal deposition: at 0.25mol / L CaCl 2 , 0.5mol / L NaH 2 PO 4 , 0.2mol / L EDTA aqueous solution, use 1mol / L NaOH to adjust the pH value of the solution to 4, u...

Embodiment 3

[0026] 1) Pretreatment: use pure titanium as the substrate, add 4% HF and 5mol / L HNO 3 Etched in the mixed acid solution for 30 seconds, then took it out, cleaned it with distilled water, and dried it at 80°C.

[0027] 2) Anodic oxidation: use pure titanium as the anode, platinum sheet as the cathode, control the distance between the cathode and the anode to be 1cm, oxidize in a dimethyl sulfoxide solution containing 4% HF by mass percentage, a voltage of 70V, and oxidize in a water bath at 30°C for 10h. Then take it out, wash it with distilled water, and dry it at 80°C. The diameter of the titanium oxide nanotube is about 150nm and the thickness of the tube wall is 20nm as observed by scanning electron microscope. From its cross-sectional view, it can be seen that the length of the nanotube tube is about 20 μm.

[0028] 3) Hydrothermal deposition: at 0.5mol / L CaCl 2 , 0.25mol / L NaH 2 PO 4, In an aqueous solution of 0.2mol / L EDTA, adjust the pH value of the solution to 6 ...

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Abstract

The invention discloses a method for preparing titanium base hydroxy apatite or titanium oxide nano tube composite coating, comprising the following steps: the pure titanium is taken as an anode while a platinum plate is taken as a cathode; in the dimethyl sulfoxide solution containing HF with the weight percent of 1 to 4 percent, under the voltage of 20 to 70 V, the pure titanium and the platinum plate are oxidized for 2 to 10 hours in the water bath with the temperature of 10 to 30 DEG C; then, a titanium oxide nano tube array film is arranged in aqueous solution which contains 0.1 to 0.5mol per liter of CaC12, 0.1 to 0.5 mol per liter of NaH2PO4 and 0.2 mol per liter of EDTA. The PH value of the solution is adjusted by NaOH to be 4 to 6. Under the condition of the temperature of 100 to 200 DEG C and hydrothermal reaction of 2 to 10 hours, the hydroxyapatite is induced to be crystallized and deposited on the surface of the array film of the nano tube and a novel hydroxyapatite coating layer which takes the array film of the titanium oxide nano tube as a buffer layer is formed. The method is characterized by taking the array film of the titanium oxide nano tube as the buffer layer, which reduces the residual stress caused by mismatch of coefficient of heat expansion of the hydroxyapatite and the titanium base and enhances the binding strength of the coating layer and the base interface.

Description

technical field [0001] The invention relates to a method for preparing a titanium-based hydroxyapatite / titanium oxide nanotube composite coating, which belongs to the preparation technology of bone repair biological materials. Background technique [0002] Titanium is currently the most attractive metal biomaterial for bone replacement due to its excellent biocompatibility, mechanical properties, and corrosion resistance. However, because it is a biologically inert material, it cannot be chemically bonded with natural bone, which easily leads to loosening of the implant and failure of the operation. The way to solve this problem is to coat a layer of biologically active materials on the surface of titanium implants by physical or chemical methods, such as coatings such as hydroxyapatite ceramics or bioglass ceramics, so that the implants have both excellent Mechanical properties and biological activity. There are more than a dozen methods for preparing hydroxyapatite coati...

Claims

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Application Information

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IPC IPC(8): C25D11/26C23C28/04A61L27/42A61L27/06A61L27/32
Inventor 肖秀峰刘榕芳李明欧
Owner FUJIAN NORMAL UNIV
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