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Porous nano titanium oxide base heterogeneous bioactive surface and its preparing process

A nano-titanium oxide, bioactive technology, applied in surface reaction electrolytic coatings, coatings, electrolytic coatings, etc., can solve the problems of low bonding strength, difficulty in porosity, lack of biological activity, etc., and achieve good plastic toughness and bonding strength. High and good biological activity

Inactive Publication Date: 2004-04-28
XI AN JIAOTONG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] Titanium and titanium alloys are commonly used materials for dental implants and load-bearing bone implants. They have good strength and toughness, but lack biological activity. They cannot form chemical bonds with bone in the early stage of implantation and the healing time is long. Surface treatment is required. Porosification and Bioactivation Modification
At present, hydroxyapatite and bioactive glass are mostly used as coating materials for bioactivation on the surface of titanium alloys. Titanium dioxide or sodium titanate gel films formed by chemical activation of titanium alloys have been used as bioactivation surfaces. These coatings Both the titanium alloy and the thin film have obvious interfaces with the titanium alloy, the bonding strength is low, and the porosity is difficult; the titanium oxide layer enriched in calcium and phosphorus formed on the surface of the titanium alloy by ion beam implantation technology has also been confirmed to have biological activity, but the surface layer cannot be porous. and the technology used is difficult to implement on complex surfaces such as threaded dental implants
In 1995, the Japanese took the lead in proposing the micro-arc oxidation process of synthesizing a porous titanium dioxide layer on the surface of titanium alloy. The surface layer has no interface with the titanium alloy matrix and has high bonding strength, but it does not have biological activity. bone apatite
Although the micro-arc oxidation surface layer can be forced to precipitate the hydroxyapatite layer by hydrothermal treatment, the bonding strength drops by 40%.
At present, the bioactive modification technology involving micro-arc oxidation is a two-step method of "micro-arc oxidation + subsequent hydrothermal treatment". The titanium oxide layer is not biologically active, and the precipitated hydroxyapatite reduces the porosity of the surface

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0009] Embodiment 1, the (CH of 0.2mol / l 3 COO) 2 Ca·H 2 O and 0.02mol / l β-C 3 h 7 Na 2 o 6 P·5H 2 O aqueous solution is mixed to make electrolyte solution. With titanium anode and stainless steel sheet as cathode, a DC pulse power supply is used at a constant voltage of 450V and an initial current density of 8A / mm 2 , frequency of 1000Hz, duty cycle of 20%, and cathode-anode plate spacing of 8cm, titanium is subjected to micro-arc oxidation for 5 minutes, and a porous surface layer with a thickness of about 15 μm can be formed on the titanium surface. The surface layer is composed of titanium dioxide, calcium titanate, α-calcium phosphate and β-calcium pyrophosphate, and the grain size is about 20nm. It can induce the deposition of bone apatite in a simulated body fluid environment for 40 days, and has good biological activity.

Embodiment 2

[0010] Embodiment 2, the (CH of 0.5mol / l 3 COO) 2 Ca·H 2 O and 0.06mol / l β-C 3 h 7 Na 2 o 6 P·5H 2 O aqueous solution is mixed to make electrolyte solution. With titanium alloy as the anode and stainless steel sheet as the cathode, a DC pulse power supply is used at a constant voltage of 700V and an initial current density of 15mA / mm 2 , frequency of 1000Hz, duty cycle of 60%, and cathode and anode plate spacing of 12cm, titanium alloy is subjected to micro-arc oxidation for 5 minutes, and a porous surface layer with a thickness of about 40 μm can be formed on the surface of titanium alloy. The surface layer is composed of rutile titanium dioxide, calcium titanate, α-calcium phosphate and β-calcium pyrophosphate, and the grain size is about 25nm. It can induce the deposition of bone apatite in a simulated body fluid environment for 20 days, and has good biological properties. active.

Embodiment 3

[0011] Embodiment 3, the (CH of 0.2mol / l 3 COO) 2 Ca·H 2 O aqueous solution and 0.06mol / l β-C 3 h 7 Na 2 o 6 P·5H 2 O aqueous solution is mixed to make electrolyte solution. With titanium alloy as the anode and stainless steel sheet as the cathode, a DC pulse power supply is used at a constant voltage of 550V and an initial current density of 10mA / mm 2 , frequency 800Hz, duty cycle 50%, and cathode-anode plate spacing 10cm, titanium alloy is subjected to micro-arc oxidation for 5 minutes, and a porous surface layer with a thickness of about 30 μm can be formed on the surface of titanium alloy. The surface layer is composed of rutile titanium dioxide, calcium titanate, α-calcium phosphate and β-calcium pyrophosphate, and the grain size is about 30nm. It can induce the deposition of bone apatite in a simulated body fluid environment for 30 days, and has good biological properties. active.

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Abstract

A prorous nanometre titanium oxide based heterogeneous bioactive surface layer is prepared by micro-arc oxidizing process, that is, the aqueous solution containing Ca and P is used as electrolyte andthe Ti or Ti-alloy is oxidized by micro-arc generated by high-voltage pulse power supply. The said bioactive surface layer is composed of TiO2, calcium titanate, alpha-calcium phosphate and beta-calcium pyrophosphate and has a thickness of over 30 microns, no interface with the matrix, multi-porous nm-crystalline structure on morphology, high bonding strength, good plastic toughness, capability of inducing the formation of apatite and good bioactivity. Its advantages are more than 30 micros for thickness, no interface with matrix, high adhesion, good plastic, toughness and bioactivity, and the elastic modulus close to that of bone.

Description

1. Technical field [0001] The invention relates to the composition and preparation technology of a novel bioactive surface layer on the surface of titanium-based medical implants (such as titanium and titanium alloy dental implants and bone implants), in particular to a porous nano-titanium oxide-based composite bioactive surface layer material and its micro-arc oxidation preparation process. 2. Background technology [0002] Titanium and titanium alloys are commonly used materials for dental implants and load-bearing bone implants. They have good strength and toughness, but lack biological activity. They cannot form chemical bonds with bone in the early stage of implantation and the healing time is long. Porosification and bioactivation modification. At present, hydroxyapatite and bioactive glass are mostly used as coating materials for bioactivation on the surface of titanium alloys. Titanium dioxide or sodium titanate gel films formed by chemical activation of titanium a...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): A61L27/00C25D11/00C25D11/26
CPCC25D11/026C25D11/26
Inventor 憨勇徐可为
Owner XI AN JIAOTONG UNIV
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