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Oxidation-carbon-coating-diamond-like composite film on the surface of medical titanium and titanium alloy and its preparation method

A surface oxidation and titanium alloy technology, which is applied in the field of surface treatment of medical metal materials, can solve the problems of limiting the connection between the film and the substrate, the thickness of the film, the high residual stress of the film, and the thin injection layer.

Active Publication Date: 2016-06-08
RESEARCH INSTITUTE OF TSINGHUA UNIVERSITY IN SHENZHEN
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] (1) The ion implantation method mainly uses high-energy ions to bombard the surface of the material to obtain a thin film, which has good adhesion and no peeling off, but the biggest disadvantage is that the implanted layer is very thin, usually no more than 1 μm, once the implanted layer is destroyed After that, the matrix will be directly exposed and participate in the friction
And the process costs a lot, and the cost performance is low
[0005] (2) Diamond-like film coating method, DLC has extremely high hardness and wear resistance, but DLC is a brittle material, which does not match the physical properties of the substrate material during the growth process, resulting in large internal stress, so that the film and the substrate The bonding strength is poor, which limits the connection between the film and the substrate and the thickness of the film
[0006] (3) Laser modification method, the metallurgical bond with high bonding strength between the coating and the substrate, the coating thickness is relatively large, and has excellent properties such as high hardness, small friction coefficient, wear resistance, corrosion resistance and high temperature resistance, but Due to the rapid cooling of the molten pool, brittle phases in the film will be generated and high residual stress will be generated on the surface, resulting in cracks
In addition, air bubbles may form in the molten pool in an overheated state, and micropores and pores sometimes appear in the cladding layer
[0007] (4) The oxidation treatment method has the advantages of simple process, high cost performance, in-situ growth, and large film thickness. Comprehensive performance
[0008] At present, a single wear-resistant modified film generally cannot meet the requirements of the complex mechanical and physiological environment of the human body. The future development trend is to prepare composite films to solve the problems of insufficient bonding force and insufficient film thickness of a single film.

Method used

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  • Oxidation-carbon-coating-diamond-like composite film on the surface of medical titanium and titanium alloy and its preparation method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] In this example, a medical titanium disc is used as a sample to prepare a composite film with a thickness of about 2 μm, a surface nanohardness of about 10.5 GPa, and a C-C structure sp in the carbon / titanium carbide carbon coating layer. 2 Bond content 66%, sp 3 The bond content is 34%, the thickness is about 300nm, and the C-C structure sp in the diamond-like layer 2 Bond content 50%, sp 3 The bond content is 50%, and the thickness is about 600nm. Specific steps are as follows:

[0033] (1) After the sample is ground and polished, the surface roughness is 0.05-0.1 μm, then ultrasonically cleaned in absolute ethanol or acetone solution for 20 minutes, then ultrasonically cleaned in deionized water for 30 minutes, and finally placed in a vacuum drying oven to dry 24 hours standby.

[0034] (2) Put the sample to be treated into a tube furnace for thermal oxidation treatment. The thermal oxidation temperature is 600°C, and the oxidation time is 2 hours. During the ox...

Embodiment 2

[0038] In this example, a medical titanium alloy disc (Ti6Al4V) was used as a sample to prepare a composite film with a thickness of 3.6 μm, a surface nanohardness of about 12 GPa, and a C-C structure sp in the carbon / titanium carbide carbon coating layer. 2 Bond content 50%, sp 3 The bond content is 50%, the layer thickness is about 600nm, and the C-C structure sp in the diamond-like layer 2 Bond content 40%, sp 3 With a bond content of 60%, the thickness of this layer is about 900 nm. Specific steps are as follows:

[0039] (1) After the sample is ground and polished, the surface roughness is 0.05-0.1 μm, then ultrasonically cleaned in absolute ethanol or acetone solution for 30 minutes, then ultrasonically cleaned in deionized water for 25 minutes, and finally placed in a vacuum drying oven to dry 30 hours to use.

[0040] (2) Put the sample to be treated into a tube furnace for thermal oxidation treatment. The thermal oxidation temperature is 700°C, and the oxidation ...

Embodiment 3

[0044] In this example, a medical titanium alloy (Ti6Al4V) artificial cervical intervertebral disc upper endplate joint prosthesis is used as a sample, and the thickness of the composite film is about 3 μm, the surface nanohardness is about 11 GPa, and the C-C structure sp in the carbon / titanium carbide carbon coating layer 2 Bond content 60%, sp 3 The bond content is 40%, the layer thickness is about 500nm, and the C-C structure sp in the diamond-like layer 2 Bond content 40%, sp 3 With a bond content of 60%, the thickness of this layer is about 800 nm. Specific steps are as follows:

[0045] (1) After professional grinding and polishing of the joint surface of the sample, the surface roughness is 0.08-0.1 μm, then ultrasonic cleaning in absolute ethanol or acetone solution for 25 minutes, then ultrasonic cleaning in deionized water for 20 minutes, and finally placed in vacuum drying Dry in the oven for 20 hours before use.

[0046] (2) Put the sample to be treated into a...

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Abstract

The invention discloses an oxidation-carbon-coated-diamond-like composite film on the surface of medical titanium and titanium alloy. carbon layer and a diamond-like layer. The invention also discloses a preparation method of the composite membrane. The composite film prepared by the present invention has relatively large film-base binding force and large film thickness based on in-situ growth, and has excellent film comprehensive performance, and the present invention has simple process, high cost performance and can be mass-produced.

Description

technical field [0001] The invention belongs to the field of surface treatment of medical metal materials, in particular to a medical titanium and titanium alloy surface oxidation-carbon-coating-diamond-like (TiO 2 -C / TiC-DLC) composite film and preparation method thereof. Background technique [0002] Titanium and titanium alloys are widely used in the biomedical field due to their excellent specific strength, elastic modulus, biocompatibility and other properties, especially as hard tissue replacement materials, such as artificial joints, artificial intervertebral discs and other prostheses. structural materials, etc. However, titanium and titanium alloys have extremely poor wear resistance. After the titanium alloy prosthesis is implanted into the human body, under the complex physiological and mechanical environment of the human body, the wear-resistant life is significantly insufficient, and even osteolysis will be caused by a large number of wear particles. cause the...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): A61L27/30A61L27/42C23C8/10C23C14/48C23C16/26C23C28/04B32B15/04
Inventor 王松卢俊哲廖振华刘伟强
Owner RESEARCH INSTITUTE OF TSINGHUA UNIVERSITY IN SHENZHEN
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