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Preparation method for hydroxylapatite coating

A hydroxyapatite and coating technology, applied in coating, metal material coating process, melt spraying and other directions, can solve the problems of large residual stress, decreased coating bonding strength, insufficient crystallinity, etc. Fine structure, reduced residual stress, controllable effect of coating porosity

Inactive Publication Date: 2016-06-08
YANGZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] However, with the deepening of research and clinical application, it is found that in the process of preparing coatings by traditional plasma spraying, due to the high temperature of plasma flame, hydroxyapatite decomposes to form impurity phases such as tricalcium phosphate, tetracalcium phosphate, and calcium oxide, while the particles The solidification and cooling stage on the surface of the substrate is another chilling process. There are a lot of amorphous in the coating, and the rapid heating-cooling process leads to insufficient crystallinity of the coating and excessive residual stress. These problems still restrict the hydroxyapatite material system. Applications
[0004] Before the present invention was made, the hydroxyapatite coating in the existing traditional plasma spraying process had problems such as easy decomposition, low crystallinity, and large residual stress, especially the consequences of insufficient crystallinity were the most serious
Hydroxyapatite with insufficient crystallinity will be rapidly dissolved by body fluids after implantation, resulting in poor biological stability
The ISO13779-2 standard stipulates that the crystallinity of the hydroxyapatite coating must be greater than 45%, but the crystallinity of the traditional plasma sprayed hydroxyapatite coating is difficult to meet this requirement, and post-treatment steps such as heat treatment are required to improve the crystallization of the coating. However, this will lead to problems such as grain growth or decrease in coating bonding strength, and the process is complicated and the molding cost is increased.

Method used

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  • Preparation method for hydroxylapatite coating
  • Preparation method for hydroxylapatite coating
  • Preparation method for hydroxylapatite coating

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0060] Disperse 35g of hydroxyapatite powder with a particle size of about 0.5μm in 500mL of absolute ethanol, add a small amount of polyethylene glycol, and form a stable suspension after magnetic stirring. The needle of mm is fed into the flame flow of the flame spray gun, and deposited on the 45 steel substrate to form the hydroxyapatite coating. The gas used by the spray gun is oxygen and acetylene, the moving speed of the spray gun is 150m / s, and each time it moves down 2mm, spraying 15 times continuously. The phase structure was observed by X-ray diffractometer, such as figure 2 As shown, through XRD phase calibration, hydroxyapatite 8, tricalcium phosphate 9, tetracalcium phosphate 10, calcium oxide 11, hydroxyapatite 8 have the strongest peak and the highest content, and the crystallinity of the coating is calculated to be 75%.

Embodiment 2

[0062] Disperse 50g of hydroxyapatite powder with a particle size of about 1 μm in 1000mL of deionized water, add a small amount of dispersant, form a stable suspension after magnetic stirring, and pass the suspension at a flow rate of 25mL / min. The needle is fed into the plume of the plasma torch, and the hydroxyapatite coating is deposited on the titanium alloy substrate. During the spraying process, the spraying power is 30kW, the moving speed of the spray gun is 200m / s, and each time moves down 2mm, spraying continuously for 20 times. The surface microstructure of the coating was observed with a field emission scanning electron microscope. Such as image 3 As shown, there is a low porosity, no large pores, and the coating is well bonded. The coating thickness is 240 μm, that is, the coating deposition rate is about 12 μm / time. Calculated by XRD spectrum, the crystallinity of the coating is 68%. This parameter is suitable for preparing hydroxyapatite coatings with thinne...

Embodiment 3

[0064] The precursors of 0.5M calcium nitrate, 0.3M diammonium hydrogen phosphate and 0.4M ammonia solution are sent into the flame flow of the plasma spray gun through a needle with an inner diameter of 0.22mm at a flow rate of 30mL / min, and deposited on the stainless steel substrate to form hydroxyapatite stone coating. During the spraying process, the spray gun moves at a speed of 250m / s, moves down 3mm each time, and sprays continuously for 20 times. The microstructure was observed with a field emission scanning electron microscope (FE-SEM). Such as Figure 4 As shown, there are small pores locally, and the porosity is moderate. Through section analysis, the thickness of the coating is 240 μm, that is, the deposition rate of the coating is about 12 μm / time, and the crystallinity of the coating is 70% calculated by the XRD pattern. This parameter is suitable for the preparation of hydroxyapatite coatings with thinner thickness and porous structure.

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Abstract

The invention relates to a preparation method for a hydroxylapatite coating. A liquid material which is a calcium salt solution precursor or hydroxylapatite suspension liquid serves as the feedstock. Plasma spraying or hypersonic flame spraying or common flame spraying thermal spraying flame flow serves as the heating means to heat liquid drops. The liquid material is injected into the flame flow through a pressure pump or a peristaltic pump, and after entering the flame flow, the liquid drops are subjected to all or a part of the processes of decomposition, evaporation, nucleation, growth, melting and acceleration and are deposited on a metallic matrix to form the coating. According to the preparation method for the hydroxylapatite coating, the defects that a hydroxylapatite coating in the plasma spraying process is prone to being decomposed, low in crystallinity, large in residual stress and the like are overcome; the flame flow is surrounded by water vapor which beneficially improves the crystallinity of the hydroxylapatite, accordingly, compared with a conventional coating method, reducing of the residual stress in the coating is facilitated through liquid material spraying, and the crystallinity of the hydroxylapatite coating is very high.

Description

technical field [0001] The invention relates to engineering and material science, in particular to a method for preparing a hydroxyapatite coating. Background technique [0002] Hydroxyapatite is the main inorganic component of human hard bone tissue. The chemical composition and crystal structure of artificially synthesized hydroxyapatite are basically the same as the main inorganic mineral components of human bone tissue. Ash has broad application prospects in bone repair substitute materials. [0003] However, with the deepening of research and clinical application, it is found that in the process of preparing coatings by traditional plasma spraying, due to the high temperature of plasma flame, hydroxyapatite decomposes to form impurity phases such as tricalcium phosphate, tetracalcium phosphate, and calcium oxide, while the particles The solidification and cooling stage on the surface of the substrate is another chilling process. There are a lot of amorphous in the coat...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C23C4/129C23C4/134C23C4/10
CPCC23C4/10
Inventor 张超徐海峰耿欣肖金坤
Owner YANGZHOU UNIV
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