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Bioactivity surface modification method used in degradable magnesium alloy

A bioactive, surface modification technology, applied in anodic oxidation, coating, medical science, etc., can solve the problems of insufficient control of degradation rate, large surface roughness, difficult process control, etc., to improve the success of implantation efficiency, improve phase composition, and improve the effect of easy damage

Inactive Publication Date: 2013-07-10
INST OF METAL RESEARCH - CHINESE ACAD OF SCI +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The purpose of the present invention is to provide a bioactive surface modification method for degradable magnesium alloys. By adopting the method provided by the present invention, the degradation rate of magnesium alloys can be controlled, and good wear resistance and good interface bonding strength can be obtained. The surface coating can solve the shortcomings of poor bonding force, low density, large surface roughness, insufficient effect of controlling degradation rate, and difficult process control when preparing coatings directly on magnesium alloy substrates.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] First, a micro-arc oxidation coating was prepared by using pure magnesium with a purity of 99.99% in a phosphate-based electrolyte with a voltage of 360V, a frequency of 800Hz, and a treatment time of 5 minutes. The electrolyte composition is as follows: sodium hexametaphosphate: 1-50g, potassium fluoride: 2-20g / L, calcium hydroxide: 0.1-1g / L, and the rest is water.

[0018] The phosphate-based micro-arc oxidation coating prepared in this example is mainly composed of magnesium phosphate and magnesium oxide, and has a thickness of 20 μm.

[0019] Then wash and dry with deionized water, and prepare a fluorine-rich coating on the outer layer of the phosphate-based micro-arc oxidation coating by fluorine treatment. In 40% hydrofluoric acid, react at 30°C for 24h, take out, rinse thoroughly with deionized water, dry in air, place in a drying oven, dry at 600°C for 3h, and cool naturally with the furnace. A crystallized magnesium fluoride layer is thus obtained on the outer...

Embodiment 2

[0022] The AZ31 (Mg-Al system) magnesium alloy was 2 SiO 3 ·9H 2 The micro-arc oxidation film was prepared in the conversion solution with O as the main component. The composition of the converted aqueous solution is: Na 2 SiO 3 ·9H 2 O: 11g / L, KOH: 4g / L, pH 12, temperature 35oC, time 20min.

[0023] The composition of the micro-arc oxidation coating prepared in this example is Mg 2 SiO 4 and MgO with a thickness of 15 μm.

[0024] Then, it is washed with deionized water and dried, and a fluorine-rich coating is prepared on the outer layer of the phosphate-based micro-arc oxidation coating by fluorine treatment. In acid, react at 30°C for 48h, take out, rinse thoroughly with deionized water, dry in air, place in a drying oven, dry at 50°C for 1h, and cool in air naturally. Thereby an amorphous magnesium fluoride layer is obtained on the outer layer of the micro-arc oxidation coating.

[0025] After the coated AZ31 magnesium alloy was immersed in simulated body fluid ...

Embodiment 3

[0027] The surface of ZK60 (Mg-Zn-Zr series) magnesium alloy is coated by micro-arc oxidation method. The electrolyte composition is, NaOH: 1-5g / l, Na2 SiO 3 : 10-40g / L, KF: 10-15g / L, the rest is water, voltage: 230~450V, time: 5-35min, to prepare a magnesium alloy micro-arc oxidation film with a thickness of 10μm. Then carry out hydrofluoric acid treatment, treatment temperature: 25-90°C, treatment time: 24-48h. A fluorine-rich coating was prepared on the outer surface with a thickness of 10 μm.

[0028] The cytotoxicity of the samples was detected by MTT method. The results showed that the toxicity of magnesium alloy after fluorine treatment coating was grade 0, which met the requirements of biomedical materials. The toxicity of untreated magnesium alloy was grade 3, which could not meet the requirements of biomedical materials for cytotoxicity, indicating that the magnesium alloy surface coating can effectively improve the biocompatibility of magnesium alloy implants.

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Abstract

The invention provides a bioactivity surface modification method used in degradable magnesium alloy. First, a layer of micro-arc oxide coating is prepared on magnesium or magnesium alloy; and with a fluorination treatment method, a fluorine-rich dense layer is prepared on the outer side of the micro-arc oxide coating. Therefore, the surface coating comprises the middle-layer micro-arc oxide coating and the outer-layer fluorine-rich layer. The middle-layer micro-arc oxide coating can control the degradation speed of the magnesium alloy in a living body environment, and assists in ameliorating poor wear resistance of a single fluorine coating and poor bonding strength between the single fluorine coating and the substrate. With the outer-layer fluorine-rich dense layer, the loose characteristic of the micro-arc oxide coating is ameliorated, and pH increasing rate of the coated alloy in the living body environment is reduced, such that early-stage inflammation and hemolysis probabilities are greatly reduced, and magnesium alloy implantation success rate can be improved. The method provided by the invention aims at solving problems such as high degradation speed, poor surface coating bonding strength, low wear resistance, and the like of biodegradable magnesium alloy.

Description

technical field [0001] The invention belongs to the technical field of biomaterials, and is particularly suitable for the field of surface modification of biomedical materials; in particular, it relates to a bioactive surface modification method for degradable magnesium alloys. Background technique [0002] In recent years, magnesium alloys have attracted great attention due to their good mechanical properties, biocompatibility and in vivo degradability, and are expected to become a new generation of degradable implant materials with better performance. Magnesium alloy has high specific strength and specific stiffness, and its strength can exceed 200MPa; the density of pure magnesium is 1.74g / cm 3 About, and the compact bone density of human bone (1.75g / cm 3 ) is equivalent; the Young’s modulus of elasticity of magnesium alloy is about 45GPa, which is closer to the elastic modulus of human bone (about 20GPa), which can significantly reduce the occurrence of stress shielding...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C25D11/30A61L27/04A61L27/30
Inventor 林潇谭丽丽杨柯蔡勇邱剑虹席小松
Owner INST OF METAL RESEARCH - CHINESE ACAD OF SCI
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