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Medical magnesium alloy surface degradable composite protective film layer and preparation method thereof

A protective film layer, magnesium alloy technology, applied in medical science, anodic oxidation, prosthesis, etc., can solve the problems of micro-arc oxidation ceramic layer adaptability to be analyzed, corrosion resistance decline, sealing agent is difficult, etc., to achieve Good blood compatibility and tissue compatibility, improved corrosion resistance, and high membrane-base binding force

Inactive Publication Date: 2012-04-04
SOUTHEAST UNIV
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AI Technical Summary

Problems solved by technology

The commonly used impregnants are mainly divided into two categories: inorganic substances (silicates) and organic substances (such as synthetic resins, anaerobic adhesives, etc.) (Guangzhou Institute of Chemistry, Chinese Academy of Sciences; Guangzhou Jianhong Chemical Factory, seal reinforcement Use methacrylate type vacuum impregnating agent: China, 01130100.7 [P]. Method: China, 200610073791.6[P].2006-04-17), but the application of vacuum impregnation technology in bioactive materials, especially hydroxyapatite / gelatin as impregnating agent, is rarely reported
Nowadays, although there are many scholars on hydroxyapatite / gelatin composite scaffold (Liu Wenbin. Preparation and performance research of hydroxyapatite / gelatin composite material [D]: Chengdu: Southwest Jiaotong University, 2005. Sun Ruixue. Gelatin / hydroxy Research on the Influence of Gelatin in Apatite Composite Microspheres on Inorganic Phase[J]. Imaging Science and Photochemistry, 2009, 27(5), Microspheres (Zhao Feng. Chitosan-gelatin network / hydroxyapatite composite material Scaffold research--preparation and morphology [J]. Chinese Journal of Prosthetic and Reconstructive Surgery, 2001, 15 (5)), coating (Peng Xianghong. Performance of chitosan / nano multilayer structure hydroxyapatite / gelatin composite film[ J]. Chinese Tissue Engineering Research and Clinical Rehabilitation, 2008, 12 (14)) research and report, but the coating obtained is often limited to specific polymers, and the adaptability of the micro-arc oxidation ceramic layer remains to be analyzed (Zhang Weiping. Research on preparation and surface modification of polylactic acid porous scaffolds [D]: Nanjing: Southeast University, 2009). At the same time, these membrane layers are often only sealed on the surface. For some through-holes and other holes, the sealing agent is difficult to be completely coated under the action of internal and external pressure, so that when the apparent sealing layer of the material is eroded, the corrosion resistance will be significantly reduced

Method used

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  • Medical magnesium alloy surface degradable composite protective film layer and preparation method thereof
  • Medical magnesium alloy surface degradable composite protective film layer and preparation method thereof
  • Medical magnesium alloy surface degradable composite protective film layer and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] (1) Sample preparation: select AZ31B magnesium alloy and process it into a wire that meets the required diameter;

[0029] (2) Pretreatment: ultrasonically clean the magnesium alloy wire with acetone, distilled water, and absolute ethanol in sequence for 10 minutes, and dry it for later use;

[0030] (3) Preparation of micro-arc oxidation electrolyte: 10 g / L of hydroxyapatite nanoparticles, 10 g / L of nano-zirconia particles, 10 g / L of silicate, 1 g / L of sodium hydroxide, and 5 g / L of phosphate;

[0031] (4) Preparation of hydroxyapatite / gelatin mixed solution: prepare a mixed solution containing 8wt% gelatin and 1wt% nano-sized hydroxyapatite, stir evenly, and set aside;

[0032] (5) Micro-arc oxidation: the magnesium alloy wire obtained in step (2) is used as the anode, and the stainless steel bucket is used as the cathode, placed in the electrolyte a, applying a positive voltage of 450V, a negative voltage of 60V, a frequency of 600Hz, and a duty cycle of 20%, the el...

Embodiment 2

[0035] (1) Sample preparation: select AZ91D magnesium alloy and process it into wires that meet the requirements;

[0036] (2) Pretreatment: ultrasonically clean the magnesium alloy wire with acetone, distilled water, and absolute ethanol in sequence for 10 minutes, and dry it for later use;

[0037] (3) Preparation of micro-arc oxidation electrolyte: hydroxyapatite nanoparticles 5g / L, nano-zirconia particles 5g / L, silicate 10g / L, potassium hydroxide 2g / L;

[0038] (4) Preparation of hydroxyapatite / gelatin mixed solution: respectively prepare mixed solutions containing 5wt% gelatin, 0.5wt% nano-sized hydroxyapatite, and 10wt% gelatin, 2wt% nano-sized hydroxyapatite mixed solution, Stir well and set aside;

[0039] (5) Micro-arc oxidation: the magnesium alloy wire obtained in step (2) is used as the anode, the stainless steel barrel is used as the cathode, and a forward current of 3A / dm is applied 2 , negative current 1A / dm 2 , the frequency is 600Hz, the duty cycle is 20%, ...

Embodiment 3

[0042] (1) Sample preparation: process the magnesium alloy into thin plates that meet the requirements;

[0043] (2) Pretreatment: adopt 200 successively # , 400 # , 600 # , 1000 # , 1200 # Grind with sandpaper, ultrasonically clean the magnesium alloy plate with acetone, distilled water, and absolute ethanol for 10 minutes, and dry it for later use;

[0044] (3) Preparation of micro-arc oxidation electrolyte: 10 g / L of hydroxyapatite nanoparticles, 5 g / L of nano-zirconia particles, 10 g / L of silicate, 1 g / L of potassium hydroxide, and 5 g / L of phosphate.

[0045] (4) Preparation of hydroxyapatite / gelatin mixed solution: prepare a mixed solution containing 6wt% gelatin and 0.5wt% nano-sized hydroxyapatite, stir evenly, and set aside;

[0046] (5) Micro-arc oxidation: the magnesium alloy sheet obtained in step (2) is used as an anode, and the stainless steel barrel is used as a cathode, and a forward voltage of 450V is applied, a negative voltage of 60V, a frequency of 600...

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Abstract

The invention relates to a medical magnesium alloy surface degradable composite protective film layer and a preparation method thereof. The degradable composite protective film is prepared on a medical magnesium alloy surface and has an internal and external bilayer film structure: the internal layer film is prepared by a microarc oxidation technology, a magnesium oxide and magnesium silicate ceramic phase is used as a substrate, and nanometer zirconia particles used for toughening and strengthening and hydroxyapatite particles used for improving bioactivity are dispersed and distributed in the substrate phase; and the external layer film is prepared in a vacuum infiltration method, gelatin is used as a substrate, and hydroxyapatite particles are dispersed and distributed in the gelatin substrate. The composite film layer can obviously improve the corrosion resisting property and toughness of material so as to achieve the purpose of controllable degradation, and simultaneously the composite film layer can improve the biocompatibility of the material.

Description

technical field [0001] The invention relates to a surface protective film material of a medical magnesium alloy and a preparation method thereof, belonging to the field of biomedical devices. Specifically, it is a degradable composite protective film layer on the surface of a medical magnesium alloy with a double-layer film structure, in which the inner film is prepared by micro-arc oxidation technology, with magnesium oxide and magnesium silicate ceramic phase as the matrix, and dispersedly distributed in the matrix phase There are nano zirconia particles for strengthening and toughening and hydroxyapatite particles for improving biological activity; the outer film is prepared by vacuum impregnation method, with gelatin as the matrix, and hydroxyapatite particles are dispersed in the gelatin matrix . Background technique [0002] Magnesium alloys play an important role in helping to repair or replace diseased or damaged body tissue. Compared with ceramic materials and pol...

Claims

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Application Information

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IPC IPC(8): A61L27/40A61L27/42A61L27/46A61L31/12C25D11/30
Inventor 储成林韩啸薛烽董寅生白晶郭超盛晓波王世栋
Owner SOUTHEAST UNIV
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