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Method for preparing zinc-doped calcium-phosphorus coating on magnesium alloy surface by one-step hydrothermal method

A calcium-phosphorus coating and magnesium alloy technology, applied in metal material coating process, coating, pharmaceutical formulation and other directions, to achieve the effects of short time consumption, good interface mechanical properties, and great commercial promotion value

Inactive Publication Date: 2020-01-03
TIANJIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] In summary, the zinc-doped calcium phosphorus coating prepared by the one-step hydrothermal method applied by the present invention combines the hydrothermal method with the Zn 2+ The combination of doping can not only effectively improve the corrosion resistance of magnesium alloys, solve the problem of rapid degradation in the human environment, but also use the high temperature and high pressure environment of the hydrothermal method and the Zn 2+ It is expected to further improve the bonding strength between the coating and the substrate and the biological activity of the calcium-phosphorus coating itself on the basis of the existing research results, so as to obtain excellent corrosion resistance on the surface of the magnesium alloy. However, there are few reports on the preparation of zinc-doped calcium-phosphorus coatings on the surface of magnesium alloys by one-step hydrothermal method.

Method used

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  • Method for preparing zinc-doped calcium-phosphorus coating on magnesium alloy surface by one-step hydrothermal method
  • Method for preparing zinc-doped calcium-phosphorus coating on magnesium alloy surface by one-step hydrothermal method
  • Method for preparing zinc-doped calcium-phosphorus coating on magnesium alloy surface by one-step hydrothermal method

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Embodiment 1

[0032] Process the AZ31 magnesium alloy into a block of 10mm×10mm×2mm, and use 800 # , 1500 # , 2000 # Polished with SiC sandpaper, then ultrasonically cleaned in acetone, deionized water, and absolute ethanol for 10 minutes, and dried with hot air. Prepare 150 mL of 3 mol / L NaOH deionized aqueous solution. Soak the polished magnesium alloy in NaOH solution at 80°C for 1 hour, then wash the magnesium alloy sample with deionized water and dry it. With Ca(NO 3 ) 2 Prepare Ca for Ca source 2+ Aqueous solution, as Na 2 HPO 4 Preparation of PO for P source 4 3- Aqueous solution, with Zn(NO 3 ) 2 Preparation of Zn for Zn source 2+ aqueous solution. Then Zn 2+ and PO 4 3- The aqueous solution was added dropwise with Ca 2+ In the aqueous solution, the pH value of the mixed solution was finally adjusted to 5 with 20 M dilute nitric acid, and magnetically stirred for 2 h. Among them, Ca in the mixed solution 2+ The concentration is 2mmol / L, Zn 2+ The concentration is...

Embodiment 2

[0034] Process the AZ91 magnesium alloy into a block of 10mm×10mm×2mm, and use 800 # , 2000 # Polished with SiC sandpaper, then ultrasonically cleaned in acetone, deionized water, and ethanol for 6 minutes, and dried with hot air. Prepare 150 mL of 2 mol / L NaOH deionized aqueous solution. Soak the polished magnesium alloy in NaOH solution at 70°C for 2 hours, then wash the magnesium alloy sample with deionized water and dry it. with CaCl 2 Prepare Ca for Ca source 2+ Aqueous solution, as NaH 2 PO 4 Preparation of PO for P source 4 3- Aqueous solution, with ZnCl 2 Preparation of Zn for Zn source 2+ aqueous solution. Then Zn 2+ and PO 4 3- The aqueous solution was added dropwise with Ca 2+ In the aqueous solution, the pH value of the mixed solution was finally adjusted to 4 with 15M dilute nitric acid, and magnetically stirred for 1.5 h. Among them, Ca in the mixed solution 2+ The concentration is 2.5mmol / L, Zn 2+ The concentration is 0.25mmol / L, PO 4 3- The c...

Embodiment 3

[0036] Process the AZ61 magnesium alloy into a block of 10mm×10mm×2mm, and use 800 # , 1200 # , 1500 # Polished with SiC sandpaper, then ultrasonically cleaned in acetone, deionized water, and ethanol for 8 minutes, and dried with hot air. Prepare 150 mL of 2 mol / L NaOH deionized aqueous solution. Soak the polished magnesium alloy in NaOH solution at 90°C for 1 hour, then wash the magnesium alloy sample with deionized water and dry it. With Ca(CH 3 COO) 2 Prepare Ca for Ca source 2+ Aqueous solution, as NaH 2 PO 4 Preparation of PO for P source 4 3- Aqueous solution, with ZnCl 2 Preparation of Zn for Zn source 2+ aqueous solution. Then Zn 2+ and PO 4 3- The aqueous solution was added dropwise with Ca 2+ In the aqueous solution, the pH value of the mixed solution was finally adjusted to 5.5 with 5M acetic acid, and magnetically stirred for 1.5 h. Among them, Ca in the mixed solution 2+ The concentration is 2.5mmol / L, Zn 2+ The concentration is 0.25mmol / L, PO ...

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Abstract

The invention relates to a method for preparing a zinc-doped calcium phosphorus coating on a magnesium alloy surface by using a one-step hydrothermal method. The method comprises the following steps:firstly preparing coating solution, respectively preparing Ca<2+> water solution, Zn<2+> water solution and PO4<3-> water solution, dropwise adding the Zn<2+> water solution and the PO4<3-> water solution into the Ca<2+> water solution, adjusting a pH value of mixed solution to 4-6 by using diluted acid; placing the coating solution in a reaction kettle, soaking a preprocessed magnesium alloy sample in the coating solution, heat-insulating at 130-150 DEG C, cooling to a room temperature along with an oven, taking out the magnesium alloy sample covered with the coating, washing, and drying, toobtain a magnesium alloy of which the surface is the zinc-doped calcium phosphorus coating. The zinc-doped calcium phosphorus coating on the magnesium alloy surface is a compact flower-like structure.The method is simple, easy to operate, and short in consumed time. The uniform zinc-doped calcium phosphorus coating can be prepared on the surface of the magnesium alloy samples in any shapes and sizes; the coating has the remarkable corrosion resistance and the good biological activity.

Description

technical field [0001] The invention relates to a one-step hydrothermal preparation method of a zinc-doped calcium-phosphorus coating on the surface of a magnesium alloy, and belongs to the technical field of surface modification of degradable magnesium alloy implants. Background technique [0002] Magnesium and its alloys have the characteristics of suitable comprehensive mechanical properties, good biocompatibility with the human body, and biodegradable absorption. They are expected to become a new class of medical implant materials. Compared with other biometal materials, the elastic modulus and density of magnesium alloy are closer to human bone, which can effectively reduce the stress shielding effect. And magnesium, as an essential element of the human body, participates in almost all metabolic processes in the human body, and plays an important role in regulating bone mineral metabolism and protein synthesis. The most important thing is that magnesium alloy has poor ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C23C18/12A61L27/04A61L27/32A61L27/50
CPCA61L27/047A61L27/32A61L27/50A61L2400/18A61L2420/02C23C18/1204C23C18/1241
Inventor 蔡舒林易树江松凌瑞谢东篱韦洁玲孙佳月
Owner TIANJIN UNIV