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Preparation method of superhydrophobic hydroxyapatite film layer on surface of magnesium alloy

A technology of hydrohydroxyapatite and magnesium alloy, which is applied in the direction of metal material coating technology, coating, and pharmaceutical formulations. The process is simple and easy, and the effect of slowing down the time of corrosion

Inactive Publication Date: 2018-03-13
CHONGQING UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] In view of the above-mentioned deficiencies in the prior art, the purpose of the present invention is to provide a method for preparing a hydrophobic film of nano-hydroxyapatite by hydrothermal method on the surface of a magnesium alloy, so as to solve the corrosion resistance of the existing magnesium alloy as a bone implant material. Poor performance and unsuitability for mass production

Method used

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  • Preparation method of superhydrophobic hydroxyapatite film layer on surface of magnesium alloy
  • Preparation method of superhydrophobic hydroxyapatite film layer on surface of magnesium alloy
  • Preparation method of superhydrophobic hydroxyapatite film layer on surface of magnesium alloy

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Experimental program
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Effect test

Embodiment 1

[0035] 1) Surface pretreatment

[0036] Cut the magnesium alloy AZ31 into a sample of 15mm×1.5mm×2mm. There is a small hole with a diameter of 1mm in the corner of the sample, which can be tied with a thin wire for hanging in the experiment. Use SiC sandpaper (the roughness of the sandpaper is 200#, 400#, 600#, 800#, 1000#) to polish the sample in turn until the surface is smooth and no scratches can be seen with the naked eye. Clean it in an ultrasonic cleaner, then put it into the polishing solution (the volume ratio is HF:HNO 3 :H 2 O=1:10:89), take it out immediately after soaking for 10 seconds, rinse the surface with deionized water, dry it with a hair dryer, and set it aside.

[0037] 2) Preparation of micro / nano-structured hydroxyapatite film by hydrothermal method

[0038] Formulated with disodium calcium salt of EDTA and NaH 2 PO 4 Aqueous solution in which disodium calcium salt of ethylenediaminetetraacetic acid and NaH 2 PO 4 The concentrations were all 0.25...

Embodiment 2

[0048] The morphology of the magnesium alloy coating prepared in Example 1 and Comparative Example 2 was observed with a Σ IGMA HDTM field emission scanning electron microscope (SEM) ( figure 1 ).

[0049] from figure 1 It can be seen that under SEM, a single hydroxyapatite film coating (comparative example 2) forms a needle-like hydroxyapatite crystal layer (such as figure 1 a), but there are many gaps between the crystals; and after further hydrophobic treatment on the surface of the hydroxyapatite film layer (Example 1), a superhydrophobic stearic acid film is formed on the surface of the hydroxyapatite film layer layer (eg figure 1 b), and the stearic acid film penetrates into the micro-nano structure hydroxyapatite film layer, filling many gaps between the crystals, effectively preventing the solution from penetrating through the gaps of the film structure to cause corrosion of the matrix.

[0050] Use the Drop Meter A-100P surface and interfacial tension measuring...

Embodiment 3

[0054] The electrochemical corrosion performance was tested by E G&G Model l273 electrochemical workstation. The measurement adopts a three-electrode system: the reference electrode is a saturated calomel electrode (SCE), the auxiliary electrode is a platinum electrode, and the working electrode is the sample to be tested. The corrosion medium is Hank's biomimetic solution with a pH of 7.4 (composition: NaCl: 8 g / l, KCl: 0.4 g / l, CaCl 2 : 0.14 g / l, NaHCO 3 :0.35 g / l, C 6 h 6 o 6 : 1.0 g / l, MgCl 2 ·6H 2 O:0.1 g / l, MgSO 4 ·7H 2 O: 0.06 g / l, KH 2 PO4: 0.06 g / l, Na 2 HPO 4 12H 2 O: 0.06 g / l). The result is as image 3 shown.

[0055] from image 3 It can be seen that compared with the single hydroxyapatite film layer, the self-corrosion potential of the magnesium alloy sample with the hydroxyapatite film layer treated with stearic acid in Hank's solution is increased, and the self-corrosion current density decreases, and the passivation potential increases. The sm...

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Abstract

The invention provides a preparation method of a superhydrophobic hydroxyapatite film layer on the surface of magnesium alloy. The preparation method comprises the following steps: performing surfacepretreatment, preparing a nano-structured hydroxyapatite layer by a hydrothermal method and performing hydrophobization treatment to the hydroxyapatite layer. The hydrothermal method is designed, andby the hydrothermal method, a rod-shaped hydroxyapatite crystal layer adopting micron-scale length and nano-scale diameter is prepared on the surface of the magnesium alloy, then a stearic acid film is prepared on the surface of the nano-structured hydroxyapatite film layer to form a superhydrophobic film layer with the contact angle of 153 degrees under a static droplet, the film layer can reducethe corrosion current density of the magnesium alloy by 2 orders of magnitude and the impedance modulus of coating is increased from 2029 Omega.cm2 to 117674 Omega.cm2. The preparation method of thenano-structured hydrophobic coating is simple, equipment is simple and easy to control, the cost is low, and the controllability is good; the preparation method is suitable for large-scale production.

Description

technical field [0001] The invention belongs to the technical field of magnesium alloy surface modification and anticorrosion, and in particular relates to a preparation method of a superhydrophobic hydroxyapatite film layer on the surface of a magnesium alloy. Background technique [0002] As a new type of biodegradable material, magnesium and magnesium alloys have a density and elastic modulus similar to that of human bone, and have good mechanical properties and biocompatibility, which have become a hot research topic for domestic and foreign scholars. However, its degradation rate in the human body is too fast, so that it cannot meet the mechanical and morphological requirements of medical biomaterials during its service, and the too fast degradation rate will cause symptoms such as local inflammation in the human body. Therefore, reducing or even controlling the degradation rate of magnesium alloys has always been an urgent problem to be solved in the field of biomateri...

Claims

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Application Information

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IPC IPC(8): A61L27/04A61L27/32A61L27/50C23C18/12
CPCA61L27/047A61L27/32A61L27/50A61L2400/18A61L2430/02C23C18/1204C23C18/1295
Inventor 张春艳张均张世雨
Owner CHONGQING UNIV OF TECH
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