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Preparation method of zinc phosphate chemical conversion coating in hierarchical structure

A technology of chemical conversion coating and hierarchical structure is applied in the preparation of novel structural chemical conversion coating and the preparation of zinc-based phosphate chemical conversion coating with graded structure on the surface of medical stainless steel substrate, which can solve the problems of unsuitable stainless steel surface modification, etc. The effect of low cost, mild conditions, and easy process operation

Active Publication Date: 2014-07-16
SHANDONG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Due to the existence of passivation film on the surface of stainless steel, the traditional chemical conversion method is not suitable for the surface modification of stainless steel

Method used

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  • Preparation method of zinc phosphate chemical conversion coating in hierarchical structure
  • Preparation method of zinc phosphate chemical conversion coating in hierarchical structure
  • Preparation method of zinc phosphate chemical conversion coating in hierarchical structure

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] (1) Preparation of chemical conversion solution A: 25g / L zinc oxide, 30ml / L nitric acid, 15ml / L phosphoric acid, 5g / L calcium nitrate, 20g / L citric acid. Then slaking with 5g / L pure iron powder for 24h to obtain chemical conversion solution A1.

[0027] (2) Using 316 medical stainless steel as the substrate, carry out acid etching treatment with 7wt% phosphoric acid, wherein the acid etching temperature is room temperature, and the acid etching time is 10 minutes;

[0028] (3) The substrate after acid etching is subjected to surface activation treatment with colloidal titanium, the surface activation operation temperature is room temperature, and the activation time is 30s;

[0029] (4) Put the activated substrate into the solution A1, at 75° C., the pH value is 2.75, after chemical conversion for 30 minutes, rinse with water to obtain a zinc phosphate chemical conversion coating.

Embodiment 2

[0031] (1) Preparation of chemical conversion solution A: 28g / L zinc oxide, 30ml / L nitric acid, 11ml / L phosphoric acid, 10g / L calcium nitrate, 18g / L citric acid. Then slaking with 5g / L pure iron powder for 12h to obtain chemical conversion solution A1.

[0032] (2) Using 316 medical stainless steel as the substrate, carry out acid etching treatment with 7wt% phosphoric acid, wherein the acid etching temperature is room temperature, and the acid etching time is 10 minutes;

[0033] (3) The substrate after acid etching is subjected to surface activation treatment with colloidal titanium, the surface activation operation temperature is room temperature, and the activation time is 30s;

[0034] (4) Put the activated substrate into the solution A1, at 75° C., the pH value is 2.6, after chemical conversion for 30 minutes, rinse with water to obtain a zinc phosphate chemical conversion coating.

Embodiment 3

[0036] (1) Preparation of chemical conversion solution A: 22g / L zinc oxide, 28ml / L nitric acid, 15ml / L phosphoric acid, 11g / L calcium nitrate, 21g / L citric acid. Then slaking with 5g / L pure iron powder for 24h to obtain chemical conversion solution A1.

[0037] (2) Using 316 medical stainless steel as the substrate, carry out acid etching treatment with 7wt% phosphoric acid, wherein the acid etching temperature is room temperature, and the acid etching time is 10 minutes;

[0038] (3) The substrate after acid etching is subjected to surface activation treatment with colloidal titanium, the surface activation operation temperature is room temperature, and the activation time is 30s;

[0039] (4) Put the activated substrate into the solution A1, at 75° C., the pH value is 2.75, after chemical conversion for 45 minutes, rinse with water to obtain a zinc phosphate chemical conversion coating.

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Abstract

The invention relates to a preparation method of a zinc phosphate chemical conversion coating in a hierarchical structure. The preparation method of the zinc phosphate chemical conversion coating comprises the following steps: preparing a chemical conversion basis solution A, wherein concentration of zinc oxide is 20-28g / L, the concentration of nitric acid is 25-35ml / L, the concentration of phosphoric acid is 10-15ml / L, the concentration of calcium nitride is 5-20g / L, and the concentration of critic acid is 18-22g / L; adding iron powder in to the chemical conversion basis solution, and curing for 12-24 hours at room temperature, so that a curing liquid A1 is obtained; carrying out acidic etching and activation on a stainless steel matrix; placing the activated matrix into the curing liquid A1, carrying out chemical conversion for 15-45 minutes at the temperature of 65-75 DEG C and pH value of 2.5-3.0, and carrying out water washing, so that the zinc phosphate chemical conversion coating is obtained. By adopting the preparation method of the zinc phosphate chemical conversion coating, a uniform dense conversion coating composed of spherical zinc phosphate aggregate which is 2-4 microns in size and composed of nanocrystals is prepared on the surface of medical stainless steel, wettability between a coating layer and simulated body fluid (SBF) is good, and corrosion resistance is good.

Description

technical field [0001] The invention relates to a preparation technology of a chemical conversion film with a novel structure, in particular to a preparation method for a zinc-based phosphate chemical conversion film (Phosphate Chemical conversion) with a graded structure on the surface of a medical stainless steel substrate, and belongs to the technical field of metal surface modification. Background technique [0002] Stainless steel has the advantages of low price, good corrosion resistance, excellent mechanical properties and easy processing, and is widely used in the field of medical implant materials. However, the stainless steel implanted in the body is likely to cause adverse reactions such as inflammation due to the dissolution of nickel ions and chromium ions. Therefore, in order to prevent the dissolution of harmful ions, improve the biocompatibility, the binding force between the film layer and the substrate, and the biological activity, the surface modification ...

Claims

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Application Information

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IPC IPC(8): C23C22/07
Inventor 吕宇鹏张娴肖桂勇
Owner SHANDONG UNIV
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