Method for preparing calcium hydrophosphate micro-nanofiber conversion coating on pure-titanium surface

A calcium hydrogen phosphate micro-nano, conversion coating technology, applied in medical science, metal material coating technology, prosthesis and other directions, can solve the problems of no retrieval, no mention of calcium-containing conversion coating, difficult film formation, etc.

Active Publication Date: 2015-09-30
SHANDONG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, titanium is an inert metal, and there is a stable oxide film on the surface. Ti does not participate in the reaction during the conversion process, so it is difficult to form a film with general conversion solution and conversion method.
It is worth mentioning that the patent CN103952745A discloses a method for preparing a zinc

Method used

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  • Method for preparing calcium hydrophosphate micro-nanofiber conversion coating on pure-titanium surface
  • Method for preparing calcium hydrophosphate micro-nanofiber conversion coating on pure-titanium surface

Examples

Experimental program
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Effect test

Embodiment 1

[0025] The preparation method of a kind of calcium hydrogen phosphate micro-nano fiber conversion film on the surface of pure titanium described in this embodiment, its specific steps are as follows:

[0026] (1) 85wt%H 3 PO 4 7ml / L, Ca(H 2 PO 4 ) 2 ·H 2 O 8g / L, Zn(H 2 PO 4 ) 2 2H 2 O 1.55g / L, NaNO 3 2g / L, NaNO 2 2g / L were mixed in sequence to prepare a chemical conversion solution.

[0027] (2) Add 5 g / L of reduced iron powder into the chemical conversion solution, leave it to mature at room temperature for 16 hours, and filter to obtain the supernatant.

[0028] (3) with H 3 PO 4 and NaOH to adjust the pH of the chemical transformation base solution to 5.00.

[0029] (4) Put the polished pure titanium substrate into 2wt% HF solution, activate it for 15s at room temperature, rinse the activated pure titanium substrate several times with deionized water, put the rinsed pure titanium substrate into the colloid In the titanium solution (titanium-containing phospha...

Embodiment 2

[0033] The preparation method of a kind of calcium hydrogen phosphate micro-nano fiber conversion film on the surface of pure titanium described in this embodiment, its specific steps are as follows:

[0034] (1) 85wt%H 3 PO 4 8ml / L, Ca(H 2 PO 4 ) 2 ·H 2 O 9g / L, Zn(H 2 PO 4 ) 2 2H 2 O 2g / L, NaNO 3 2.5g / L, NaNO 2 2.5g / L were mixed in sequence to prepare a chemical conversion solution.

[0035] (2) Add 6 g / L of reduced iron powder into the chemical transformation solution, leave it to mature at room temperature for 18 hours, and filter to get the supernatant.

[0036] (3) with H 3 PO 4 and NaOH to adjust the pH of the chemical transformation base solution to 5.00.

[0037] (4) Put the polished pure titanium substrate into 2wt% HF solution, activate it for 15s at room temperature, rinse the activated pure titanium substrate several times with deionized water, put the rinsed pure titanium substrate into the colloid In the titanium solution (titanium-containing phosp...

Embodiment 3

[0041] (1) 85wt%H 3 PO 4 10ml / L, Ca(H 2 PO 4 ) 2 ·H 2 O 15g / L, Zn(H 2 PO 4 ) 2 2H 2 O 4g / L, NaNO 3 3g / L, NaNO 2 4g / L mixed in sequence to prepare a chemical conversion solution.

[0042] (2) Add 7 g / L of reduced iron powder into the chemical conversion solution, leave it to mature at room temperature for 24 hours, and filter to obtain the supernatant.

[0043] (3) with H 3 PO 4 and NaOH to adjust the pH of the chemical transformation base solution to 5.00.

[0044] (4) Put the polished pure titanium substrate into 2wt% HF solution, activate it for 15s at room temperature, rinse the activated pure titanium substrate several times with deionized water, put the rinsed pure titanium substrate into the colloid In the titanium solution (titanium-containing phosphate colloidal solution), the surface is adjusted for 30s at room temperature.

[0045] (5) Coupling the pure titanium sample treated in step (4) with pure iron, first acting in a 250w ultrasonic field for 20 m...

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Abstract

The invention relates to a method for preparing a calcium hydrophosphate micro-nanofiber conversion coating on a pure-titanium surface. A method that under the proper pH-value condition, a chemical conversion solution carries out chemical conversion treatment on the pure-titanium surface is adopted, and a chemical conversion solution is a solution composed of the proper amount of phosphoric acid, compounds containing calcium ions, zinc ions and dihydrogen phosphates, and an accelerant; and according to chemical conversion treatment, a pure-titanium sample obtained after proper activation treatment and surface adjustment is coupled with pure iron, then, ultrasonic field manufacturing and water bath heating are carried out, and the calcium hydrophosphate micro-nanofiber conversion coating on the pure-titanium surface is obtained. A phase of the conversion coating prepared on the pure-titanium surface through the method is a CaHPO4 2H2O crystal, and a crystal aggregate can induce and promote formation of hydroxyapatite (HA) in simulated body fluid; and the formed conversion coating is of a micro-nano fiber-shaped structure close to a human body multi-level micro-nano structure, and the method has the important significance in regulating and controlling cells, the tissue reaction and the like.

Description

technical field [0001] The invention relates to a preparation method of calcium hydrogen phosphate micro-nano fiber conversion film on the surface of pure titanium, and belongs to the technical field of surface modification of biomedical metal materials. Background technique [0002] Calcium hydrogen phosphate dihydrate (CaHPO 4 2H 2 O) It has been proved to have good biocompatibility because it is similar to the chemical substance of the calcified tissue of the organism, and it is non-toxic, has no immune rejection, has absorbability, and has a good osseointegration effect in the process of bone mineralization, It is widely used in biomedical fields such as dentistry and plastic surgery. Studies have proved that calcium hydrogen phosphate can be directly converted into hydroxyapatite (HA) by homogeneous precipitation method, and many researchers use it as the precursor to form HA film. The elastic modulus of pure titanium is similar to that of bone, and it has high speci...

Claims

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Application Information

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IPC IPC(8): C23C22/07C23C22/80A61L27/06A61L27/32A61L27/50
Inventor 吕宇鹏刘冰肖桂勇
Owner SHANDONG UNIV
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