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Electrochemical method for preparing HA/ZrO2 (hydroxylapatite/zirconia) gradient coating on surface of medical titanium

A hydroxyapatite and gradient coating technology, applied in the direction of coating, electrolysis process, electrolysis components, etc., can solve the problems of affecting the mechanical properties of the coating, poor coating dispersion, agglomeration of component particles, etc. Corrosion resistance and biocompatibility, mitigation of thermal expansion coefficient mismatch, uniform and dense coating effect

Inactive Publication Date: 2010-11-10
UNIV OF ELECTRONIC SCI & TECH OF CHINA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

There are still some problems with plasma spray coating materials: (1) due to the linear spraying process, the surface coating of the rough substrate is uneven and the surface coating of the complex shape substrate cannot be carried out; (2) the gap between the coating and the substrate during the cooling process High residual interfacial stress is generated, even causing cracks in the coating, causing the coating to loosen or fall off; (3) The high temperature process in spraying can easily decompose HA and generate Ca in the coating. 3 (PO 4 ) 2 and heterogeneous phases such as amorphous HA, thus affecting the biological properties of the coating
During electrophoretic deposition, HA and ZrO 2 Both exist in the electrolyte in the form of powder, so that ZrO 2 The dispersion of particles in the coating is not good, which affects the mechanical properties of the coating, and the coating is prone to agglomeration of the particles of each component, and the overall performance of the final coating is poor
The main disadvantage of magnetron sputtering is that the obtained coating is too thin and dissolves quickly in the body

Method used

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  • Electrochemical method for preparing HA/ZrO2 (hydroxylapatite/zirconia) gradient coating on surface of medical titanium
  • Electrochemical method for preparing HA/ZrO2 (hydroxylapatite/zirconia) gradient coating on surface of medical titanium
  • Electrochemical method for preparing HA/ZrO2 (hydroxylapatite/zirconia) gradient coating on surface of medical titanium

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] (1) Wire-cut medical pure titanium into 1×1×0.1cm titanium sheets; grind the titanium sheets with sandpaper until the surface is smooth without machining traces; use absolute ethanol, acetone, and deionized water to mix Ultrasonic cleaning, the time is 8min; then use HF:HNO 3 :H 2 O=1:1:8 acid solution for acid etching; finally use deionized water and ultrasonic cleaning for 8 minutes. Put the sample into the sample bag with tweezers, ready for experiment.

[0027] (2) The Ti sheet was used as the cathode working electrode, the platinum electrode was used as the counter electrode, and saturated calomel was used as the reference electrode, and the distance between the electrodes was 3 cm.

[0028] (3) Weigh 0.5781g of anhydrous zirconyl nitrate, dissolve it with 100ml of dilute nitric acid, then set the volume to 200ml, place the beaker on a magnetic stirrer and stir, adjust the pH of the solution to 2.3 with ammonia water, and finally obtain a uniform electrolyte. Th...

Embodiment 2

[0034] (1) Wire-cut medical pure titanium into 1×1×0.1cm titanium sheets; grind the titanium sheets with sandpaper until the surface is smooth without machining traces; use absolute ethanol, acetone, and deionized water to mix Ultrasonic cleaning, the time is 8min; then use HF:HNO 3 :H 2 O=1:1:8 acid solution for acid etching; finally use deionized water and ultrasonic cleaning for 8 minutes. Put the sample into the sample bag with tweezers, ready for experiment.

[0035] (2) The Ti sheet was used as the cathode working electrode, the platinum electrode was used as the counter electrode, and saturated calomel was used as the reference electrode, and the distance between the electrodes was 3 cm.

[0036] (3) Weigh 1.1562 g of anhydrous zirconyl nitrate, dissolve it with 100 ml of dilute nitric acid, then set the volume to 200 ml, place the beaker on a magnetic stirrer and stir, adjust the pH of the solution to 2.3 with ammonia water, and finally obtain a uniform electrolyte. ...

Embodiment 3

[0040] (1) Wire-cut medical pure titanium into 1×1×0.1cm titanium sheets; grind the titanium sheets with sandpaper until the surface is smooth without machining traces; use absolute ethanol, acetone, and deionized water to mix Ultrasonic cleaning, the time is 8min; then use HF:HNO 3 :H 2 O=1:1:8 acid solution for acid etching; finally use deionized water and ultrasonic cleaning for 8 minutes. Put the sample into the sample bag with tweezers, ready for experiment.

[0041] (2) The Ti sheet was used as the cathode working electrode, the platinum electrode was used as the counter electrode, and saturated calomel was used as the reference electrode, and the distance between the electrodes was 3 cm.

[0042] (3) Weigh 1.7343g of anhydrous zirconyl nitrate, dissolve it with 100ml of dilute nitric acid, then set the volume to 200ml, place the beaker on a magnetic stirrer and stir, adjust the pH of the solution to 2.3 with ammonia water, and finally obtain a uniform electrolyte. Th...

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Abstract

The invention discloses an electrochemical method for preparing a HA / ZrO2 (hydroxylapatite / zirconia) gradient coating on the surface of medical titanium. The method comprises the following steps of: carrying out electro-deposition in an electrolytic cell with a three-electrode system, wherein the medical titanium to be coated is a working electrode; carrying out electro-deposition to obtain a Zr (OH) 4 coating in a zirconium oxynitrate solution with certain concentration and pH value, wherein the deposition current is 20mA, and the deposition time is 600s; then, depositing a CaHPO42H2O coating in an electrolyte which has certain concentration and pH value and consists of calcium nitrate and ammonium dihydrogen phosphate, wherein the deposition current is 1.5mA, and the deposition time is 900s; and finally, carrying out vacuum sintering on the obtained coating materials, and raising the sintering temperature to 650 DEG C at a heating rate of 10 DEG C / min, then preserving the heat for two hours, and subsequently cooling the coating materials with a furnace so as to obtain the HA / ZrO2 composite coating. The electrochemical method of the invention has the advantages that: the ingredients of the coating are deposited on a substrate in the form of ions, so that the bonding strength of the HA / ZrO2 gradient coating and the Ti substrate is improved greatly; and the anti-corrosion and simulated body fluid experiment shows that even the HA on the surface is dissolved completely due to the biological effect, the remaining ZrO2 coating still has good anti-corrosion performance and certain biocompatibility.

Description

technical field [0001] The invention relates to a preparation method for preparing a hydroxyapatite / zirconia gradient coating on the surface of a medical biological material by constant current electrodeposition, and is especially suitable for the preparation of a bioactive coating on the surface of a dental implant biometal material. Background technique [0002] Hydroxyapatite [Ca 10 (PO 4 ) 6 (OH) 2 ] is the main inorganic component of vertebrate bones and teeth, has excellent biocompatibility, and can react with the bone tissue of the body to form a chemical bond. Under the action of body fluids, HA will partially degrade, release free calcium and phosphorus, be absorbed and utilized by human tissues, induce the growth of new tissues, and thus produce bone conduction, which has attracted extensive attention from material workers and medical workers. . At present, a research and development focus of hard tissue implants focuses on coating HA on the surface of titaniu...

Claims

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Application Information

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IPC IPC(8): C25B1/20C25B1/00A61L27/32
Inventor 庞小峰黄勇何从军曹郁
Owner UNIV OF ELECTRONIC SCI & TECH OF CHINA
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