Electrochemical method for preparing citric acid-hydroxyapatite/zirconia transition coating on surface of biomedical titanium

A hydroxyapatite and electrochemical technology, applied in electrolytic inorganic material coating and other directions, can solve problems such as affecting the stability and durability of the coating, low bonding strength of the coating and the substrate, shortening the service life of the material, etc., to alleviate thermal expansion. The effect of coefficient mismatch, enhanced bonding strength, and high utilization of raw materials

Inactive Publication Date: 2013-05-08
UNIV OF ELECTRONICS SCI & TECH OF CHINA
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Plasma spraying is one of the widely used methods for preparing HA coatings. It has many advantages: simple process, wide range of coating and substrate selection, wide range of coating thickness, high deposition rate and easy formation of composite coatings, etc. But there are also serious problems: (1) the bonding strength between the coating and the substrate is low
The process temperature of plasma spraying is very high. At high temperature, HA crystals decompose to form amorphous phases (ACP, TCP, CaO, etc.), which affect the stability and durability of the coating in the body. Due to the existence of these amorphous phases, crystallization degree alone cannot reflect the quality of the coating
[0004] The disadvantages of low bonding strength and low crystallinity between the HA coating and the Ti matrix make the coating have potential problems such as shedding and dissolution under the action of force and erosion of biological fluids, which shortens the service life of the material

Method used

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  • Electrochemical method for preparing citric acid-hydroxyapatite/zirconia transition coating on surface of biomedical titanium
  • Electrochemical method for preparing citric acid-hydroxyapatite/zirconia transition coating on surface of biomedical titanium
  • Electrochemical method for preparing citric acid-hydroxyapatite/zirconia transition coating on surface of biomedical titanium

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] (1) Wire-cut medical pure titanium into 10×10×1mm titanium sheets; grind the titanium sheets with sandpaper until the surface is smooth without machining traces; respectively use absolute ethanol, acetone, and deionized water with ultrasonic waves Cleaning time is 10min; then use HF:HNO 3 :H 2 O=1:1:10 acid solution for acid etching; finally anodizing treatment (voltage 20V, time 15min) to obtain a titanium sheet with a rough and uniform surface; use deionized water and ultrasonic cleaning for 10min. Put the sample into the sample bag with tweezers, ready for experiment.

[0026] (2) The Ti sheet was used as the cathode working electrode, the platinum electrode was used as the counter electrode, and the saturated calomel electrode was used as the reference electrode, and the distance between the electrodes was 2.5 cm.

[0027] (3) Weigh 0.5781g of anhydrous zirconium oxynitrate, dissolve it with 100ml of hot dilute nitric acid, set the volume to 200ml after cooling, s...

Embodiment 2

[0033] (1) Wire-cut medical pure titanium into 10×10×1mm titanium sheets; grind the titanium sheets with sandpaper until the surface is smooth without machining traces; respectively use absolute ethanol, acetone, and deionized water with ultrasonic waves Cleaning time is 10min; then use HF:HNO 3 :H 2 O=1:1:10 acid solution for acid etching; finally anodizing treatment (voltage 20V, time 15min) to obtain a titanium sheet with a rough and uniform surface; use deionized water and ultrasonic cleaning for 10min. Put the sample into the sample bag with tweezers, ready for experiment.

[0034] (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 2.5 cm.

[0035] (3) Weigh 1.1562g of anhydrous zirconium oxynitrate, dissolve it with 100ml of hot dilute nitric acid, set the volume to 200ml after cooling, stir the beaker...

Embodiment 3

[0039] (1) Wire-cut medical pure titanium into 10×10×1mm titanium sheets; grind the titanium sheets with sandpaper until the surface is smooth without machining traces; respectively use absolute ethanol, acetone, and deionized water with ultrasonic waves Cleaning time is 10min; then use HF:HNO 3 :H 2 O=1:1:10 acid solution for acid etching; finally anodizing treatment (voltage 20V, time 15min) to obtain a titanium sheet with a rough and uniform surface; use deionized water and ultrasonic cleaning for 10min. Put the sample into the sample bag with tweezers, ready for experiment.

[0040] (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 2.5 cm.

[0041] (3) Weigh 1.1562g of anhydrous zirconium oxynitrate, dissolve it with 100ml of hot dilute nitric acid, set the volume to 200ml after cooling, stir the beaker...

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Abstract

The invention discloses an electrochemical method for preparing a citric acid-hydroxyapatite / zirconia transition coating on the surface of biomedical titanium. The electrochemical method comprises the following steps of 1, carrying out electrodeposition in an electrolytic cell with a three-electrode system by based on a biomedical titanium slice as a work electrode, carrying out electrodeposition in a zirconium oxynitrate solution having a certain concentration and a certain pH at an electrodeposition electric current of 11.1mA for 50s to obtain a Zr(OH)4 coating and carrying out electrodeposition in an electrolyte which is composed of calcium nitrate, ammonium dihydrogen phosphate, sodium citrate and hydrogen peroxide and has a certain concentration and a certain pH at an electrodeposition electric current of 0.9mA for 2700s to obtain a citric acid-modified HA(Cit-HA) coating, and 2, carrying out vacuum sintering at a temperature of 450 DEG C to obtain the citric acid-hydroxyapatite / zirconia transition coating. Citric acid radical prolongs a nucleation period of HA crystals. A micron-size chrysanthemum petal shape of the coating is changed into a nano-size needle shape. The HA coating realizes transition from an inner compact layer to an outer loose layer. ZrO2 is used as a transition layer between a titanium matrix and the HA coating, and the Cit-HA / ZrO2 transition coating has high bonding strength with the Ti matrix. A late-stage simulated body fluid immersion experiment proves that the Cit-HA / ZrO2 transition coating has good biological activity.

Description

technical field [0001] The invention relates to a method for preparing a citric acid-hydroxyapatite / zirconia transition coating on the surface of a medical metal material by constant current electrodeposition, and is especially suitable for the bioactive coating on the surface of a dental implant biometal material preparation. Background technique [0002] At present, a research and development focus of hard tissue implants focuses on coating HA on the surface of titanium alloy. The obtained material not only has the strength and toughness of the base metal, but also has the bioactivity and biocompatibility of HA, so that the overall function Get a durable and reliable implant material close to natural bone. [0003] Plasma spraying is one of the widely used methods for preparing HA coatings. It has many advantages: simple process, wide range of coating and substrate selection, wide range of coating thickness, high deposition rate and easy formation of composite coatings, e...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C25D9/08
Inventor 庞小峰黄勇严雅静
Owner UNIV OF ELECTRONICS SCI & TECH OF CHINA
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