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Preparation method of homoporous biological ceramic implant material having gradient calcium and phosphor content

A technology of bioceramics and implants, applied in the direction of electrolytic coatings, coatings, surface reaction electrolytic coatings, etc., can solve the problem that the oxidation voltage and frequency should not be too high, the ceramic layer lacks a gradient of calcium and phosphorus content, and it is difficult to adjust the calcium and phosphorus content. Pore ​​structure and other issues, to achieve good osteoinduction and osseointegration performance, uniform micropores, and good biocompatibility

Inactive Publication Date: 2014-02-26
SHANDONG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, due to the influence of the unchangeable concentration of calcium and phosphorus ions in the electrolyte, the inner layer of the ceramic layer contains less calcium and phosphorus elements, and the entire ceramic layer lacks the necessary gradient of calcium and phosphorus content; also due to the limitation of the temperature of the electrolyte (usually 40°C), so that the oxidation voltage and frequency of the process should not be too high, and the pores formed are not ideal
Therefore, it is difficult for the ceramic layer to obtain the calcium and phosphorus content and pore structure that are beneficial to the initial osteoinduction and osseointegration of the implant.

Method used

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  • Preparation method of homoporous biological ceramic implant material having gradient calcium and phosphor content
  • Preparation method of homoporous biological ceramic implant material having gradient calcium and phosphor content
  • Preparation method of homoporous biological ceramic implant material having gradient calcium and phosphor content

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Effect test

Embodiment 1

[0019] Perform micro-arc oxidation treatment on titanium or titanium alloy in 1L of ice-water mixed low-temperature electrolyte containing calcium and phosphorus, freeze deionized water (or distilled water) into 1L of ice and place it in the electrolyte. The process parameters are: constant voltage micro-arc oxidation process, electrode voltage U=650V, electrode frequency f=800Hz, duty cycle d=15%, micro-arc oxidation treatment time t=20min; electrolyte contains calcium ion concentration C( Ca)=15mmol / L, phosphorus ion concentration C(P)=3mmol / L. The surface micropores of the oxide film obtained by treating the titanium surface with this process are uniform and uniform, and the phase composition is anatase TiO 2 + rutile phase TiO 2 +CaTiO 3 +PO 4 3- group, the thickness of the oxide film is 22.8 μm, the Ca / P in the oxide film is 1.608, the critical load value is 29.7N, and the maturation period of the bone interface is shortened from 3 to 6 months for titanium implants to...

Embodiment 2

[0021] Perform micro-arc oxidation treatment on titanium or titanium alloy in 1L of ice-water mixed low-temperature electrolyte containing calcium and phosphorus, freeze deionized water (or distilled water) into 1L of ice and place it in the electrolyte. The process parameters are: constant voltage micro-arc oxidation process, electrode voltage U=600V, electrode frequency f=700Hz, duty cycle d=15%, micro-arc oxidation treatment time t=25min; electrolyte contains calcium ion concentration C( Ca)=20mmol / L, phosphorus ion concentration C(P)=4mmol / L. The micropores on the surface of the oxide film obtained by treating the titanium surface with this process are uniform and uniform.

Embodiment 3

[0023] Perform micro-arc oxidation treatment on titanium or titanium alloy in 1L of ice-water mixed low-temperature electrolyte containing calcium and phosphorus, freeze deionized water (or distilled water) into 1L of ice and place it in the electrolyte. The process parameters are: constant voltage micro-arc oxidation process, electrode voltage U=700V, electrode frequency f=900Hz, duty cycle d=20%, micro-arc oxidation treatment time t=15min; electrolyte contains calcium ion concentration C( Ca)=10mmol / L, phosphorus ion concentration C(P)=2mmol / L. The micropores on the surface of the oxide film obtained by treating the titanium surface with this process are uniform and consistent.

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Abstract

The invention relates to a preparation method of a homoporous biological ceramic implant material having gradient calcium and phosphor content. The preparation method comprises the following steps of 1, low-temperature electrolyte preparation: preparing an electrolyte having a calcium ion concentration C(Ca) of 8-30mmol / L and a phosphorus ion concentration C(P) of 2-5mmol / L by deionized water, freezing deionized water and putting the freezed deionized water into the electrolyte to obtain an ice-water mixed low-temperature electrolyte, and 2, micro-arc oxidation treatment on titanium or a titanium alloy in the low-temperature electrolyte. Micropores of the ceramic membrane on the surface of the implant material have the same sizes and are uniform; gradient calcium and phosphor content is realized in the membrane and the inner membrane contains more calcium and phosphor elements; compared with a bone-implant interface mature period of the existing titanium implant tooth, a bone-implant interface mature period of the homoporous biological ceramic implant material is shortened to be within 3 months from 3-6 months; and biological properties satisfy prescribes of ISO, Chinese pharmacopoeia and American pharmacopeia.

Description

technical field [0001] The invention relates to a preparation method of a biomedical implant material, in particular to a preparation method of a fine-pore bioceramic implant material containing calcium and phosphorus elements. Background technique [0002] Titanium and titanium alloys are implant materials with a wide range of applications. They have good biocompatibility, but they have no biological activity. It is difficult to form a chemical bond with bone directly in the early stage of implantation, and the healing time is long. In order to improve its biological activity, plasma spraying, ion sputtering, electrophoresis, microwave sintering and other technologies are currently used to prepare hydroxyapatite and bioactive glass coatings on its surface, or to prepare titanium dioxide or sodium titanate by chemical activation treatment. Gel bioactive films, but these coatings or films have obvious interfaces with titanium and titanium alloy substrates, and the bonding str...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C25D11/26
Inventor 朱瑞富王宏元吕宇鹏王晓亭
Owner SHANDONG UNIV
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