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A kind of preparation method of silicon-doped α-tricalcium phosphate ceramics

A technology of tricalcium phosphate and ceramics, which is applied in the field of preparation of silicon-doped α-tricalcium phosphate ceramics, can solve the problems of energy consumption, large grain size and high preparation temperature, achieve stable α-TCP phase, overcome grain size Coarse, energy-saving effect

Active Publication Date: 2016-10-05
SOUTH CHINA UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The above-mentioned Si-α-TCP preparation temperature is relatively high, the crystal melts and grows, the grain size is large, the grain size cannot be effectively controlled, and more energy is consumed at the same time

Method used

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  • A kind of preparation method of silicon-doped α-tricalcium phosphate ceramics
  • A kind of preparation method of silicon-doped α-tricalcium phosphate ceramics
  • A kind of preparation method of silicon-doped α-tricalcium phosphate ceramics

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Embodiment 1

[0038] The preparation of silicon-doped α-TCP in this embodiment, in this embodiment, the silicon doping amount (relative to the precursor nano-silicon-doped hydroxyapatite powder) is 0-4.0wt%, including the following steps:

[0039] (1) Prepare 0.5mol / L Ca(NO 3 ) 2 4H 2 O solution and 0.25mol / L (NH 4 ) 3 PO 4 ·3H 2 O solution was used as calcium source and phosphorus source respectively, and tetraethyl orthosilicate (TEOS) was used as silicon source. Adjust the amount of calcium source, phosphorus source and silicon source to control the molar ratio of Ca / (P+Si) to 1.67; use ammonia water to adjust the pH of the calcium source to be greater than 11, and the pH of the phosphorus source to be greater than 10, and add the dispersant polyethylene glycol (6000) Stir the calcium source for 30 minutes, add tetraethyl orthosilicate to the phosphorus source and stir for 30 minutes; add the mixed solution of the silicon source and the phosphorus source to the calcium source drop ...

Embodiment 2

[0046] The preparation of silicon-doped α-TCP in this embodiment, the amount of silicon doped in this embodiment (relative to the precursor silicon-doped hydroxyapatite powder) is 0 ~ 4.0wt%, including the following steps:

[0047] (1) Prepare 0.5mol / L Ca(NO 3 ) 2 4H 2 O solution and 0.25mol / L (NH 4 ) 3 PO 4 ·3H 2 O solution was used as calcium source and phosphorus source respectively, and tetraethyl orthosilicate (TEOS) was used as silicon source. Adjust the amount of calcium source, phosphorus source and silicon source to control the molar ratio of Ca / (P+Si) to 1.67; use ammonia water to adjust the pH of the calcium source to be greater than 11, and the pH of the phosphorus source to be greater than 10, and add the dispersant polyethylene glycol (6000) Stir the calcium source for 20 minutes, add tetraethyl orthosilicate to the phosphorus source and stir for 20 minutes; add the mixed solution of the phosphorus source and the silicon source to the calcium source drop by...

Embodiment 3

[0054] The preparation of silicon-doped α-TCP in this embodiment, in this embodiment, the silicon doping amount (relative to the precursor silicon-doped hydroxyapatite) is 0-4.0wt%, including the following steps:

[0055] (1) Prepare 0.5mol / L Ca(NO 3 ) 2 4H 2 O solution and 0.25mol / L (NH 4 ) 3 PO 4 ·3H 2 O solution was used as calcium source and phosphorus source respectively, and tetraethyl orthosilicate (TEOS) was used as silicon source. Adjust the amount of calcium source, phosphorus source and silicon source to control the molar ratio of Ca / (P+Si) to 1.67; use ammonia water to adjust the pH of the calcium source to be greater than 11, and the pH of the phosphorus source to be greater than 10, and add the dispersant polyethylene glycol (6000) Stir the calcium source for 30 minutes, add tetraethyl orthosilicate to the phosphorus source and stir for 30 minutes; add the mixed solution of the silicon source and the phosphorus source to the calcium source drop by drop at 8...

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Abstract

The invention discloses a preparation method of silicon-doped alpha-tricalcium phosphate ceramic. The preparation method comprises the following steps: (1) mixing Ca(NO3)2.4H2O, (NH4)3PO4.3H2O and Si(OCH2CH3)4 of different amounts at a certain temperature according to a molar ratio Ca / (P+Si)=1.67 to obtain precursor nano silicon-doped hydroxyapatite powder; and (2) sintering the precursor nano silicon-doped hydroxyapatite powder in a muffle at 900-1,200 DEG C according to a heating rate of 5-10 DEG C / min, preserving heat for 3-10h, and cooling to normal temperature at a cooling rate of 5-10 DEG C / min to obtain ceramic powder. Compared with the prior art, the method disclosed by the invention can be used for preparing Si-alpha-TCP ceramic powder without beta-TCP at a relatively low temperature, and the content of Si-alpha-TCP can be controlled by controlling the silicon doping amount and the precursor synthesis temperature.

Description

technical field [0001] The invention relates to the preparation of calcium phosphate bioactive materials, in particular to a preparation method of silicon-doped alpha-tricalcium phosphate ceramics. Background technique [0002] α-Tricalcium phosphate (TCP) is an ideal material for bone repair because of its good solubility and osteoinductive properties. Experiments have found that ion doping can significantly affect the solubility, grain size, size, morphology, and physical and chemical properties of the surface of hydroxyapatite bioceramics, thereby affecting the bioactivity and osteoinductive regeneration ability of the ceramics. Bones and teeth contain trace amounts of silicon, and many studies have shown that silicon-containing materials can improve the connection between materials and surrounding tissues and new bone. Therefore, silicon-doped hydroxyapatite materials have been widely concerned. [0003] Silicate in silicon-doped α-TCP (Si-α-TCP) replaces phosphate int...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C04B35/447C04B35/626
Inventor 邓春林董刚郑艳霞王迎军
Owner SOUTH CHINA UNIV OF TECH
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