明胶溶液中沉淀法制备纯相β-磷酸三钙

doi:10.7517/j.issn.1674-0475.2012.04.269

影像科学与光化学 ›› 2012, Vol. 30 ›› Issue (4): 269-279.DOI: 10.7517/j.issn.1674-0475.2012.04.269

明胶溶液中沉淀法制备纯相β-磷酸三钙

马铭^1,2, 王雪松¹, 张兵¹, 郭燕川¹

1. 中国科学院理化技术研究所, 北京100190;
2. 中国科学院研究生院, 北京100049

收稿日期:2012-02-10 修回日期:2012-03-28 出版日期:2012-07-15 发布日期:2012-07-15
通讯作者: 郭燕川
基金资助:
北京市自然科学基金(2093035).

Synthesis of Pure β-Ca₃(PO₄)₂ Bioceramics with Gelatin by Precipitation Method

MA Ming^1,2, WANG Xue-song¹, ZHANG Bing¹, GUO Yan-chuan¹

1. Technical Institute of Physics and Chemistry, Chinese Academy of Sciences, Beijing 100190, P.R.China;
2. Graduate University of Chinese Academy of Sciences, Beijing 100049, P.R.China

Received:2012-02-10 Revised:2012-03-28 Online:2012-07-15 Published:2012-07-15
Supported by:
Nature Science Foundation of Beijing (2093035).

摘要/Abstract

摘要： 本文以明胶、硝酸钙Ca(NO₃)₂和磷酸氢二铵(NH₄)₂HPO₄为前驱体,初始Ca/P为1.5,制备了纯相的β-磷酸三钙.红外谱图和X射线晶体衍射结果表明,溶液中直接沉淀得到的产物为缺钙磷灰石,该产物在明胶浓度≥0.22 %(质量分数)时热转化为纯相的β-磷酸三钙.通过晶体尺寸计算和比表面积测定,缺钙磷灰石的晶体大小随着明胶用量的增加而变小.透射电镜结果显示溶液中直接沉淀的缺钙磷灰石呈针状形貌,经过高温煅烧后,针状的缺钙磷灰石将相互融合形成葡萄状的β-磷酸三钙.差热/热重结果表明,明胶与生成的缺钙磷灰石形成了化学键合,这将有助于吸附较多的水分子,随后水分子与缺钙磷灰石发生化学反应生成羟基磷灰石,羟基磷灰石继续与沉淀中的偏磷酸钙反应生成β-磷酸三钙.本文还研究了明胶对纯相β-磷酸三钙的生成机理.

关键词: 明胶, 纯相β-磷酸三钙, 缺钙磷灰石, 骨修复, 沉淀法

Abstract: Pure β-tricalcium phosphate (β-TCP) was synthesized using the precipitation method, starting from the gelatin, Ca (NO₃)₂ and (NH₄)₂HPO₄ precursors by adopting the initial Ca/P ratio of 1.5. FT-IR spectroscopy and X-ray diffractometry indicated the solution derived precipitate was calcium deficient phosphate (Ca-dHAP) and it would thermally transform into pure β-TCP as the amount of gelatin exceeds 0.22% (mass concentration). The Ca-dHAP crystal dimensions decreased with increasing gelatin amount as shown by crystallite calculation and SSA measurement. TEM results showed that the as prepared Ca-dHAP powders were needle-like and formed a botryoidal shape characteristic of β-TCP when being calcined at high temperatures. The DTA/TG results showed that gelatin chemically bonded with the Ca-dHAP crystals which could be beneficial for the absorption of water molecules and the absorbed water molecules, then subsequently reacted with Ca-dHAP to form HA which would react with a second phase calcium pyrophosphate (Ca₂P₂O₇) (CPP) to prepare pure β-TCP. In this paper, we also studied the mechanism of gelatin on the formation of β-TCP.

Key words: gelatin, pure β-TCP, Ca-dHAP, bone repair, precipitation

中图分类号:

马铭, 王雪松, 张兵, 郭燕川. 明胶溶液中沉淀法制备纯相β-磷酸三钙[J]. 影像科学与光化学, 2012, 30(4): 269-279.

MA Ming, WANG Xue-song, ZHANG Bing, GUO Yan-chuan. Synthesis of Pure β-Ca₃(PO₄)₂ Bioceramics with Gelatin by Precipitation Method[J]. Imaging Science and Photochemistry, 2012, 30(4): 269-279.

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明胶溶液中沉淀法制备纯相β-磷酸三钙

Synthesis of Pure β-Ca₃(PO₄)₂ Bioceramics with Gelatin by Precipitation Method

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明胶溶液中沉淀法制备纯相β-磷酸三钙

Synthesis of Pure β-Ca3(PO4)2 Bioceramics with Gelatin by Precipitation Method

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Synthesis of Pure β-Ca₃(PO₄)₂ Bioceramics with Gelatin by Precipitation Method