丙酰胺为沉淀剂水热合成羟基磷灰石纤维

doi:10.3724/SP.J.1077.2013.12254

无机材料学报 ›› 2013, Vol. 28 ›› Issue (1): 63-68.DOI: 10.3724/SP.J.1077.2013.12254 CSTR: 32189.14.SP.J.1077.2013.12254

丙酰胺为沉淀剂水热合成羟基磷灰石纤维

郝丽静, 杨辉, 赵娜如, 王迎军

(华南理工大学国家人体组织功能重建工程技术研究中心, 材料科学与工程学院, 广州510641)

收稿日期:2012-04-21 修回日期:2012-06-13 出版日期:2013-01-10 网络出版日期:2012-12-20
作者简介:郝丽静(1986–), 女, 硕士研究生. E-mail: haolijing709@163.com
基金资助:
国家973科技计划项目(2012CB619100, 2011CB606204);国家自然科学基金重点项目(50732003, U0834003)

Hydrothermal Synthesis of Hydroxyapatite Fibers Precipitated by Propionmide

HAO Li-Jing, YANG Hui, ZHAO Na-Ru, WANG Ying-Jun

(Nation Engineering Research Center for Tissue Restoration and Reconstruction, College of Materials Science and Engineering, South China University of Technology, Guangzhou 510641, China)

Received:2012-04-21 Revised:2012-06-13 Published:2013-01-10 Online:2012-12-20
About author:HAO Li-Jing. E-mail: haolijing709@163.com
Supported by:
National Basic Research Program of China (973 Program) (2012 CB619100, 2011 CB606204);National Natural Science Foundation of China (50732003, U0834003)

摘要/Abstract

摘要：

采用四水硝酸钙和磷酸氢二铵的混合物为前驱体, 以丙酰胺(PA)为沉淀剂来控制溶液的过饱和度, 经水热均相法处理成功制备了高结晶度、形貌均一、分散性良好的纤维状羟基磷灰石(HA)粉体。通过X射线衍射(XRD)、傅里叶红外光谱(FT-IR)、扫描电镜(SEM)和透射电镜(TEM)对所制备的HA进行了表征, 研究了初始pH值和前驱体浓度对HA形貌、组成、结晶度及生长习性的影响。结果表明: 初始pH值较低时有利于纤维状HA粉体的形成, 前驱体浓度较低时则能促进纤维的宽化; 但是初始pH值和前驱体浓度对产物的晶体结构、组成及结晶度影响不大。

关键词: 羟基磷灰石, 丙酰胺, 纤维, 水热法

Abstract:

Fibrous hydroxyapatite (HA) powder was successfully synthesized through hydrothermal method. Calcium nitrate tetrahydrate and diammonium hydrogen phosphate were added as precursors and propionamide (PA) as precipitant was used to control the degree of supersaturation of the reaction solution. XRD, FTIR, SEM and TEM were used to characterize the product. The synthesized HA powder was found to possess high crystallinity and regular morphology, as well as good dispersion. The effects of starting pH value and the concentration of precursors on the morphology, constitution, crystallinity and the growth characteristics of HA were investigated. The results show that the starting pH and concentration significantly affect the morphology at different extents, but not on the constitution and crystallinity. In fact, low starting pH controls orientation of fibrous HA while low concentration widens HA fibers.

Key words: hydroxyapatite, propionamide, fiber, hydrothermal synthesis

中图分类号:

TB321

郝丽静, 杨辉, 赵娜如, 王迎军. 丙酰胺为沉淀剂水热合成羟基磷灰石纤维[J]. 无机材料学报, 2013, 28(1): 63-68.

HAO Li-Jing, YANG Hui, ZHAO Na-Ru, WANG Ying-Jun. Hydrothermal Synthesis of Hydroxyapatite Fibers Precipitated by Propionmide[J]. Journal of Inorganic Materials, 2013, 28(1): 63-68.

图/表 8

Table 1 Formulation and reactional condition of hydrothermal synthesis

[Ca] /(mmol·L^-1)	Initial pH	Final pH
60	1	5.03
60	2	5.46
60	3	5.53
60	4	5.50
60	5	5.58
20	3	5.85
40	3	5.55
80	3	5.33
100	3	5.22

图1 不同初始pH值下HA纤维产物的SEM照片

Fig. 1 SEM images of fibrous HA products under various starting pH values (a) pH=1; (b) pH=2; (c) pH=3; (d) pH=4; (e) pH=5

图2 不同[Ca2+]下HA纤维产物的SEM照片

Fig. 2 SEM images of fibrous HA products under various [Ca2+]

图3 不同初始pH值下HA纤维产物的XRD图谱

Fig. 3 XRD patterns of fibrous HA products under various starting pH value

图4 不同[Ca2+]浓度下HA纤维产物的XRD图谱

Fig. 4 XRD patterns of fibrous HA under various [Ca]

图5 不同初始pH值下HA纤维的FTIR图谱

Fig. 5 FTIR spectra of fibrous HA under various staring pH values

图6 不同[Ca2+]下HA纤维产物的FTIR图谱

Fig. 6 FTIR spectra of fibrous HA under various [Ca2+]

图7 合成HA纤维的TEM照片和选区电子衍射图

Fig. 7 TEM image (a) and SAED pattern (b) of synthesized fibrous HA

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丙酰胺为沉淀剂水热合成羟基磷灰石纤维

Hydrothermal Synthesis of Hydroxyapatite Fibers Precipitated by Propionmide

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