造孔剂和发泡剂结合法制备氟化羟基磷灰石多孔支架研究

doi:10.3724/SP.J.1077.2014.13309

无机材料学报 ›› 2014, Vol. 29 ›› Issue (3): 289-293.DOI: 10.3724/SP.J.1077.2014.13309 CSTR: 32189.14.SP.J.1077.2014.13309

造孔剂和发泡剂结合法制备氟化羟基磷灰石多孔支架研究

巩梦安^1,2, 饶群力¹, 王鸿烈³

(1. 上海交通大学分析测试中心, 上海200240; 2. 上海交通大学微纳科学技术研究院, 上海200240; 3. 密歇根大学口腔医学系, 密歇根州48109)

收稿日期:2013-06-15 修回日期:2013-08-21 出版日期:2014-03-20 网络出版日期:2014-02-18
作者简介:巩梦安(1990-), 男, 硕士研究生. E-mail:zhizhedayu@163.com
基金资助:
上海交通大学研究生创新能力培养专项基金(z-404-001)

A Novel Technique to Prepare Porous 3D Fluoridated Hydroxyapatite Scaffold Using Pore-forming and Foaming Agents

GONG Meng-An^1,2, Rao Qun-Li¹, WANG Hong-Lie³

(1. Instrumental Analysis Center, Shanghai Jiao Tong University, Shanghai 200240, China; 2. Research Institute of Micro/Nano Science and Technology, Shanghai Jiao Tong University, Shanghai 200240, China; 3. Department of Oral Medicine, University of Michigan, Michigan 48109, America)

Received:2013-06-15 Revised:2013-08-21 Published:2014-03-20 Online:2014-02-18
About author:GONG Meng-An. E-mail:zhizhedayu@163.com
Supported by:
Graduate Creative Ability Special Fund of Shanghai Jiao Tong University(z-404-001)

摘要/Abstract

摘要：

本研究采用添加造孔剂和发泡剂相结合法制备多孔氟化羟基磷灰石, 合成具有大孔与小孔套连、3D方向上分布的多孔支架。通过化学沉淀法制备了氟化羟基磷灰石(FHA)粉体, 以碳酸氢铵为发泡剂、PMMA为造孔剂, 通过烘干和烧结工艺制备孔洞均匀且相互贯通、坯体致密的多孔支架。经X射线衍射分析, 支架的相组成是FHA和β-TCP。SEM观察结果显示支架孔洞形貌规整、大孔尺寸100~400 µm, 小孔尺寸10~50 µm。以HA和β-TCP为原料对造孔方法的普适性进行验证, 并对支架孔的形成及其影响因素进行了分析。

关键词: 碳酸氢铵, PMMA, 氟化羟基磷灰石, 多孔支架

Abstract:

A novel technology using pore-forming agent and foaming agent was developed to prepare multi-porous fluoridate hydroxyapatite scaffolds. With this technology, scaffolds were produced with uniform and highly interconnected pores in which large pores containing small ones on their walls distributing along 3-dimension. First, the precursor, FHA powder, was prepared by chemical precipitation method. Then it was used to form scaffold through heat treatments by adding ammonium bicarbonate as foaming agent and polymethyl methacrylate as pore-forming agent, and a dense frame of multi-porous structure was obtained. Investigated by X-ray diffraction (XRD), a dual-phase of FHA/β-TCP in scaffold was confirmed. The uniform morphology in scaffolds and the pore size distribution of large pores (100-400 µm) containing small ones (10~50 µm) were demonstrated by SEM images. HA and β-TCP were also used to prove the universality of this method. Furthermore, the pore formation and its mechanism were discussed in detail.

Key words: ammonium bicarbonate, polymethyl methacrylate, fluoridated hydroxyapatite, multi-porous scaffold

中图分类号:

TQ174

巩梦安, 饶群力, 王鸿烈. 造孔剂和发泡剂结合法制备氟化羟基磷灰石多孔支架研究[J]. 无机材料学报, 2014, 29(3): 289-293.

GONG Meng-An, Rao Qun-Li, WANG Hong-Lie. A Novel Technique to Prepare Porous 3D Fluoridated Hydroxyapatite Scaffold Using Pore-forming and Foaming Agents[J]. Journal of Inorganic Materials, 2014, 29(3): 289-293.

图/表 6

图1 HA粉体(a)、FHA粉体(b)、β-TCP粉体(c)、1000℃ 烧结的FHAP粉体(d)和FHA支架研磨后粉体(e)的XRD图谱

Fig. 1 XRD patterns for HA(a), FHA(b), β-TCP(c), Sintered FHA at 1000℃(d) and FHA scaffold(e)

图2 化学沉淀法制备的FHA粉体SEM低倍(a)和高倍(b)照片

Fig. 2 SEM images of FHA powders prepared by chemical precipitation method at low (a) and high (b) magnification

图3 不同热处理方法制备的多孔FHA支架的SEM照片

Fig.3 SEM images of prepared porous FHA scaffolds under different heat treatments (a) Drying at 50℃; (b) Sintered at 1000℃

图4 烧结的多孔FHA支架结构的孔(a)和孔壁(b)SEM照片

Fig. 4 SEM images of porous FHA scaffold showing the sintered structure of pores (a) and wall of pore (b)

图5 不同热处理工艺下多孔支架的SEM照片

Fig. 5 SEM images of porous FHA scaffold under different heat treatment processes (a) Sintered at 1000℃ without ammonium bicarbonate; (b) Drying at 35℃; (c) Drying at 60℃; (d) Sintered at the rate of 5℃/min to 1000℃

图6 1000℃烧结的HA(a)和β-TCP(b)多孔支架结构的SEM照片

Fig. 6 SEM images of HA (a) and β-TCP (b) scaffold showing the sintered porous structure

参考文献 14

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造孔剂和发泡剂结合法制备氟化羟基磷灰石多孔支架研究

A Novel Technique to Prepare Porous 3D Fluoridated Hydroxyapatite Scaffold Using Pore-forming and Foaming Agents

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