铁掺杂羟基磷灰石的制备及在强磁场中的定向研究

doi:10.15541/jim20170137

无机材料学报 ›› 2018, Vol. 33 ›› Issue (1): 75-80.DOI: 10.15541/jim20170137 CSTR: 32189.14.10.15541/jim20170137

铁掺杂羟基磷灰石的制备及在强磁场中的定向研究

王小龙^1,2, 任忠鸣¹, 常江²

1. 上海大学省部共建高品质特殊钢冶金与制备国家重点实验室, 上海市钢铁冶金新技术开发应用重点实验室, 材料科学与工程学院, 上海200072;
2.中国科学院上海硅酸盐研究所, 上海200050

收稿日期:2017-03-24 修回日期:2017-06-06 出版日期:2018-01-23 网络出版日期:2017-12-15
作者简介:王小龙(1990-), 男, 硕士研究生. E-mail: 1990.wangxiaolong@163.com
基金资助:
国家自然基金重点项目(81430012) National Natural Science Foundation of China (81430012)

Synthesis and Orientation of Fe-doped Hydroxyapatite in High Magnetic Field

WANG Xiao-Long^1,2, REN Zhong-Ming¹, CHANG Jiang²

1. State Key Laboratory of Advanced Special Steel, Shanghai Key Laboratory of Advanced Ferrometallurgy, School of Materials Science and Engineering, Shanghai University, Shanghai 200072, China;
2. Shanghai Institute of Ceramics, Chinese Academy of Sciences, Shanghai 200050, China

Received:2017-03-24 Revised:2017-06-06 Published:2018-01-23 Online:2017-12-15
Supported by:
National Natural Science Foundation of China (81430012)

摘要/Abstract

摘要：

生物陶瓷表面纳米结构能够影响成骨细胞增殖和分化, 其表面微观结构的控制, 特别是烧结前晶粒取向调控, 是设计开发生物活性陶瓷的关键之一。针对羟基磷灰石晶粒取向调控问题, 重点研究了铁掺杂羟基磷灰石晶体在强磁场中的取向。分别采用共沉淀法和共沉淀-水热法合成了羟基磷灰石(HA)和铁-羟基磷灰石(Fe-HA), 通过XRD、SEM、TEM、PPMS和ICP等对HA和Fe-HA的物相、微观形貌、磁学性能、元素组成进行了表征和分析。研究发现：Fe-HA物相与HA相同, 没有明显的杂质相; HA为抗磁性, Fe-HA转化为顺磁性; 共沉淀法粉体为针状, 共沉淀-水热法粉体为短棒状, 针状粉体在强磁场中不能定向, 短棒状粉体能够定向; 在单一方向强磁场中, HA不能单轴定向, Fe-HA能够在一定程度上沿c轴取向。

关键词: 铁-羟基磷灰石, 强磁场, 顺磁性, 定向

Abstract:

The surface nanostructure of bioceramics can affect osteoblast proliferation and differentiation, therefore the control of the surface microstructure of bioceramics, especially grain orientation before the ceramic sintering, is one of key to design and develop bioactive ceramics for bone regeneration. This study aimed to investigate the crystal orientation of Fe-doped hydroxyapatite in high magnetic field. Pure hydroxyapatite (HA) and Fe-doped hydroxyapatite (Fe-HA) powders were prepared by co-precipitation method and co-precipitation-hydrothermal method, and their phase composition, microstructure, magnetic property, and elementary composition were analyzed by XRD, SEM, TEM, PPMS, and ICP. The results showed that the phase of Fe-HA is the same as HA with no impurity phase. HA is diamagnetic originally, while Fe-HA becomes paramagnetic. The microstructure of samples prepared by co-precipitation method is needle cluster-like but that prepared by co-precipitation-hydrothermal method is rod-like. It is the rad-like but not the needle cluster-like Fe-HA can be orientated in high magnetic field. Therefore, the orientation of rod-like Fe-HA can be regulated by high magnetic field. Furthermore, pure HA cannot be uniaxial orientated in single-directed high magnetic field. while Fe-HA can be oriented along c axis in certain degree in single- directed high magnetic field.

Key words: Fe-HA, high magnetic field, paramagnetic, orientate

中图分类号:

TQ174

王小龙, 任忠鸣, 常江. 铁掺杂羟基磷灰石的制备及在强磁场中的定向研究[J]. 无机材料学报, 2018, 33(1): 75-80.

WANG Xiao-Long, REN Zhong-Ming, CHANG Jiang. Synthesis and Orientation of Fe-doped Hydroxyapatite in High Magnetic Field[J]. Journal of Inorganic Materials, 2018, 33(1): 75-80.

图/表 8

图1 添加1mol%、2mol%和5mol%铁离子样品的XRD图谱

Fig. 1 XRD patterns of the samples doped with 1mol%, 2mol%, 5mol% Fe ion^(a) Co-precipitation; (b) Coprecipitation-hydrothermal

图2 样品的磁化曲线(Oe=A/m, emu/g=4π×10-7 Wb•m/kg)

Fig. 2 B-H curves of sample

表1 4组5mol%Fe-HA样品的元素组成

Table 1 Elemental composition of four kinds of samples

Sample	Fe/Ca	Ca/P	(Ca+Fe)/P
S1	0.050	1.561	1.639
S2	0.052	1.580	1.663
S3	0.052	1.583	1.665
S4	0.051	1.589	1.669

图3 Fe-HA和HA的SEM照片

Fig. 3 SEM images of Fe-HA and HA^(a) Co-precipitation Fe-HA; (b) Coprecipitation-hydrothermal Fe-HA; (c) Coprecipitation-hydrothermal HA

图4 不同合成方法的HA和Fe-HA的TEM照片

Fig. 4 TEM images of Fe-HA and HA prepared with different methods^(a) Co-precipitation HA; (b) Co-precipitation Fe-HA; (c) Coprecipitation-hydrothermal HA; (d) Coprecipitation-hydrothermal Fe-HA

图5 使用不同分散剂在强磁场中注浆成型的陶瓷片XRD图谱

Fig. 5 XRD patterns of the samples with different dispersant casting in high magnetic field

图6 Fe-HA和HA在强磁场中注浆成型的陶瓷片XRD图谱

Fig. 6 XRD patterns of Fe-HA and HA samples casting in high magnetic field^(a) Coprecipitation-hydrothermal Fe-HA; (b) Coprecipitation-hydrothermal HA; (c) Co-precipitation Fe-HA

图7 HA/Fe-HA在强磁场中的定向原理示意图

Fig. 7 Orientation principle of HA/Fe-HA in high magnetic field^(a) Effect of dispersant on HA orientation; (b) Effect of Fe ions on the orientation of HA

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铁掺杂羟基磷灰石的制备及在强磁场中的定向研究

Synthesis and Orientation of Fe-doped Hydroxyapatite in High Magnetic Field

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