目的 制备医用羟基磷灰石(HA)纳米粒并观测其纳米结构及纳米尺寸效应;方法 采用常态表面活性剂(水包油)制备HA纳米粒,用电子显微镜、X射线仪、核磁共振仪、分光光度计和傅里叶变换红外光谱仪等对HA纳米粒进行观测。结果 HA纳米粒的平均尺寸为。10-30nm;共振分析表明,磷至少以2种类型存在;在200nm波长处,光谱包含六面体Ca^2+典型的光谱带;HA纳米粒微晶的Eg值分别为1.60和1.64ev;傅里叶变换红外光谱中包含2种振波;在956.5、1026.1和1.108.7cm光带处的3种PO4^3-曲态分别为v1(PO4)、v3(PO4)、v3(PO4)。在565.2 and 600.0cm光带处的2种PO4^3-曲态为v4(PO4)。结论 纳米尺寸产生的从纳米粒到微晶的边缘能量增加伴随着簇晶体积的下降和Ca^2+周围配基的变化。这些变化与量子尺寸效应有关。
[Objective] To prepare a kind of hydroxyapatite nanoparticle for medical utilization and to observe its nanostructure and nanosize effect. [Method] The nanoparticles of hydroxyapatite (HA) had been synthesized using normal (oil in water) surfactant. Ultrastructure of nanoparticles was studied through HRTEM, FTIR, NMR, XRD. [Results] The experimental results showed that the size of nanorod samples was about 10-30 nm. The presence of these resonance of phosphorus in at least two types of phosphorus environments. The spectra of nanorod contained typical bands of hexahedra Ca^2+ at 200 nm. The Eg values for the HA of microcrystalline, nanorod samples were 1.60 and 1.64ev, respectively. The FTIR spectra of the nanorods include two types of vibration; three PO4^3- stretching modes at 956.5, 1 026.1 and 1 108.7cm^-1 band were attributed to the vl (PO4), v3 (PO4), v3 (PO4) modes respectively. Two PO4^3- bending modes at 565.2 and 600.0 cm^-1 bands were attributed to the v4(PO4) modes. [Conclusion] A minor increase of edge energy of nanorods to microcrystalline resulted in by nanosize might be associated with a decrease in cluster sized as welt as the ligand changes around Ca^2+ ions. These changes might relate to quantum size effect.