非均相悬浮法制备多孔羟基磷灰石微球

Preparation of porous hydroxyapatite microspheres by heterogeneous suspension method

为了获得具有吸附和生物学功能的多孔羟基磷灰石(HA)微球,以自制的纳米羟基磷灰石(HA)粉体为原料,用非均相悬浮法制备了HA/明胶微球,将微球在1 250℃下焙烧,成功制备了直径100~500μm的多孔HA微球.采用光学显微镜、SEM分析、XRD分析和BET氮吸附法研究了微球形貌、尺寸、物相组成、比表面积和孔径,测定了微球对水中F-离子的吸附性能.结果表明:微球具有良好球形形貌和相互贯通的纳米微孔;尺寸比较均匀,分散性良好;微球的主要结晶相为羟基磷灰石;BET表面积为1.867 0~2.089 5 m^2/g,孔径6.53~6.85 nm;对氟离子的平衡吸附容量为1.909~1.940 mg/g.通过控制m(HA)/m(明胶)比例、油温、搅拌速度和搅拌时间,可以在一定范围内控制微球直径和比表面积.

In order to obtain porous hydroxyapatite（HA） microspheres with adsorption and biological functions,HA/gelatin microspheres were prepared by heterogeneous suspension method using nanohydroxyapatite（HA） powders as raw material.After 1 250 ℃ calcinations,the porous HA microspheres with diameters ranging 100~500 μm were successfully prepared.The morphology,size,phase composition,specific surface area and pore size of the microspheres were examined by optical microscope,scanning electron microscope（SEM）,X-ray diffraction（XRD） and BET.The adsorption properties of the microspheres on F-ion in water were also studied.The results showed that the microspheres have excellent spherical morphology and interpenetrating nano-pores.The microspheres are homogeneous and well dispersed.The main crystalline phase of the microspheres is HA.The BET surface area of the microspheres,the pore size,and the equilibrium adsorption capacity of fluoride ion were 1.867 0~2.089 5 m^2/g,6.53~6.85 nm,1.909~1.940 mg/g,respectively.The diameter and specific surface area of the microspheres can be finely controlled within a certain range by tuning the HA/gelatin ratio,oil temperature,and stirring speed and time.