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Synthesis of mesoporous hydroxyapatite nanoparticles using a template-free sonochemistry-assisted microwave method

机译:无模板声化学辅助微波法合成介孔羟基磷灰石纳米粒子

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摘要

A facile template-free sonochemistry-assisted microwave method was successfully developed for the synthesis of mesoporous hydroxyapatite nanoparticles (MHN) in a short time. The prepared MHN were characterized by means of X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), transmission electron microscopy (TEM), and N_2 adsorption-desorption isotherms. TEM images showed a clear rod-like morphology with length of 50-100 nm and width of about 20 nm. XRD and FTIR indicated a typical hydroxyapatite phase with high crystallinity. N_2 adsorption-desorption isotherms revealed an irregular mesoporous structure. Judging from the values calculated from N_2 isotherms, the specific surface area and pore volume obviously decreased after the sintering process. In a typical example, the specific surface area, pore volume, and pore size of MHN before and after calcination were 79.74 m~2/g, 0.46 cm~3/g, 2.7 nm and 45.41 m~2/g, 0.22 cm~3/g, 2.8 nm, respectively. In addition, MHN could be synthesized in a period of time as short as 10 min. Further investigation indicated that microwave radiation played a dominant role in the emergence of mesoporous structure, while ultrasound irradiation acted as a supporting role. Based on the above results, a possible mechanism of formation of mesoporous hydroxyapatite has been proposed.
机译:成功开发了一种简便的无模板声波化学辅助微波方法,用于在短时间内合成介孔羟基磷灰石纳米粒子(MHN)。通过X射线衍射(XRD),傅立叶变换红外光谱(FTIR),透射电子显微镜(TEM)和N_2吸附-脱附等温线对制备的MHN进行表征。 TEM图像显示出清晰的棒状形态,其长度为50-100nm,宽度为约20nm。 XRD和FTIR表明具有高结晶度的典型羟基磷灰石相。 N_2吸附-解吸等温线显示不规则的介孔结构。从N_2等温线计算得出的值,烧结后比表面积和孔容明显下降。在一个典型的例子中,煅烧前后MHN的比表面积,孔体积和孔径为79.74m〜2 / g,0.46cm〜3 / g,2.7nm和45.41m〜2 / g,0.22cm〜。 3 / g,2.8 nm。此外,MHN可以在短至10分钟的时间内合成。进一步的研究表明,微波辐射在介孔结构的出现中起主要作用,而超声辐射起辅助作用。基于以上结果,提出了介孔羟基磷灰石形成的可能机理。

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