Zhao Pingtang, Wang Jinmin, Chen Guoe, Xiao Zhou, Zhou Jing, Chen Dean, Huang Kaixun
Department of Chemistry Huazhong University of Science and Technology, 1037 Luoyu Lu, Hongshan Qu, Wuhan, Hubei 430074, People's Republic of China.
J Nanosci Nanotechnol. 2008 Jan;8(1):379-85.
PbS hollow spheres were successfully prepared by a sodium citrate-assisted hydrothermal process at 120 degrees C for 12 h, employing lead acetate trihydrate, thiourea and sodium citrate as precursors. The diameter of PbS hollow spheres is 200-400 nm, which is composed of about 50-80 nm nanoparticles. The synthesized product was characterized by powder X-ray diffraction (XRD), field emission scanning electron microscopy (FESEM), transmission electron microscopy (TEM), high-resolution transmission electron microscopy (HRTEM), electron diffraction (ED), Fourier transform-infrared (FT-IR) spectroscopy, ultraviolet-visible spectrometer (UV-vis) and near-infrared absorption spectrometer (NIR). The effects of the reaction conditions on morphologies of PbS structures were investigated. Star-shaped and flat PbS crystals were obtained by changing some experiment conditions. The results show that temperature, sodium citrate concentration, sulfur sources and solvent play key roles on the final morphologies formation of PbS crystals. Especially, ED result indicates that PbS hollow spheres hold single crystal-like electron diffraction patterns. And the possible formation mechanism of hollow spheres was proposed.
通过柠檬酸钠辅助水热法,在120℃下反应12小时,以三水合醋酸铅、硫脲和柠檬酸钠为前驱体,成功制备了硫化铅空心球。硫化铅空心球的直径为200 - 400纳米,由约50 - 80纳米的纳米颗粒组成。采用粉末X射线衍射(XRD)、场发射扫描电子显微镜(FESEM)、透射电子显微镜(TEM)、高分辨率透射电子显微镜(HRTEM)、电子衍射(ED)、傅里叶变换红外(FT-IR)光谱、紫外可见光谱仪(UV-vis)和近红外吸收光谱仪(NIR)对合成产物进行了表征。研究了反应条件对硫化铅结构形貌的影响。通过改变一些实验条件获得了星形和平坦的硫化铅晶体。结果表明,温度、柠檬酸钠浓度、硫源和溶剂对硫化铅晶体最终形貌的形成起着关键作用。特别是,电子衍射结果表明硫化铅空心球具有单晶状电子衍射图案。并提出了空心球可能的形成机制。