Zhao Pingtang, Wang Jinmin, Cheng Guoe, Huang Kaixun
Department of Chemistry, Huazhong University of Science and Technology, Wuhan, Hubei 430074, People's Republic of China.
J Phys Chem B. 2006 Nov 16;110(45):22400-6. doi: 10.1021/jp064392t.
Symmetric hierarchical hollow PbS structures consisting of nanowalls were successfully fabricated by a facile solvothermal process in ethylenediamine at 120 degrees C for 12 h, employing lead acetate trihydrate and dithizone as precursors; the thickness of the nanowalls is about 80 nm. No surfactants or other templates were used in the process. The synthesized product was characterized by X-ray powder diffraction (XRD), Fourier transform infrared (FT-IR) spectroscopy, field emission scanning electron microscopy (FESEM), energy-dispersive X-ray spectroscopy (EDS), transmission electron microscopy (TEM), high-resolution transmission electron microscopy (HRTEM), electron diffraction (ED), ultraviolet-visible spectrometer (UV-vis), near-infrared absorption spectroscopy (near-IR), and fluorescence spectrophotometer. The effect of the reaction conditions on the size and morphologies of PbS structures was investigated. The results show that the temperatures, solvent, and sulfur sources are crucial factors on the morphologies and sizes of the symmetric hierarchical hollow PbS microcrystals. A possible growth mechanism of hierarchical hollow PbS structures is presented. UV-vis absorption spectrum holds a weak peak at 253 nm; the near-infrared absorption spectrum of PbS microcrystals has the two absorption peaks centered at 9613 cm(-1) (1040 nm) and 6771 cm(-1) (1477 nm), showing a blue shift compared with the bulk PbS (approximately 3020 nm). And the fluorescence spectrum of PbS microcrystals consists of an emission peak with a maximum at 305 nm. These PbS microcrystals may have potential applications in the fundamental study of nanostructures as well as fabricating nanodevices.
通过在120℃的乙二胺中采用三水合醋酸铅和双硫腙作为前驱体进行简便的溶剂热法，成功制备了由纳米壁组成的对称分级空心硫化铅结构，反应12小时；纳米壁的厚度约为80纳米。该过程中未使用表面活性剂或其他模板。通过X射线粉末衍射（XRD）、傅里叶变换红外（FT-IR）光谱、场发射扫描电子显微镜（FESEM）、能量色散X射线光谱（EDS）、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）、紫外可见光谱仪（UV-vis）、近红外吸收光谱（近红外）和荧光分光光度计对合成产物进行了表征。研究了反应条件对硫化铅结构尺寸和形貌的影响。结果表明，温度、溶剂和硫源是影响对称分级空心硫化铅微晶形貌和尺寸的关键因素。提出了分级空心硫化铅结构可能的生长机制。紫外可见吸收光谱在253纳米处有一个弱峰；硫化铅微晶的近红外吸收光谱有两个以9613厘米-1（1040纳米）和6771厘米-1（1477纳米）为中心的吸收峰，与块状硫化铅（约3020纳米）相比呈现蓝移。并且硫化铅微晶的荧光光谱由一个在305纳米处最大的发射峰组成。这些硫化铅微晶在纳米结构的基础研究以及制造纳米器件方面可能具有潜在应用。
