Synthesis And Characterization Of Inorganic Nanomaterials By Solvothermal Methods

The present thesis is focused on the first step of inorganic nanomaterials research -- the synthesis and characterization of inorganic nanomaterials. By the adoption of new hydrothermal/solvothermal methods and varying the experimental parameters such as reaction source species and amounts, temperature and time, solvents species and concentration, etc., the shape, size and phase-controlled synthesis of metal submicrocrystallites, and semiconducting metal sulfides (ZnS, CdS) nanocrystals has been achieved. Meanwhile, many techniques including X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), transmission electron microscopy (TEM), scan electron microscopy (SEM), high-resolution transmission electron microscopy (HRTEM) and selected area electron diffraction (SAED), UV-Vis absorption spectra, fluorence spectra, and so on, were used to characterize the as-synthesized products.The main work completed in this thesis can be summarized as the following:1. Pure submicrometer-sized copper and silver crystallites have been directly synthesized via solvothermal treatment of CuCl2·2H2O or AgNO3 in ethylenediamine (EDA) at 80-180°C for 15-20 h, and characterized by means of X-ray power diffraction, X-ray photoelectron spectroscopy and transmission electron microscopy. It was suggested that the formation of copper and silver crystallites in this solvothermal system be through a typical complexation–reduction process, in which EDA serves not only as a reducing reagent, but also as a complexing solvent.2. The phase, shape and size-controlled synthesis of ZnS nanocrystals from an air-stable single-source molecular precursor (zinc diethyldithiocarbamate: Zn-(DDTC)₂) has been achieved by two facile steps: firstly, the Zn-(DDTC)₂ precursor was prepared directly through the precipitation reaction of zinc acetate and sodium diethyldithiocarbamate in distilled water under ambient condition; secondly, pure cubic...