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以无机盐SnCl4·5H2O和SbCl3为初始原料,以乙醇作为溶剂,采用溶胶-凝胶法结合超临界流体干燥(supercritical fluid drying,SCFD)技术制备了纳米锑掺杂氧化锡(antimony doped tin oxide,ATO)粉体。通过热重-差示扫描热分析、X射线衍射、扫描电子显微镜、透射电镜,对前驱体粒子以及ATO粒子的结构进行了分析。探讨了热处理温度、前驱体干燥方式对前驱体以及纳米粒子的形貌、粒径、分散性、晶型、结晶度的影响,并讨论了SCFD技术干燥前驱体的机理。结果表明:采用溶胶-凝胶法结合超临界CO2干燥技术,在给定的反应条件下,能够制得疏松的、良好掺杂的四方型结构的纳米ATO粒子,粒径约15～30nm,分散性好。
Inorganic salts SnCl4 · 5H2O and SbCl3 were used as raw materials and ethanol was used as solvent to prepare antimony doped tin oxide (SnO2) nanoparticles by sol-gel method and supercritical fluid drying (SCFD) ATO) powder. The structures of precursor particles and ATO particles were analyzed by thermogravimetric-differential scanning calorimetry, X-ray diffraction, scanning electron microscopy and transmission electron microscopy. The effect of heat treatment temperature and precursor drying method on the morphology, particle size, dispersity, crystal form and crystallinity of the precursors and nanoparticles were discussed. The mechanism of SCFD drying of precursors was also discussed. The results show that nano-sized ATO particles with a size of about 15 ~ 30nm can be obtained by the sol-gel method combined with the supercritical CO2 drying technology under the given reaction conditions. Good sex.