作　　者： ; ; ; ; ; ; ;

机构地区： 华南理工大学化学与化工学院

出　　处： 《高校化学工程学报》 2009年第3期460-465,共6页

摘　　要： 以无机盐SnCl4·5H2O,SbCl3为起始原料,以乙醇为溶剂,采用溶胶-凝胶法制备纳米锑掺杂氧化锡(ATO)粒子。在洗涤除去醇凝胶中的NH4+和Cl-后,尝试将超临界流体干燥(Supercritical Fluid Drying,SCFD)技术应用于醇凝胶的干燥。醇凝胶干粉经过高温烧结后,制得了疏松结构的纳米ATO粉体。采用XRD、TG/DSC、FESEM、TEM等分析方法对制得的前驱体干粉、纳米ATO粒子进行表征。XRD结果表明,采用溶胶-凝胶法结合超临界流体干燥技术制得了疏松的、四方型金红石结构的纳米ATO粉体,纳米ATO晶化程度高,并随着烧结温度的升高而升高。TG/DSC分析显示,600℃时前驱体分解完全,得到约78.2%的ATO粒子。从FESEM及TEM照片可以看出,疏松的纳米ATO粒子轻微地贴在一起,粒子的粒径在25nm左右。经过对超临界CO2干燥技术(SCFD)消除前驱体粒子团聚的机理进行分析,揭示了采用超临界CO2流体干燥醇凝胶能够使前驱体粒子保持松散的结构。因此采用溶胶-凝胶法结合超临界流体技术制得疏松的前驱体干粉,对最终获得粒径小、低团聚、分散性好的纳米ATO粉体的至关重要。 Using the alcohol as reaction solvent, the nano-sizes antimony doped tin oxide （ATO） particles were prepared from inorganic salts of SnCl4.5H2O and SbCl3 by sol-gel method. The alcogels are the precursors of ATO, and after the impurities of NH4＋ and Cl- in them were removed, the alcogels were dried by applying the technology of supercritical fluid drying （SCFD）. Under atmosphere, the dry precursors were annealed at different temperatures and the weakly agglomerated nano-sized ATO particles with tetragonal phase structure were obtained. The obtained nanoparticles were characterized by thermogravimetric and differential scanning calorimetry （TG/DSC）, X-ray diffraction （XRD）, field emission scanning electron microscopy （FESEM） and transmission electron microscopy （TEM）. The XRD data indicate that the ATO particles with tetragonal phase structure are well crystallized, and their crystallinity increases with the increase of annealing temperature. According to the TG/DSC analysis, it was found that the decomposition reaction of the precursors obtained with SCFD completes over 600~C, and the obtained mass fraction of ATO is about 78.2%. The TEM and FESEM photographs show that the loose ATO powder obtained with SCFD primarily consists of particles weakly attached to each other, and their average size is around 25 nm. Since the particles of the precursors can keep loose morphology after treated by SCFD is caused by the superiority of the supercritical fluid CO2, the technology of SCFD with CO2 is the key technology for the preparation of weekly agglomerated nano-sized ATO particles.

关 键 词： 锑掺杂氧化锡 溶胶 凝胶法 超临界流体干燥 消除团聚

领　　域： [一般工业技术] [化学工程]