Ultrafine indium tin oxide (ITO) powders were successfully synthesised by the combined methods of ultrasonic spray and microwave assisted pyrolysis, which is a single step, facile, rapid and continuous method without post-heating treatment. Crystallinity, morphology and microstructure of the samples were investigated by X-ray diffractometer, scanning electron microscope, transmission electron microscope, energy dispersive X-ray spectroscope, selected area electron diffraction pattern and laser grain size analyser. Results indicate that pure solid solution ITO ultrafine powders with homogeneous and narrow size distribution, highly dense and smooth surface morphology can be obtained under optimum conditions. Each uniform spherical particle consisted of many smaller crystallites with diameter of <10 nm.
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