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Nanocrystalline titanium dioxide particles with anatase structure and high thermal stability have been synthesized using the basic sol-gel method. The particle size and morphology were refined under hydrothermal conditions in the presence of different concentrations of tetramethylammonium hydroxide (TMAH) at 210°C and 230°C. XRD and TEM analysis showed that the TiO2 particles obtained were homogeneous and monodispersive at low contents of TMAH. All intense peaks, clearly observed in the XRD patterns, were assigned to the anatase phase and no rutile phase was observed. At high contents of TMAH, nanoscale small (10–30 nm) and larger (>100 nm) TiO2 particles were one-pot synthesized. The nanocrystalline TiO2 particles synthesized by this method have good thermal stability. With the sintering temperature of up to 650°C, all the XRD peaks maintained good agreement with the anatase reference data. [ABSTRACT FROM AUTHOR]