Laboratory synthesis of microsheets of titanium dioxide from titanyl sulfate involves the use of ammonia solution, whereas another inorganic base is most likely to be employed at the industrial level, as ammonia is a toxic agent and therefore should be avoided according to European Union (EU) regulations. Selected nontoxic bases such as sodium, potassium, and lithium hydroxides have been tested as an alternative to ammonia solution to obtain amorphous and crystalline TiO2-based microsheets. The final products obtained at each step of the procedure (samples lyophilized and annealed at 230 and 800 °C) were analyzed with electron and atomic force microscopy, X-ray powder diffraction, thermal analysis, and Fourier transform infrared (FTIR) and Raman spectroscopies to determine their morphology and phase composition. The differences in the morphology of the obtained products were described in detail as well as phase and structural composition throughout the process. It was found that, in the last step of the synthesis, microsheets annealed at 800 °C were built of small rods and oval or platy crystalline particles depending on the base used. The temperature of formation of anatase, rutile, and alkali-metal titanates in correlation with the ionic radius of the alkali metal present in the sample was discussed.
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