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 TiO 2 -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.

Looking at the façade of a historical building, it is often difficult to distinguish between the original decoration and later additions. One such building is the Holy Virgin Mary Church at the Malbork Castle (Northern Poland), built between 1276 and 1406. During the latest restoration works, ceramic tiles with some remnants of the green glaze, decorating the Holy Virgin Mary Church façade, were studied in situ using portable X-ray fluorescence spectrometry. Micro-samples were analyzed in laboratory by scanning electron microscopy with energy dispersive X-ray spectrometry (SEM-EDS) and wavelength-dispersive X-ray spectrometry (SEM-WDS), micro-Raman spectroscopy and powder X-ray micro-diffraction. We found that what was originally thought to be a paint layer was in fact a heavily deteriorated SiO 2 -PbO glaze. White, yellow and black pigments were found to have been added into the glaze as opacifiers and colorants. Copper and iron were used as glaze colorants. The originally added pigments were transformed into new phases, such as antimony-doped tin oxide. The technology used to produce the glazed tiles was identified. All the results collectively confirmed the medieval origin of the green glazed tiles.

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