In this paper, a survey of the most important results obtained in the study of electrocatalytic thin film evolution under in situ conditions is given. With the combination of simultaneous thermal analysis, thermogravimetry-mass spectrometry, secondary ion mass spectrometry, and emission FTIR spectroscopy, a detailed description of the elementary processes taking place in the precursor gel prepared on titanium metal support upon heating to 600 °C are discussed. The systems studied include RuO2 and IrO2 coatings stabilized by TiO2, ZrO2, Ta2O5, and SnO2. The precursor compounds were RuCl3·3H2O, IrCl3·3H2O, Ti-diisopropoxide-pentanedionate, ZrOCl2·8H2O, TaCl5, and SnCl2·2H2O in alcoholic solution. With this combined approach, the identification of reactions taking place in certain temperature intervals, the conversion mechanism of the different chlorides to oxides, the nature of evolved gases, and the formation and catalytic decomposition of organic surface species were possible. With the secondary ion mass spectrometry and emission FTIR techniques, characterization of the oxide surfaces as well as the identification of segregation phenomena affecting surface morphology and electrode performance were made.
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