We found for the first time a new origin of selection of perovskite crystallization pathways from DMF solutions containing MAI and PbI 2 to present here a comprehensive study of a full set of essential intermediate phases determining the perovskite's morphology. For all three discovered structurally different intermediate phases forming at a given precursor ratio, we refined their crystal structures by synchrotron X-ray radiation and investigated dynamics and phase assemblage in the course of decomposition. As a result, we revealed a clear correlation between the composition of the intermediate phases, peculiarities of their crystal structure, and the morphology of the final perovskite films. Using the DFT method we calculated formation enthalpies of these intermediate phases and explained the preferential precipitation of DMSO-adduct rather than DMF-adduct in an antisolvent approach. This finding opens up a possibility of design-on-demand of perovskite materials using simple soft chemistry approaches.
The Rb 2 La 2 Ti 3 O 10 layered oxide was synthesized by the solid-state method. Three phases with different protonation degrees and intercalated water contents were obtained from the initial compound by the treatment with distilled water and hydrochloric acid. The obtained samples were characterized by powder X-ray diffraction, SEM, X-ray microanalysis, BET, DRS, and TG. It was found that the complete ion exchange of Rb + for H + in the layered oxide Rb 2 La 2 Ti 3 O 10 proceeds through the formation of two metastable intermediate phases with average protonation degrees of 0.5 and 0.75, which successively transform from one to another. Each of these phase transformations is accompanied not only by the contraction of the interlayer distance but also by the displacement of adjacent perovskite layers by 1/2 of the cell parameter which results in the change in the space group. The photocatalytic activity of obtained samples decreases with the increase in the protonation degree, which correlates with the decrease in the intercalated water content.
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