Publication date: 22nd July 2026
Holistic understanding of thin film crystallisation requires bridging the gap between precursor solution chemistry and final crystal structure. While diffraction techniques reveal the crystalline phase evolution, and solution studies characterize precursor solution complexes, the intermediary steps remain poorly understood: how do solvated building blocks transform into nucleation seeds for long-range crystalline order?
To address this question, we employ simultaneous multimodal in situ characterization during perovskite thin film formation. Using a beamline-designed slot-die roll-to-roll coater, we track the same film spot during film formation through coating, gas quenching and thermal annealing. Our measurement suite combines: (1) GIWAXS for crystalline phase evolution, (2) optical spectroscopy (X-ray excited optical luminescence, XEOL, and white light reflection, WLR) for optoelectronic quality and film thickness, (3) X-ray fluorescence (XRF) for solvent tracking, and (4) X-ray absorption spectroscopy (XAS) to probe local Pb geometry, oxidation state and coordination environment.
By correlating the evolution of the local Pb environment (XAS), with solvent removal kinetics (XRF) and crystallisation dynamics (GIWAXS) in perovskite films containing commonly-used additives, we identify key relationships between solvent removal, precursor decomplexation and additive-mediated crystallisation pathways. We identify three distinct Pb coordination regimes during gas quenching and thermal annealing, with the nature of the additive modulating the transition kinetics between these regimes. This multimodal approach reveals previously hidden correlations between molecular-scale Pb coordination dynamics and macroscopic film properties, providing mechanistic insight for additive-controlled crystallisation.
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