Geon Woo Yoon, Seo‐Ryeong Lee, Si Eun Park, Hyungju Ahn, Do Kyung Lee, Oh Yeong Gong, Gill Sang Han, Carolin M. Sutter‐Fella, Bo Ram Lee, Jin‐Wook Lee, Hyun Suk Jung
Controlling the crystallization pathway of inorganic CsPbI 3 perovskite is essential for achieving high efficiency and stability in optoelectronic devices. Here, we report a solvent-engineering strategy that combines an antisolvent process with vacuum treatment (AVT) to modulate evaporation dynamics of the precursor, guiding the formation of highly oriented (CH 3 ) 2 NH 2 PbI 3 (DMAPbI 3 ) and Cs 4 PbI 6 intermediate phases. Synchrotron and in situ analyses revealed correlations between intermediate orientation and γ-CsPbI 3 crystallinity. This directional crystallization pathway promotes vertical alignment and grain enlargement in γ-CsPbI 3 films, resulting in fewer voids, lower defect densities, and reduced tensile strain. Photovoltaic devices based on AVT-processed films achieved a power conversion efficiency of 18.47% with a fill factor of 83.14% and retained 101.9% of their initial efficiency after 526 h without encapsulation. This study first reports that the quality of DMAPbI 3 and Cs 4 PbI 6 intermediates, controlled by combination of antisolvent and vacuum treatment, plays a crucial role in achieving high-quality γ-CsPbI 3 films.