X-ray dose effects and strategies to mitigate beam damage in metal halide perovskites under high brilliance X-ray photon sources

Abstract

Metal halide perovskites (MHP) suffer from photo-structural-chemical instabilities whose intricacy requires state-of-the-art tools to investigate their properties under various conditions. This study addresses the damage caused by focused X-ray beams on MHP through a correlative multi-technique approach. The damage after high-dose irradiation is noticeable in many ways: the loss of iodine and organic components, whose relative amount is reduced; the formation of an excavated area modifying the sample morphology; and an altered optical reflectivity indicating an optically inactive layer. The damage mechanism combines radiolysis and sputtering processes. Interestingly, the bulk underneath the excavated area maintains the initial halide proportion demonstrated by a stable photoluminescence emission energy. We also show that controlling the beam dose and environment is an excellent strategy to mitigate the dose harm. Hence, we combined a controlled X-ray dose with an inert N2 atmosphere to certify the conditions to probe MHP properties while mitigating damage efficiently. Finally, we applied optimized conditions in an X-ray ptychography experiment, reaching a 15-nm spatial resolution, an outcome that has never been attained in this class of materials.