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Lead halide perovskites are promising materials for a range of applications owing to their unique crystal structure and optoelectronic properties. Understanding the relationship between the atomic/mesostructures and the associated properties of perovskite materials is crucial to their application performances. Herein, the detailed pressure processing of CsPbBr perovskite nanocube superlattices (NC-SLs) is reported for the first time. By using in situ synchrotron-based small/wide angle X-ray scattering and photoluminescence (PL) probes, the NC-SL structural transformations are correlated at both atomic and mesoscale levels with the band-gap evolution through a pressure cycle of 0 ↔ 17.5 GPa. After the pressurization, the individual CsPbBr NCs fuse into 2D nanoplatelets (NPLs) with a uniform thickness. The pressure-synthesized perovskite NPLs exhibit a single cubic crystal structure, a 1.6-fold enhanced photoluminescence quantum yield, and a longer emission lifetime than the starting NCs. This study demonstrates that pressure processing can serve as a novel approach for the rapid conversion of lead halide perovskites into structures with enhanced properties.

Lead-free double perovskite nanocrystals (NCs) have emerged as a new category of materials that hold the potential for overcoming the instability and toxicity issues of lead-based counterparts. Doping chemistry represents a unique avenue toward tuning and optimizing the intrinsic optical and electronic properties of semiconductor materials. In this study, we report the first example of doping Yb 3+ ions into lead-free double perovskite Cs 2 AgBiX 6 (X = Cl − , Br − ) NCs via a hot injection method. The doping of Yb 3+ endows the double perovskite NCs with a newly emerged near-infrared emission band (sensitized from the NC hosts) in addition to their intrinsic trap-related visible photoluminescence. By controlling the Yb-doping concentration, the dual emission profiles and photon relaxation dynamics of the double perovskite NCs can be systematically tuned. Furthermore, we have successfully inserted divalent Mn 2+ ions in Cs 2 AgBiCl 6 NCs and observed emergence of dopant emission. Our work illustrates an effective and facile route toward modifying and optimizing optical properties of double perovskite Cs 2 AgBiX 6 (X = Cl − , Br − ) NCs with an indirect bandgap nature, which can broaden a range of their potential applications in optoelectronic devices.