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ARTICLE SUMMARY Where Sharp Interfaces Are Generally Present, Without Any Obvious Preferred Orientation

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ARTICLE SUMMARY Where Sharp Interfaces Are Generally Present, Without Any Obvious Preferred Orientation RESEARCH ◥ ture is preserved up to the grain boundaries, RESEARCH ARTICLE SUMMARY where sharp interfaces are generally present, without any obvious preferred orientation. HYBRID PEROVSKITES Near-120° triple boundaries are most com- monly observed at the intersection of three Atomic-scale microstructure of metal grains, which we generally found to be crys- tallographically continuous and associated halide perovskite with minimal lattice distortion. Finally, we identified the nature of defects, Mathias Uller Rothmann, Judy S. Kim, Juliane Borchert, Kilian B. Lohmann, Colum M. O’Leary, dislocations, and stacking faults in the FAPbI3 Alex A. Sheader, Laura Clark, Henry J. Snaith, Michael B. Johnston, Peter D. Nellist*, Laura M. Herz* lattice. We discovered dislocations that are dissociated in a direction perpendicular to their glide plane (climb-dissociated), aligned INTRODUCTION: Hybrid metal halide perov- but ordered perovskite lattice, apparent as point defects in the form of vacancies on the skites are highly favorable materials for light-and-dark checkered patterns in STEM Pb-I sublattice, and stacking faults corre- efficient photovoltaic and optoelectronic ap- images. Further electron beam exposure leads sponding to a shift of half a unit cell, con- – plications. The mechanisms behind their to the expected deterioration to PbI2 as the necting Pb-I columns with I columns rather impressive performance have yet to be fully final decomposition product. We propose that than with FA+ columns. understood, but they likely depend on atomic- the observed intermediate checkered pat- level properties that may be unique to these tern is triggered by an initially random, beam- CONCLUSION: Our findings provide an atomic- Downloaded from perovskites. Atomic-resolution transmission induced loss of FA+, followed by subsequent level understanding of the technologically electron microscopy is well suited to provide reordering of FA+ ions. The discovery of this important class of hybrid lead halide pe- new insights but is challenging because of intermediate structure explains why the rovskites, revealing several mechanisms that the highly beam-sensitive nature of hybrid perovskite structure can sustain significant de- underpin their remarkable performance. The perovskites. viations from stoichiometry and recovers re- highly adaptive nature of the perovskite struc- markably well from damage. ture upon organic cation loss yields exception- http://science.sciencemag.org/ RATIONALE: We used low-dose scanning trans- We further revealed the atomic arrange- al regenerative properties of partly degraded missionelectronmicroscopy(STEM)imaging ment at interfaces within the hybrid perov- material. The observation of coherent perov- to determine the microstructure of thin hybrid skite films. We found that PbI2 precursor skite interfaces with PbI2 explains the barely perovskite films. Thermally evaporated thin remnants commonly encountered in hybrid diminished optoelectronic performance upon films of formamidinium and methylammo- perovskite films readily and seamlessly inter- such precursor inclusions, while sharp inter- nium lead triiodide (FAPbI3 and MAPbI3, grow with the FAPbI3 and MAPbI3 lattice and faces between perovskite grains grant a respectively) were examined on ultrathin can distort from their bulk hexagonal struc- benign nature. Such atomically localized carbon-coated copper TEM grids to reveal the ture to form a surprisingly coherent transition information enables the targeted design of nature of boundaries, defects, and decompo- boundary, exhibiting low lattice misfit and methods to eliminate defects and optimize sition pathways. strain. We observed PbI2 domains that nearly interfaces in these materials. ▪ perfectly follow the surrounding perovskite on November 2, 2020 RESULTS: Using low-dose low-angle annular structure and orientation, which suggests The list of author affiliations is available in the full article online. dark field (LAADF) STEM imaging, we ob- that PbI2 may seed perovskite growth. These *Corresponding author. Email: [email protected] tained atomic-resolution micrographs of FAPbI observations help to explain why the pres- (L.M.H.); [email protected] (P.D.N.) 3 Cite this article as M. U. Rothmann et al., Science 370, films in the cubic phase. We found that pro- ence of excess PbI2 tends not to impede solar eabb5940 (2020). DOI: 10.1126/science.abb5940 longed electron irradiation leads to a loss of cell performance. + FA ions, which initially causes the perovskite Images of FAPbI3 grain boundaries further READ THE FULL ARTICLE AT structure to change to a partially FA+-depleted revealed that the long-range perovskite struc- https://doi.org/10.1126/science.abb5940 ABCD Partially FA-depleted perovskite Coherent Pbl2:FAPbl3 interface Sharp FAPbl3 grain boundaries Stacking fault and dislocation 5 nm 55 nmnm5 nm 5 nm –2 Atomic-resolution STEM images of FAPbI3. (A) Checkered intensity pattern formed upon electron beam exposure with ~200 e Å .(B) Native intergrowth between PbI2 (shaded yellow) and FAPbI3 within the vapor-deposited film. (C) Abrupt grain boundaries meeting at a near-120° triple junction, showing no amorphous or intergranular phase. (D) Intrinsic stacking fault (orange rectangle, left) and climb-dissociated dislocation (green rectangle, right). Scale bars, 5 nm. Rothmann et al., Science 370, 548 (2020) 30 October 2020 1of1 RESEARCH ◥ RESEARCH ARTICLE (31). To resolve both “near-stoichiometric” polycrystalline FAPbI3 films and those formed with substantial excess PbI2 precursor (“PbI2- HYBRID PEROVSKITES rich”), we prepared two different types of thermally evaporated materials on ultrathin Atomic-scale microstructure of metal carbon-coated copper TEM grids: thinner 30-nm FAPbI3 films close to stoichiometry halide perovskite [FA:Pb:I ratios close to 1:1:3, containing a small excess of PbI2 (as used to optimize for solar cell Mathias Uller Rothmann1, Judy S. Kim2,3,4, Juliane Borchert1, Kilian B. Lohmann1, Colum M. O’Leary2, applications) (32)] and thicker 90-nm films 2 2 1 1 Alex A. Sheader , Laura Clark , Henry J. Snaith , Michael B. Johnston , containing substantial excess PbI2. To examine Peter D. Nellist2*, Laura M. Herz1* whether similar atomic-scale microstructures were also observable for methylammonium lead Hybrid organic-inorganic perovskites have high potential as materials for solar energy applications, but triiodide (MAPbI3), we also deposited 30-nm their microscopic properties are still not well understood. Atomic-resolution scanning transmission MAPbI3 films containing substantial excess PbI2. electron microscopy has provided invaluable insights for many crystalline solar cell materials, and we Full details of the sample preparation proce- used this method to successfully image formamidinium lead triiodide [CH(NH2)2PbI3] thin films with a dures and characterization are provided in the low dose of electron irradiation. Such images reveal a highly ordered atomic arrangement of sharp grain supplementary materials and fig. S1. We have boundaries and coherent perovskite/PbI2 interfaces, with a striking absence of long-range disorder in reported thin films of FAPbI3 and MAPbI3 the crystal. We found that beam-induced degradation of the perovskite leads to an initial loss of deposited by us from such dual-source vapor- Downloaded from + formamidinium [CH(NH2)2 ] ions, leaving behind a partially unoccupied perovskite lattice, which explains deposition protocols to achieve photovoltaic the unusual regenerative properties of these materials. We further observed aligned point defects and power conversion efficiencies of 14.2 to 18.2% climb-dissociated dislocations. Our findings thus provide an atomic-level understanding of when incorporated into suitable device archi- technologically important lead halide perovskites. tectures (32, 33). STEM samples were annealed according to protocols previously developed to optimize photovoltaic performance. http://science.sciencemag.org/ any of the advances in the perform- of the technologically important CH(NH2)2PbI3 In Fig. 1, we show a low-angle annular dark ance of hybrid metal halide perovskite (formamidinium lead triiodide, FAPbI3)MHP field (LAADF, inner radius of 33 mrad; see (MHP) solar cells have resulted from is still uncertain (21). Therefore, truly atomic- materials and methods for full low-dose image M improvements in device architecture resolution imaging of MHPs has great poten- acquisition conditions) STEM micrograph and material composition studied on tial to provide urgently needed understanding of a 90-nm FAPbI3 film containing excess a mesoscopic to macroscopic scale (1–7), and for a plethora of puzzling observations already PbI2. LAADF STEM is similar to high-angle changes in material properties have usually established for perovskite devices, which in turn annular dark field (HAADF) STEM in that it been inferred from relatively “large area” would lead to a further increase in their effi- detects scattered electrons, making it sensitive probes (8–11). Although these probes can re- ciency. In addition, grain boundaries have been to atomic number (Z) variations, but has the solve properties on the scale of a few hundred postulated to have a substantial impact on the advantage of collecting a higher fraction of the nanometers to a few millimeters, the mecha- long-term stability of MHPs (22, 23), yet their scattered electrons, leading to a higher atomic on November 2, 2020 nisms behind the impressive performance of exact nature is still
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