Persistent dopants and phase segregation in organolead mixed-halide perovskites

Rosales, Bryan A.; Men, Long; Cady, Sarah D.; Hanrahan, Michael P.; Rossini, Aaron J.; Vela, Javier

doi:10.1021/acs.chemmater.6b01874

Title: Persistent dopants and phase segregation in organolead mixed-halide perovskites

Journal Article · Mon Jul 25 00:00:00 EDT 2016 · Chemistry of Materials

DOI:https://doi.org/10.1021/acs.chemmater.6b01874· OSTI ID:1321908

Rosales, Bryan A. ^[1]; Men, Long ^[2]; Cady, Sarah D. ^[1]; Hanrahan, Michael P. ^[2]; Rossini, Aaron J. ^[2]; Vela, Javier ^[2]

Iowa State Univ., Ames, IA (United States)
Ames Lab. and Iowa State Univ., Ames, IA (United States)

Organolead mixed-halide perovskites such as CH₃NH₃PbX_3–aX'_a (X, X' = I, Br, Cl) are interesting semiconductors because of their low cost, high photovoltaic power conversion efficiencies, enhanced moisture stability, and band gap tunability. Using a combination of optical absorption spectroscopy, powder X-ray diffraction (XRD), and, for the first time, ²⁰⁷Pb solid state nuclear magnetic resonance (ssNMR), we probe the extent of alloying and phase segregation in these materials. Because ²⁰⁷Pb ssNMR chemical shifts are highly sensitive to local coordination and electronic structure, and vary linearly with halogen electronegativity and band gap, this technique can provide the true chemical speciation and composition of organolead mixed-halide perovskites. We specifically investigate samples made by three different preparative methods: solution phase synthesis, thermal annealing, and solid phase synthesis. ²⁰⁷Pb ssNMR reveals that nonstoichiometric dopants and semicrystalline phases are prevalent in samples made by solution phase synthesis. We show that these nanodomains are persistent after thermal annealing up to 200 °C. Further, a novel solid phase synthesis that starts from the parent, single-halide perovskites can suppress phase segregation but not the formation of dopants. Our observations are consistent with the presence of miscibility gaps and spontaneous spinodal decomposition of the mixed-halide perovskites at room temperature. This underscores how strongly different synthetic procedures impact the nanostructuring and composition of organolead halide perovskites. In conclusion, better optoelectronic properties and improved device stability and performance may be achieved through careful manipulation of the different phases and nanodomains present in these materials.

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Research Organization:: Ames Laboratory (AMES), Ames, IA (United States)

Sponsoring Organization:: USDOE Office of Science (SC), Basic Energy Sciences (BES)

Grant/Contract Number:: AC02-07CH11358

OSTI ID:: 1321908

Report Number(s):: IS-J-9000

Journal Information:: Chemistry of Materials, Journal Name: Chemistry of Materials; ISSN 0897-4756

Publisher:: American Chemical Society (ACS)Copyright Statement

Country of Publication:: United States

Language:: English

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Cited by: 116 works

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Methylamine-induced defect-healing and cationic substitution: a new method for low-defect perovskite thin films and solar cells Yang, Jin-an; Qin, Tianxu; Xie, Lisha Journal of Materials Chemistry C, Vol. 7, Issue 35 https://doi.org/10.1039/c9tc03490k	journal	January 2019
Solvent‐Free Mechanochemical Synthesis of a Systematic Series of Pure‐Phase Mixed‐Halide Perovskites MAPb(I _x Br _{1− x} ) ₃ and MAPb(Br _x Cl _{1− x} ) ₃ for Continuous Composition and Band‐Gap Tuning Tang, Sheng; Xiao, Xinyu; Hu, Jing ChemPlusChem, Vol. 85, Issue 1 https://doi.org/10.1002/cplu.201900723	journal	January 2020
Lead- and Iodide-Deficient (CH ₃ NH ₃ )PbI ₃ ( d -MAPI): The Bridge between 2D and 3D Hybrid Perovskites Leblanc, Antonin; Mercier, Nicolas; Allain, Magali Angewandte Chemie, Vol. 129, Issue 50 https://doi.org/10.1002/ange.201710021	journal	November 2017
Lead- and Iodide-Deficient (CH ₃ NH ₃ )PbI ₃ ( d -MAPI): The Bridge between 2D and 3D Hybrid Perovskites Leblanc, Antonin; Mercier, Nicolas; Allain, Magali Angewandte Chemie International Edition, Vol. 56, Issue 50 https://doi.org/10.1002/anie.201710021	journal	November 2017
Phase Segregation in Cs-, Rb- and K-Doped Mixed-Cation (MA) _x (FA) _{1– x} PbI ₃ Hybrid Perovskites from Solid-State NMR Kubicki, Dominik J.; Prochowicz, Daniel; Hofstetter, Albert Journal of the American Chemical Society, Vol. 139, Issue 40 https://doi.org/10.1021/jacs.7b07223	journal	September 2017

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