Surface Termination of CsPbBr3 Perovskite Quantum Dots Determined by Solid-State NMR Spectroscopy

Chen, Yunhua; Smock, Sara R.; Flintgruber, Anne H.; Perras, Frédéric A.; Brutchey, Richard L.; Rossini, Aaron J.

doi:10.1021/jacs.9b13396

Surface Termination of CsPbBr₃ Perovskite Quantum Dots Determined by Solid-State NMR Spectroscopy

Journal Article · Mon Mar 02 00:00:00 EST 2020 · Journal of the American Chemical Society

DOI:https://doi.org/10.1021/jacs.9b13396· OSTI ID:1728699

Chen, Yunhua ^[1]; Smock, Sara R. ^[2]; Flintgruber, Anne H. ^[3]; ^[3]; ^[2]; ^[4]

Ames Lab., and Iowa State Univ., Ames, IA (United States); University of Southern California
Univ. of Southern California, Los Angeles, CA (United States)
Ames Lab., Ames, IA (United States)
Ames Lab., and Iowa State Univ., Ames, IA (United States)

Cesium lead halide perovskite quantum dots (QDs) have gained significant attention as next-generation optoelectronic materials; however, their properties are highly dependent on their surface chemistry. The surfaces of cuboidal CsPbBr₃ QDs have been intensively studied by both theoretical and experimental techniques, but fundamental questions still remain about the atomic termination of the QDs. The surface binding sites and modes of ligands at the surface remain unproven. Herein, we demonstrate that solid-state NMR spectroscopy allows the unambiguous assignment of organic surface ligands via ¹H, ¹³C, and ³¹P NMR. Surface-selective ¹³³Cs solid-state NMR spectra show the presence of an additional ¹³³Cs NMR signal with a unique chemical shift that is attributed to Cs atoms terminating the surface of the particle and which are likely coordinated by carboxylate ligands. Dipolar dephasing curves that report on the distance between the surface ammonium ligands and Cs and Pb were recorded using double resonance ¹H{¹³³Cs} and ¹H{²⁰⁷Pb} RESPDOR experiments. Model QD surface slabs with different possible surface terminations were generated from the CsPbBr₃ crystal structure and theoretical RESPDOR dipolar dephasing curves considering all possible ¹H-¹³³Cs/²⁰⁷Pb spin pairs were then calculated. Comparison of the calculated and experimental RESPDOR curves indicates the particles are CsBr terminated (not PbBr₂ terminated) with alkylammonium ligands substituting into some surface Cs sites, consistent with the surface-selective ¹³³Cs NMR experiments. Lastly, these results highlight the utility of high-resolution solid-state NMR spectroscopy for studying ligand binding and the surface structure of nanomaterials.

View Accepted Manuscript (DOE)

Research Organization:: Univ. of Southern California, Los Angeles, CA (United States)

Sponsoring Organization:: USDOE Office of Science (SC), Basic Energy Sciences (BES). Materials Sciences & Engineering Division

Grant/Contract Number:: SC0006812

OSTI ID:: 1728699

Journal Information:: Journal of the American Chemical Society, Journal Name: Journal of the American Chemical Society Journal Issue: 13 Vol. 142; ISSN 0002-7863

Publisher:: American Chemical Society (ACS)Copyright Statement

Country of Publication:: United States

Language:: English

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