Sensitivity-Enhanced 207Pb Solid-State NMR Spectroscopy for the Rapid, Non-Destructive Characterization of Organolead Halide Perovskites

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

doi:10.1021/acs.chemmater.8b01899

Title: Sensitivity-Enhanced ²⁰⁷Pb Solid-State NMR Spectroscopy for the Rapid, Non-Destructive Characterization of Organolead Halide Perovskites

Abstract

Here, organolead halide and mixed halide perovskites (CH₃NH₃PbX₃, CH₃NH₃PbX_3–nY_n, X and Y = Cl^–, Br^–, or I^–) are promising materials for photovoltaics and optoelectronic devices. ²⁰⁷Pb solid-state NMR spectroscopy has previously been applied to characterize phase segregation and halide ion speciation in mixed halide perovskites. However, NMR spectroscopy is an insensitive technique that often requires large sample volumes and long signal averaging periods. This is especially true for mixed halide perovskites, which give rise to extremely broad ²⁰⁷Pb solid-state NMR spectra. Here, we quantitatively compare the sensitivity of the various solid-state NMR techniques on pure and mixed halide organolead perovskites and demonstrate that both fast MAS and DNP can provide substantial gains in NMR sensitivity for these materials. With fast MAS and proton detection, high signal-to-noise ratio two-dimensional (2D) ²⁰⁷Pb–¹H heteronuclear correlation (HETCOR) NMR spectra can be acquired in less than half an hour from only ca. 4 μL of perovskite material. Modest relayed DNP enhancements on the order of 1 to 20 were obtained for perovskites. The cryogenic temperatures (110 K) used for DNP experiments also provide a significant boost in sensitivity. Consequently, it was possible to obtain the ²⁰⁷Pb solid-state NMR spectrum of a 300 nm thick modelmore »« less

Authors:

Hanrahan, Michael P. ^[1];

^[1]; Rosales, Bryan A. ^[2];

^[1];

^[1]

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

Publication Date:: 2018-09-18

Research Org.:: Ames Lab., Ames, IA (United States)

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

OSTI Identifier:: 1477201

Report Number(s):: IS-J-9762
Journal ID: ISSN 0897-4756

Grant/Contract Number:: CHE-1253058; AC02-07CH11358

Resource Type:: Accepted Manuscript

Journal Name:: Chemistry of Materials

Additional Journal Information:: Journal Volume: 30; Journal Issue: 20; Journal ID: ISSN 0897-4756

Publisher:: American Chemical Society (ACS)

Country of Publication:: United States

Language:: English

Subject:: 36 MATERIALS SCIENCE; 37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CHEMISTRY

Citation Formats


                    Hanrahan, Michael P., Men, Long, Rosales, Bryan A., Vela, Javier, and Rossini, Aaron J. Sensitivity-Enhanced 207Pb Solid-State NMR Spectroscopy for the Rapid, Non-Destructive Characterization of Organolead Halide Perovskites.  United States: N. p., 2018. 
Web.  doi:10.1021/acs.chemmater.8b01899.

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                    Hanrahan, Michael P., Men, Long, Rosales, Bryan A., Vela, Javier, & Rossini, Aaron J. Sensitivity-Enhanced 207Pb Solid-State NMR Spectroscopy for the Rapid, Non-Destructive Characterization of Organolead Halide Perovskites.  United States.  https://doi.org/10.1021/acs.chemmater.8b01899

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                    Hanrahan, Michael P., Men, Long, Rosales, Bryan A., Vela, Javier, and Rossini, Aaron J. Tue .  
"Sensitivity-Enhanced 207Pb Solid-State NMR Spectroscopy for the Rapid, Non-Destructive Characterization of Organolead Halide Perovskites".  United States.  https://doi.org/10.1021/acs.chemmater.8b01899.  https://www.osti.gov/servlets/purl/1477201.

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@article{osti_1477201,

  title        = {Sensitivity-Enhanced 207Pb Solid-State NMR Spectroscopy for the Rapid, Non-Destructive Characterization of Organolead Halide Perovskites},

  author       = {Hanrahan, Michael P. and Men, Long and Rosales, Bryan A. and Vela, Javier and Rossini, Aaron J.},

  abstractNote = {Here, organolead halide and mixed halide perovskites (CH3NH3PbX3, CH3NH3PbX3–nYn, X and Y = Cl–, Br–, or I–) are promising materials for photovoltaics and optoelectronic devices. 207Pb solid-state NMR spectroscopy has previously been applied to characterize phase segregation and halide ion speciation in mixed halide perovskites. However, NMR spectroscopy is an insensitive technique that often requires large sample volumes and long signal averaging periods. This is especially true for mixed halide perovskites, which give rise to extremely broad 207Pb solid-state NMR spectra. Here, we quantitatively compare the sensitivity of the various solid-state NMR techniques on pure and mixed halide organolead perovskites and demonstrate that both fast MAS and DNP can provide substantial gains in NMR sensitivity for these materials. With fast MAS and proton detection, high signal-to-noise ratio two-dimensional (2D) 207Pb–1H heteronuclear correlation (HETCOR) NMR spectra can be acquired in less than half an hour from only ca. 4 μL of perovskite material. Modest relayed DNP enhancements on the order of 1 to 20 were obtained for perovskites. The cryogenic temperatures (110 K) used for DNP experiments also provide a significant boost in sensitivity. Consequently, it was possible to obtain the 207Pb solid-state NMR spectrum of a 300 nm thick model thin film of CH3NH3PbI3 in 34 h by performing solid-state NMR experiments with a sample temperature of 110 K. This result demonstrates the possibility of using NMR spectroscopy for characterization of perovskite thin films.},

  doi          = {10.1021/acs.chemmater.8b01899},

  journal      = {Chemistry of Materials},

  number       = 20,

  volume       = 30,

  place        = {United States},

  year         = {2018},

  month        = {9}

}

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https://doi.org/10.1021/acs.chemmater.8b01899

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Cited by: 3 works

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Figure 1: (A) Comparison of ²⁰⁷Pb solid-state NMR spectra of CH₃NH₃PbBr₃ obtained with different NMR methods: (blue, top trace) DNP enhanced, 110 K ¹H→²⁰⁷Pb CPMAS, (green) proton detected, 40 kHz MAS 2D ²⁰⁷Pb→¹H CP-HETCOR, (red) 50 kHz MAS direct detection ²⁰⁷Pb spin echo, (yellow) 2D ¹H{²⁰⁷Pb} D-HMQC, (purple, lower trace)more »

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Works referencing / citing this record:

Determination of the Full 207Pb Chemical Shift Tensor of Anglesite, PbSO4, and Correlation of the Isotropic Shift to Lead–Oxygen Distance in Natural Minerals
journal, January 2019

Zeman, Otto; Steinadler, Jennifer; Hochleitner, Rupert
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Mechanosynthesis, Optical, and Morphological Properties of MA, FA, Cs-SnX ₃ (X = I, Br) and Phase-Pure Mixed-Halide MASnI _x Br ₃ _{- x} Perovskites: Mechanosynthesis, Optical, and Morphological Properties of MA, FA, Cs-SnX ₃ (X = I, Br) and Phase-Pure Mixed-Halide MASnI _x Br ₃ _{- x} Perovskites
journal, March 2019

Saski, Marcin; Prochowicz, Daniel; Marynowski, Wojciech
European Journal of Inorganic Chemistry, Vol. 2019, Issue 22
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Title: Sensitivity-Enhanced 207Pb Solid-State NMR Spectroscopy for the Rapid, Non-Destructive Characterization of Organolead Halide Perovskites

Abstract

Citation Formats

Figures / Tables:

Cesium-containing triple cation perovskite solar cells: improved stability, reproducibility and high efficiency journal, January 2016

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Cationic Dynamics in the Crystalline Phases of (CH 3 NH 3 )PbX 3 (X: Cl, Br) as Studied by Proton Magnetic Resonance Techniques journal, November 1989

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Short-range ion dynamics in methylammonium lead iodide by multinuclear solid state NMR and 127 I NQR journal, January 2018

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Membrane topologies of the PGLa antimicrobial peptide and a transmembrane anchor sequence by Dynamic Nuclear Polarization/solid-state NMR spectroscopy journal, February 2016

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Title: Sensitivity-Enhanced ²⁰⁷Pb Solid-State NMR Spectroscopy for the Rapid, Non-Destructive Characterization of Organolead Halide Perovskites

Cesium-containing triple cation perovskite solar cells: improved stability, reproducibility and high efficiency
journal, January 2016

Incorporation of rubidium cations into perovskite solar cells improves photovoltaic performance
journal, September 2016

NQR Investigation of Phase Transitions in Cesium Plumbochloride
journal, January 1969

Nuclear quadrupole spin-lattice relaxation of ⁸⁵ Rb, ⁸⁷ Rb and ¹³³ Cs in RbCdCl ₃ and CsPbCl ₃ near the cubic-tetragonal phase transition
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Dynamics of the n-decylammonium chains in the perovskite-type layer structure compound (C10H21NH3)2CdCl4
journal, January 1979

Low-temperature incommensurate-commensurate phase sequence of ( $C_{3}$ $H_{7}$ ${ND}_{3}$ $)_{2}$ ${MnCl}_{4}$
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Cationic Dynamics in the Crystalline Phases of (CH ₃ NH ₃ )PbX ₃ (X: Cl, Br) as Studied by Proton Magnetic Resonance Techniques
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Structure and Bonding of Tribromocadmates, ACdBr ₃ , A = NH ₄ , Rb, Cs, CH ₃ NH ₃ , (CH ₃ ) ₂ NH ₂ , (CH ₃ ) ₄ N], [H ₂ NNH ₃ , and (H ₂ N) ₃ C. An X-ray Diffraction and ^79-81 Br NQR Study
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Short-range ion dynamics in methylammonium lead iodide by multinuclear solid state NMR and ¹²⁷ I NQR
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Solvent Annealing of Perovskite-Induced Crystal Growth for Photovoltaic-Device Efficiency Enhancement
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