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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, 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 modelmore » 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.« less

Authors:
 [1]; ORCiD logo [1];  [2]; ORCiD logo [1]; ORCiD logo [1]
+ Show Author Affiliations
  1. Ames Lab. and Iowa State Univ., Ames, IA (United States)
  2. Iowa State Univ., Ames, IA (United States)
Publication Date:
Research Org.:
Ames Laboratory (AMES), 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 = {Tue Sep 18 00:00:00 EDT 2018},
month = {Tue Sep 18 00:00:00 EDT 2018}
}
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https://doi.org/10.1021/acs.chemmater.8b01899
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Figures / Tables:

Figure 1 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 » static 207Pb spin echo. (B) 2D 207Pb→1H CP-HETCOR spectrum with 40 kHz MAS and (C) 2D 1H{207Pb} D-HMQC spectrum with 40 kHz MAS. In (A) the 207Pb NMR sensitivity for each experiment is noted beside each spectrum. For (B) and (C) the 1H sensitivity of the first $t$1 increment of the 2D NMR experiment is displayed to the left of the 1H spectrum, the 207Pb sensitivity is displayed in the bottom left corner of the correlation experiment and the total experiment time is indicated in the lower right hand corner.« less
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  • Journal of the American Chemical Society, Vol. 128, Issue 18
  • DOI: 10.1021/ja0578597

Proton-detected nitrogen-14 NMR by recoupling of heteronuclear dipolar interactions using symmetry-based sequences
journal, September 2007

Through-space R3-HETCOR experiments between spin-1/2 and half-integer quadrupolar nuclei in solid-state NMR
journal, June 2007

Ramped-Amplitude Cross Polarization in Magic-Angle-Spinning NMR
journal, October 1994

  • Metz, G.; Wu, X. L.; Smith, S. O.
  • Journal of Magnetic Resonance, Series A, Vol. 110, Issue 2
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Proton-Selective 17 O− 1 H Distance Measurements in Fast Magic-Angle-Spinning Solid-State NMR Spectroscopy for the Determination of Hydrogen Bond Lengths
journal, November 2006

  • Brinkmann, Andreas; Kentgens, Arno P. M.
  • Journal of the American Chemical Society, Vol. 128, Issue 46
  • DOI: 10.1021/ja065415k

Comparison of several hetero-nuclear dipolar recoupling NMR methods to be used in MAS HMQC/HSQC
journal, May 2008

Non-aqueous solvents for DNP surface enhanced NMR spectroscopy
journal, January 2012

  • Zagdoun, Alexandre; Rossini, Aaron J.; Gajan, David
  • Chem. Commun., Vol. 48, Issue 5
  • DOI: 10.1039/C1CC15242D

Large Molecular Weight Nitroxide Biradicals Providing Efficient Dynamic Nuclear Polarization at Temperatures up to 200 K
journal, August 2013

  • Zagdoun, Alexandre; Casano, Gilles; Ouari, Olivier
  • Journal of the American Chemical Society, Vol. 135, Issue 34
  • DOI: 10.1021/ja405813t

An Improved Broadband Decoupling Sequence for Liquid Crystals and Solids
journal, January 2000

  • Fung, B. M.; Khitrin, A. K.; Ermolaev, Konstantin
  • Journal of Magnetic Resonance, Vol. 142, Issue 1
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