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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]
  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.
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
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.
@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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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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Works referenced in this record:

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

  • Saliba, Michael; Matsui, Taisuke; Seo, Ji-Youn
  • Energy & Environmental Science, Vol. 9, Issue 6
  • DOI: 10.1039/C5EE03874J

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


Persistent Dopants and Phase Segregation in Organolead Mixed-Halide Perovskites
journal, August 2016


Lead Halide Perovskites: Challenges and Opportunities in Advanced Synthesis and Spectroscopy
journal, March 2017


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

  • Tovborg‐Jensen, N.
  • The Journal of Chemical Physics, Vol. 50, Issue 1
  • DOI: 10.1063/1.1670853

Nuclear Quadrupole Resonance (NQR) of79Br and81Br in Perovskite and Orthorhombic Forms of CsPbBr3 and CsPbJ3
journal, January 1969

  • Volkov, A. F.; Venevtsev, Yu. N.; Semin, G. K.
  • physica status solidi (b), Vol. 35, Issue 2
  • DOI: 10.1002/pssb.19690350277

Crystal preparation and properties of cesium tin(II) trihalides
journal, March 1974

  • Scaife, David E.; Weller, Paul F.; Fisher, Wayne G.
  • Journal of Solid State Chemistry, Vol. 9, Issue 3, p. 308-314
  • DOI: 10.1016/0022-4596(74)90088-7

Dynamics of the n-decylammonium chains in the perovskite-type layer structure compound (C10H21NH3)2CdCl4
journal, January 1979

  • Kind, R.; Pleko, S.; Arend, H.
  • The Journal of Chemical Physics, Vol. 71, Issue 5
  • DOI: 10.1063/1.438584

Cation rotation in methylammonium lead halides
journal, November 1985


Low-temperature incommensurate-commensurate phase sequence of ( C 3 H 7 ND 3 ) 2 MnCl 4
journal, July 1988


81 Br NQR and 119 Sn Mössbauer Study for MSnBr 3 (M=Cs and CH 3 NH 3 )
journal, December 1988

  • Yamada, Koji; Nose, Sayuri; Umehara, Takako
  • Bulletin of the Chemical Society of Japan, Vol. 61, Issue 12
  • DOI: 10.1246/bcsj.61.4265

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

  • Furukawa, Yoshihiro; Nakamura, Daiyu
  • Zeitschrift für Naturforschung A, Vol. 44, Issue 11
  • DOI: 10.1515/zna-1989-1115

Structure and Bonding of Two Modifications of CsSnI3 by Means of Powder X-Ray Diffraction, 127I NQR, and DTA
journal, August 1989

  • Yamada, Koji; Tsuritani, Tomoko; Okuda, Tsutomu
  • Chemistry Letters, Vol. 18, Issue 8, p. 1325-1328
  • DOI: 10.1246/cl.1989.1325

Alkylammonium lead halides. Part 2. CH 3 NH 3 PbX 3 (X = Cl, Br, I) perovskites: cuboctahedral halide cages with isotropic cation reorientation
journal, March 1990

  • Knop, Osvald; Wasylishen, Roderick E.; White, Mary Anne
  • Canadian Journal of Chemistry, Vol. 68, Issue 3
  • DOI: 10.1139/v90-063

Structural Phase Transition and Electrical Conductivity of the Perovskite CH 3 NH 3 Sn 1 - x Pb x Br 3 and CsSnBr 3
journal, September 1990

  • Yamada, Koji; Kawaguchi, Hiroshi; Matsui, Takashi
  • Bulletin of the Chemical Society of Japan, Vol. 63, Issue 9
  • DOI: 10.1246/bcsj.63.2521

Phase Transitions in CsSnCl 3 and CsPbBr 3 An NMR and NQR Study
journal, April 1991

  • Sharma, Surendra; Weiden, Norbert; Weiss, Alarich
  • Zeitschrift für Naturforschung A, Vol. 46, Issue 4
  • DOI: 10.1515/zna-1991-0406

Molecular Motions and Phase Transitions in Solid CH3NH3PbX3 (X = C1, Br, I) as Studied by NMR and NQR
journal, January 1991

  • Xu, Qiang; Eguchi, Taro; Nakayama, Hirokazu
  • Zeitschrift für Naturforschung A, Vol. 46, Issue 3
  • DOI: 10.1515/zna-1991-0305

Successive Phase Transitions and High Ionic Conductivity of Trichlorogermanate (II) Salts as Studied by 35C1 NQR and Powder X-Ray Diffraction
journal, February 1994

  • Yamada, K.; Isobe, K.; Okuda, T.
  • Zeitschrift für Naturforschung A, Vol. 49, Issue 1-2
  • DOI: 10.1515/zna-1994-1-238

Phase Transition and Electric Conductivity of ASnCl 3 (A = Cs and CH 3 NH 3 )
journal, January 1998

  • Yamada, Koji; Kuranaga, Yasuhisa; Ueda, Keita
  • Bulletin of the Chemical Society of Japan, Vol. 71, Issue 1
  • DOI: 10.1246/bcsj.71.127

Static and dynamic structures of CD3ND3GeCl3 studied by TOF high resolution neutron powder diffraction and solid state NMR
journal, April 2002

  • Yamada, Koji; Mikawa, Keiko; Okuda, Tsutomu
  • Journal of the Chemical Society, Dalton Transactions, Issue 10
  • DOI: 10.1039/b201611g

Phase Transition Study by using 133 Cs and 207 Pb Nuclear Magnetic Resonance in a CsPbCl 3 Single Crystal
journal, February 2004

  • Ran Lim, Ae; Gyoo Kim, In
  • Journal of the Physical Society of Japan, Vol. 73, Issue 2
  • DOI: 10.1143/JPSJ.73.475

A combined single crystal neutron/X-ray diffraction and solid-state nuclear magnetic resonance study of the hybrid perovskites CH 3 NH 3 PbX 3 (X = I, Br and Cl)
journal, January 2015

  • Baikie, Tom; Barrow, Nathan S.; Fang, Yanan
  • Journal of Materials Chemistry A, Vol. 3, Issue 17
  • DOI: 10.1039/C5TA01125F

Structure of Colloidal Quantum Dots from Dynamic Nuclear Polarization Surface Enhanced NMR Spectroscopy
journal, October 2015

  • Piveteau, Laura; Ong, Ta-Chung; Rossini, Aaron J.
  • Journal of the American Chemical Society, Vol. 137, Issue 43
  • DOI: 10.1021/jacs.5b09248

Multinuclear NMR as a tool for studying local order and dynamics in CH 3 NH 3 PbX 3 (X = Cl, Br, I) hybrid perovskites
journal, January 2016

  • Roiland, Claire; Trippé-Allard, Gaelle; Jemli, Khaoula
  • Physical Chemistry Chemical Physics, Vol. 18, Issue 39
  • DOI: 10.1039/C6CP02947G

Multinuclear Magnetic Resonance Tracking of Hydro, Thermal, and Hydrothermal Decomposition of CH 3 NH 3 PbI 3
journal, January 2017

  • Askar, Abdelrahman M.; Bernard, Guy M.; Wiltshire, Benjamin
  • The Journal of Physical Chemistry C, Vol. 121, Issue 2
  • DOI: 10.1021/acs.jpcc.6b10865

Methylammonium lead chloride: A sensitive sample for an accurate NMR thermometer
journal, October 2017


Symmetry, Dynamics, and Defects in Methylammonium Lead Halide Perovskites
journal, December 2016

  • Franssen, Wouter M. J.; van Es, Sverre G. D.; Dervişoğlu, Rıza
  • The Journal of Physical Chemistry Letters, Vol. 8, Issue 1
  • DOI: 10.1021/acs.jpclett.6b02542

Cation Dynamics in Mixed-Cation (MA) x (FA) 1– x PbI 3 Hybrid Perovskites from Solid-State NMR
journal, July 2017

  • Kubicki, Dominik J.; Prochowicz, Daniel; Hofstetter, Albert
  • Journal of the American Chemical Society, Vol. 139, Issue 29
  • DOI: 10.1021/jacs.7b04930

Phase Segregation in Cs-, Rb- and K-Doped Mixed-Cation (MA) x (FA) 1– x PbI 3 Hybrid Perovskites from Solid-State NMR
journal, September 2017

  • Kubicki, Dominik J.; Prochowicz, Daniel; Hofstetter, Albert
  • Journal of the American Chemical Society, Vol. 139, Issue 40
  • DOI: 10.1021/jacs.7b07223

The Nature of Ion Conduction in Methylammonium Lead Iodide: A Multimethod Approach
journal, May 2017

  • Senocrate, Alessandro; Moudrakovski, Igor; Kim, Gee Yeong
  • Angewandte Chemie International Edition, Vol. 56, Issue 27
  • DOI: 10.1002/anie.201701724

Composition-Tunable Formamidinium Lead Mixed Halide Perovskites via Solvent-Free Mechanochemical Synthesis: Decoding the Pb Environments Using Solid-State NMR Spectroscopy
journal, May 2018

  • Askar, Abdelrahman M.; Karmakar, Abhoy; Bernard, Guy M.
  • The Journal of Physical Chemistry Letters, Vol. 9, Issue 10
  • DOI: 10.1021/acs.jpclett.8b01084

Methylammonium Cation Dynamics in Methylammonium Lead Halide Perovskites: A Solid-State NMR Perspective
journal, February 2018

  • Bernard, Guy M.; Wasylishen, Roderick E.; Ratcliffe, Christopher I.
  • The Journal of Physical Chemistry A, Vol. 122, Issue 6
  • DOI: 10.1021/acs.jpca.7b11558

Mechanochemical Synthesis of Methylammonium Lead Mixed–Halide Perovskites: Unraveling the Solid-Solution Behavior Using Solid-State NMR
journal, March 2018


Formation of Stable Mixed Guanidinium–Methylammonium Phases with Exceptionally Long Carrier Lifetimes for High-Efficiency Lead Iodide-Based Perovskite Photovoltaics
journal, February 2018

  • Kubicki, Dominik J.; Prochowicz, Daniel; Hofstetter, Albert
  • Journal of the American Chemical Society, Vol. 140, Issue 9
  • DOI: 10.1021/jacs.7b12860

Degradation of the Formamidinium Cation and the Quantification of the Formamidinium–Methylammonium Ratio in Lead Iodide Hybrid Perovskites by Nuclear Magnetic Resonance Spectroscopy
journal, February 2018

  • Van Gompel, Wouter T. M.; Herckens, Roald; Reekmans, Gunter
  • The Journal of Physical Chemistry C, Vol. 122, Issue 8
  • DOI: 10.1021/acs.jpcc.7b09805

Dynamic nuclear polarization at high magnetic fields
journal, February 2008

  • Maly, Thorsten; Debelouchina, Galia T.; Bajaj, Vikram S.
  • The Journal of Chemical Physics, Vol. 128, Issue 5
  • DOI: 10.1063/1.2833582

High Frequency Dynamic Nuclear Polarization
journal, April 2013

  • Ni, Qing Zhe; Daviso, Eugenio; Can, Thach V.
  • Accounts of Chemical Research, Vol. 46, Issue 9
  • DOI: 10.1021/ar300348n

Dynamic Nuclear Polarization Surface Enhanced NMR Spectroscopy
journal, March 2013

  • Rossini, Aaron J.; Zagdoun, Alexandre; Lelli, Moreno
  • Accounts of Chemical Research, Vol. 46, Issue 9
  • DOI: 10.1021/ar300322x

Is solid-state NMR enhanced by dynamic nuclear polarization?
journal, April 2015


Dynamic Nuclear Polarization Solid-State NMR in Heterogeneous Catalysis Research
journal, October 2015

  • Kobayashi, Takeshi; Perras, Frédéric A.; Slowing, Igor I.
  • ACS Catalysis, Vol. 5, Issue 12
  • DOI: 10.1021/acscatal.5b02039

DNP-Enhanced Ultrawideline Solid-State NMR Spectroscopy: Studies of Platinum in Metal–Organic Frameworks
journal, June 2016

  • Kobayashi, Takeshi; Perras, Frédéric A.; Goh, Tian Wei
  • The Journal of Physical Chemistry Letters, Vol. 7, Issue 13
  • DOI: 10.1021/acs.jpclett.6b00860

Dynamic nuclear polarization for sensitivity enhancement in modern solid-state NMR
journal, November 2017

  • Lilly Thankamony, Aany Sofia; Wittmann, Johannes J.; Kaushik, Monu
  • Progress in Nuclear Magnetic Resonance Spectroscopy, Vol. 102-103
  • DOI: 10.1016/j.pnmrs.2017.06.002

Sensitivity Enhancement in Solid State 15N NMR by Indirect Detection with High-Speed Magic Angle Spinning
journal, January 2000

  • Ishii, Yoshitaka; Tycko, Robert
  • Journal of Magnetic Resonance, Vol. 142, Issue 1
  • DOI: 10.1006/jmre.1999.1976

Sensitivity Enhancement in Solid-State 13 C NMR of Synthetic Polymers and Biopolymers by 1 H NMR Detection with High-Speed Magic Angle Spinning
journal, March 2001

  • Ishii, Yoshitaka; Yesinowski, James P.; Tycko, Robert
  • Journal of the American Chemical Society, Vol. 123, Issue 12
  • DOI: 10.1021/ja015505j

Inverse Detection and Heteronuclear Editing in 1H–15N Correlation and 1H–1H Double-Quantum NMR Spectroscopy in the Solid State under Fast MAS
journal, May 2001

  • Schnell, Ingo; Langer, Benedikt; Söntjens, Serge H. M.
  • Journal of Magnetic Resonance, Vol. 150, Issue 1
  • DOI: 10.1006/jmre.2001.2312

Chemical Shift Correlation NMR Spectroscopy with Indirect Detection in Fast Rotating Solids:  Studies of Organically Functionalized Mesoporous Silicas
journal, September 2007

  • Wiench, Jerzy W.; Bronnimann, Charles E.; Lin, Victor S. -Y
  • Journal of the American Chemical Society, Vol. 129, Issue 40, p. 12076-12077
  • DOI: 10.1021/ja074746+

Proton-Detected Solid-State NMR Spectroscopy of Fully Protonated Proteins at 40 kHz Magic-Angle Spinning
journal, September 2007

  • Zhou, Donghua H.; Shah, Gautam; Cormos, Mircea
  • Journal of the American Chemical Society, Vol. 129, Issue 38
  • DOI: 10.1021/ja073462m

Rapid Analysis of Organic Compounds by Proton-Detected Heteronuclear Correlation NMR Spectroscopy with 40 kHz Magic-Angle Spinning
journal, September 2008

  • Zhou, Donghua H.; Rienstra, Chad M.
  • Angewandte Chemie International Edition, Vol. 47, Issue 38
  • DOI: 10.1002/anie.200802108

Studies of minute quantities of natural abundance molecules using 2D heteronuclear correlation spectroscopy under 100 kHz MAS
journal, April 2015


Fast magic-angle sample spinning solid-state NMR at 60–100 kHz for natural abundance samples
journal, September 2016


NMR longitudinal relaxation enhancement in metal halides by heteronuclear polarization exchange during magic-angle spinning
journal, June 2016

  • Shmyreva, Anna A.; Safdari, Majid; Furó, István
  • The Journal of Chemical Physics, Vol. 144, Issue 22
  • DOI: 10.1063/1.4953540

Rapid acquisition of wideline MAS solid-state NMR spectra with fast MAS, proton detection, and dipolar HMQC pulse sequences
journal, January 2016

  • Rossini, Aaron J.; Hanrahan, Michael P.; Thuo, Martin
  • Physical Chemistry Chemical Physics, Vol. 18, Issue 36
  • DOI: 10.1039/C6CP04279A

Suppression of signals from the probe in bloch decay spectra
journal, October 1988


Solid-state dynamic nuclear polarization at 263 GHz: spectrometer design and experimental results
journal, January 2010

  • Rosay, Melanie; Tometich, Leo; Pawsey, Shane
  • Physical Chemistry Chemical Physics, Vol. 12, Issue 22
  • DOI: 10.1039/c003685b

Surface Enhanced NMR Spectroscopy by Dynamic Nuclear Polarization
journal, November 2010

  • Lesage, Anne; Lelli, Moreno; Gajan, David
  • Journal of the American Chemical Society, Vol. 132, Issue 44
  • DOI: 10.1021/ja104771z

TOTAPOL: A Biradical Polarizing Agent for Dynamic Nuclear Polarization Experiments in Aqueous Media
journal, September 2006

  • Song, Changsik; Hu, Kan-Nian; Joo, Chan-Gyu
  • Journal of the American Chemical Society, Vol. 128, Issue 35
  • DOI: 10.1021/ja061284b

Dynamic Nuclear Polarization NMR Spectroscopy of Microcrystalline Solids
journal, September 2012

  • Rossini, Aaron J.; Zagdoun, Alexandre; Hegner, Franziska
  • Journal of the American Chemical Society, Vol. 134, Issue 40
  • DOI: 10.1021/ja308135r

Measuring Nano- to Microstructures from Relayed Dynamic Nuclear Polarization NMR
journal, July 2017

  • Pinon, Arthur C.; Schlagnitweit, Judith; Berruyer, Pierrick
  • The Journal of Physical Chemistry C, Vol. 121, Issue 29
  • DOI: 10.1021/acs.jpcc.7b04438

NMR at Low and Ultralow Temperatures
journal, March 2013

  • Tycko, Robert
  • Accounts of Chemical Research, Vol. 46, Issue 9
  • DOI: 10.1021/ar300358z

Fast passage dynamic nuclear polarization on rotating solids
journal, November 2012

  • Mentink-Vigier, Frederic; Akbey, Ümit; Hovav, Yonatan
  • Journal of Magnetic Resonance, Vol. 224
  • DOI: 10.1016/j.jmr.2012.08.013

Nuclear depolarization and absolute sensitivity in magic-angle spinning cross effect dynamic nuclear polarization
journal, January 2015

  • Mentink-Vigier, Frédéric; Paul, Subhradip; Lee, Daniel
  • Physical Chemistry Chemical Physics, Vol. 17, Issue 34
  • DOI: 10.1039/C5CP03457D

The ordered phase of methylammonium lead chloride CH3ND3PbCl3
journal, May 2005

  • Chi, Lisheng; Swainson, Ian; Cranswick, Lachlan
  • Journal of Solid State Chemistry, Vol. 178, Issue 5
  • DOI: 10.1016/j.jssc.2004.12.037

Total suppression of sidebands in CPMAS C-13 NMR
journal, September 1982


Nontemplate Synthesis of CH 3 NH 3 PbBr 3 Perovskite Nanoparticles
journal, January 2014

  • Schmidt, Luciana C.; Pertegás, Antonio; González-Carrero, Soranyel
  • Journal of the American Chemical Society, Vol. 136, Issue 3
  • DOI: 10.1021/ja4109209

Lead Halide Perovskite Nanocrystals in the Research Spotlight: Stability and Defect Tolerance
journal, August 2017


Benzyl Alcohol-Treated CH 3 NH 3 PbBr 3 Nanocrystals Exhibiting High Luminescence, Stability, and Ultralow Amplified Spontaneous Emission Thresholds
journal, November 2017


Shape Evolution and Single Particle Luminescence of Organometal Halide Perovskite Nanocrystals
journal, February 2015


Observing Apparent Nonuniform Sensitivity Enhancements in Dynamic Nuclear Polarization Solid-State NMR Spectra of Polymers
journal, August 2014

  • Mollica, Giulia; Le, Dao; Ziarelli, Fabio
  • ACS Macro Letters, Vol. 3, Issue 9
  • DOI: 10.1021/mz500459p

Magnetic resonance spectral reconstruction using frequency‐shifted and summed Fourier transform processing
journal, March 1995

  • Clark, W. G.; Hanson, M. E.; Lefloch, F.
  • Review of Scientific Instruments, Vol. 66, Issue 3
  • DOI: 10.1063/1.1145643

71Ga and 69Ga nuclear magnetic resonance study of β-Ga2O3: resolution of four- and six-fold coordinated Ga sites in static conditions
journal, May 1995

  • Massiot, Dominique; Farnan, Ian; Gautier, Nathalie
  • Solid State Nuclear Magnetic Resonance, Vol. 4, Issue 4
  • DOI: 10.1016/0926-2040(95)00002-8

Ultra-Wideline Solid-State NMR Spectroscopy
journal, June 2013

  • Schurko, Robert W.
  • Accounts of Chemical Research, Vol. 46, Issue 9
  • DOI: 10.1021/ar400045t

Role of Chloride in the Morphological Evolution of Organo-Lead Halide Perovskite Thin Films
journal, October 2014

  • Williams, Spencer T.; Zuo, Fan; Chueh, Chu-Chen
  • ACS Nano, Vol. 8, Issue 10
  • DOI: 10.1021/nn5041922

Solvent Annealing of Perovskite-Induced Crystal Growth for Photovoltaic-Device Efficiency Enhancement
journal, August 2014


Moisture assisted perovskite film growth for high performance solar cells
journal, November 2014

  • You, Jingbi; Yang, Yang (Michael); Hong, Ziruo
  • Applied Physics Letters, Vol. 105, Issue 18
  • DOI: 10.1063/1.4901510

Controlling Nucleation and Growth of Metal Halide Perovskite Thin Films for High-Efficiency Perovskite Solar Cells
journal, February 2017


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

  • Salnikov, Evgeniy Sergeevich; Aisenbrey, Christopher; Aussenac, Fabien
  • Scientific Reports, Vol. 6, Issue 1
  • DOI: 10.1038/srep20895

Analysis of Molecular Orientation in Organic Semiconducting Thin Films Using Static Dynamic Nuclear Polarization Enhanced Solid-State NMR Spectroscopy
journal, October 2017

  • Suzuki, Katsuaki; Kubo, Shosei; Aussenac, Fabien
  • Angewandte Chemie International Edition, Vol. 56, Issue 47
  • DOI: 10.1002/anie.201707208

Photophysical properties of wavelength-tunable methylammonium lead halide perovskite nanocrystals
journal, January 2017

  • Freppon, Daniel J.; Men, Long; Burkhow, Sadie J.
  • Journal of Materials Chemistry C, Vol. 5, Issue 1
  • DOI: 10.1039/C6TC03886G

NMR nomenclature. Nuclear spin properties and conventions for chemical shifts(IUPAC Recommendations 2001)
journal, January 2001

  • Harris, Robin K.; Becker, Edwin D.; Cabral de Menezes, Sonia M.
  • Pure and Applied Chemistry, Vol. 73, Issue 11
  • DOI: 10.1351/pac200173111795

Spin Echoes
journal, November 1950


Measuring Amide Nitrogen Quadrupolar Coupling by High-Resolution 14 N/ 13 C NMR Correlation under Magic-Angle Spinning
journal, May 2006

  • Gan, Zhehong
  • 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
  • DOI: 10.1006/jmra.1994.1208

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
  • DOI: 10.1006/jmre.1999.1896

Figures/Tables have been extracted from DOE-funded journal article accepted manuscripts.