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Methylammonium lead chloride: A sensitive sample for an accurate NMR thermometer.

Authors
  • Bernard, Guy M1
  • Goyal, Atul1
  • Miskolzie, Mark1
  • McKay, Ryan1
  • Wu, Qichao1
  • Wasylishen, Roderick E2
  • Michaelis, Vladimir K3
  • 1 Department of Chemistry, University of Alberta, Edmonton, AB T6G 2G2, Canada. , (Canada)
  • 2 Department of Chemistry, University of Alberta, Edmonton, AB T6G 2G2, Canada. Electronic address: [email protected] , (Canada)
  • 3 Department of Chemistry, University of Alberta, Edmonton, AB T6G 2G2, Canada. Electronic address: [email protected] , (Canada)
Type
Published Article
Journal
Journal of Magnetic Resonance
Publisher
Elsevier
Publication Date
Oct 01, 2017
Volume
283
Pages
14–21
Identifiers
DOI: 10.1016/j.jmr.2017.08.002
PMID: 28843057
Source
Medline
Keywords
License
Unknown

Abstract

A new solid-state nuclear magnetic resonance (NMR) thermometry sample is proposed. The 207Pb NMR chemical shift of a lead halide perovskite, methylammonium lead chloride (MAPbCl3) is very sensitive to temperature, 0.905±0.010ppmK-1. The response to temperature is linear over a wide temperature range, from its tetragonal to cubic phase transition at 178K to >410K, making it an ideal standard for temperature calibrations in this range. Because the 207Pb NMR lineshape for MAPbCl3 appears symmetric, the sample is ideal for calibration of variable temperature NMR data acquired for spinning or non-spinning samples. A frequency-ratio method is proposed for referencing 207Pb chemical shifts, based on the 1H and 13C frequencies of the methylammonium cation, which are used asan internal standard. Finally, this new NMR thermometer has been used to measure the degree of frictional heating asa function of spinning frequency for a series of MAS rotors ranging in outer diameter from 1.3 to 7.0mm. As expected, the largest diameter rotors are more susceptible to frictional heating, but lower diameter rotors are subjected to higher frictional heating temperatures as they are typically spun at much higher spinning frequencies.

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