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Multinuclear NMR as a tool for studying local order and dynamics in CH 3 NH 3 PbX 3 (X = Cl, Br, I) hybrid perovskites.
Physical Chemistry Chemical Physics : PCCP 2016 October 6
We report on207 Pb,79 Br,14 N,1 H,13 C and2 H NMR experiments for studying the local order and dynamics in hybrid perovskite lattices.207 Pb NMR experiments conducted at room temperature on a series of MAPbX3 compounds (MA = CH3 NH3 + ; X = Cl, Br and I) showed that the isotropic207 Pb NMR shift is strongly dependent on the nature of the halogen ions. Therefore207 Pb NMR appears to be a very promising tool for the characterisation of local order in mixed halogen hybrid perovskites.207 Pb NMR on MAPbBr2 I served as a proof of concept. Proton,13 C and14 N NMR experiments confirmed the results previously reported in the literature. Low temperature deuterium NMR measurements, down to 25 K, were carried out to investigate the structural phase transitions of MAPbBr3 . Spectral lineshapes allow following the successive phase transitions of MAPbBr3 . Finally, quadrupolar NMR lineshapes recorded in the orthorhombic phase were compared with simulated spectra, using DFT calculated electric field gradients (EFG). Computed data do not take into account any temperature effect. Thus, the discrepancy between the calculated and experimental EFG evidences the fact that MA cations are still subject to significant dynamics, even at 25 K.
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