Chandran, C. Vinod

Heitjans, Paul

Pristat, Sylke

Tietz, Frank

Witt, Elena

English

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The Open-Access Journal for the Basic Principles of Diffusion Theory, Experiment and Application Solid-State NMR Studies on Li+ Ion Dynamics and Structure of  Li1+xAlxTi2-x(PO4)3 C. Vinod Chandran,1 Sylke Pristat,2 Elena Witt,1 Frank Tietz,2 Paul Heitjans1 1Institut für Physikalische Chemie und Elektrochemie, Leibniz Universität Hannover, Callinstr. 3 - 3a, 30167 Hannover, Germany 2Forschungszentrum Jülich GmbH, Jülich, Wilhelm-Johnen-Straße 52425 Jülich, Germany  Corresponding author: Paul Heitjans, E-Mail: heitjans@pci.uni-hannover.de Solid-state nuclear magnetic resonance (NMR) studies of Li+ ion dynamics based on spin-lattice relaxation (SLR) experiments on lithium aluminum titanium phosphates (LATP) are reported. The samples were synthesized by conventional solid-state reaction using stoichiometric amounts of Li2CO3, TiO2, (NH4)H2PO4 and Al2O3 at high pressure and heated in a Pt crucible up to 1000 °C for 12 hours [1-4]. LATP with different lithium contents is studied with 7Li SLR measurements (in the laboratory frame (T1) and rotating frame (T1)) as well as multinuclear magic-angle spinning (MAS) NMR experiments. The solid-state SLR experiments were done with a Bruker 600 AV-III spectrometer at a 7Li Larmor frequency of 233 MHz over a wide range of temperature. The high-temperature range was achieved using LASER-heating in a 7mm MAS probe at 3 kHz spinning. 7Li, 27Al and 31P MAS NMR measurements were done using a 4mm MAS probe at 7-11 kHz spinning frequencies.    Fig. 1: 31P and 27Al MAS (at 11 kHz) NMR of Li1+xAlxTi2-x(PO4)3 with different cation contents.  From the diffusion induced 7Li NMR SLR rates Li jump rates and activation energies were deduced and the LATPs were found to be fairly fast ion conductors. The different compositions provided signature NMR signals for different cation stoichiometries (Fig. 1). From the various NMR methods, a detailed characterization of LATPs is obtained, with information on local ion dynamics and many structural aspects.  References  [1] B. Key, D. J. Schroeder, B. J. Ingram, J. T. Vaughey, Chem. Mater. 24 (2012) 287-293. [2] S. Duluard, A. Paillassa, L. Puech, P. Vinatier, V. Turq, P. Rozier, P. Lenormand, P. L. Taberna, P. Simon, F.  Ansart, J. Eur. Ceram. Soc. 33 (2013) 1145-1153. [3] H. Morimoto, H. Awano, J. Terashima, Y. Shindo, S. Nakanishi, N. Ito, K. Ishikawa, S. Tobishima, J. Pow.  Sources 240 (2013) 636-643. [4] E. Dashjav, R. Hermann, F. Tietz, poster presentation, this conference.   This work is licensed under a Creative Commons Attribution 4.0 International License. To view a copy of this license, visit http://creativecommons.org/licenses/by/4.0/1

Solid-State NMR Studies on Li+ Ion Dynamics and Structure of Li1+xAlxTi2-x(PO4)3

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Solid-State NMR Studies on Li+ Ion Dynamics and Structure of Li1+xAlxTi2-x(PO4)3

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