Access to metastable complex ion conductors via mechanosynthesis: Preparation, microstructure and conductivity of (Ba,Sr)LiF3 with inverse perovskite structure

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Original languageEnglish
Pages (from-to)6238-6250
Number of pages13
JournalJournal of Materials Chemistry
Volume21
Issue number17
Early online date24 Mar 2011
Publication statusPublished - 7 May 2011

Abstract

Highly metastable Ba1-xSrxLiF3 (0 < x ≤ xmax ≈ 0.4) with an inverse perovskite structure analogous to that of BaLiF3 was synthesized by soft mechanical treatment of BaF2 and LiF together with SrF2 at ambient temperature. Ex as well as in situ X-ray powder diffraction (XRPD) measurements show that heat treatment at 393 K initiates the decomposition of the mixed phase into BaLiF3, LiF and (Sr,Ba)F2. Structural details of the metastable compound (Ba,Sr)LiF3 were investigated by ultrafast 19F magic angle spinning (MAS) nuclear magnetic resonance (NMR) spectroscopy. Interestingly, five magnetically inequivalent F sites were identified which correspond to fluorine anions coordinated by a variable number of Ba and Sr cations, respectively. Details from XRPD and NMR spectroscopy are discussed with respect to the formation mechanisms and thermal stability of the as prepared fluorides. Impedance spectroscopy is used to characterize (long-range) ionic transport properties. Results are compared with those obtained recently on mechanosynthesized BaLiF3.

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Access to metastable complex ion conductors via mechanosynthesis: Preparation, microstructure and conductivity of (Ba,Sr)LiF3 with inverse perovskite structure. / Düvel, André; Wegner, S.; Efimov, Konstantin et al.
In: Journal of Materials Chemistry, Vol. 21, No. 17, 07.05.2011, p. 6238-6250.

Research output: Contribution to journalArticleResearchpeer review

Düvel A, Wegner S, Efimov K, Feldhoff A, Heitjans P, Wilkening M. Access to metastable complex ion conductors via mechanosynthesis: Preparation, microstructure and conductivity of (Ba,Sr)LiF3 with inverse perovskite structure. Journal of Materials Chemistry. 2011 May 7;21(17):6238-6250. Epub 2011 Mar 24. doi: 10.1039/c0jm03439h
Düvel, André ; Wegner, S. ; Efimov, Konstantin et al. / Access to metastable complex ion conductors via mechanosynthesis : Preparation, microstructure and conductivity of (Ba,Sr)LiF3 with inverse perovskite structure. In: Journal of Materials Chemistry. 2011 ; Vol. 21, No. 17. pp. 6238-6250.
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T1 - Access to metastable complex ion conductors via mechanosynthesis

T2 - Preparation, microstructure and conductivity of (Ba,Sr)LiF3 with inverse perovskite structure

AU - Düvel, André

AU - Wegner, S.

AU - Efimov, Konstantin

AU - Feldhoff, Armin

AU - Heitjans, Paul

AU - Wilkening, M.

PY - 2011/5/7

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N2 - Highly metastable Ba1-xSrxLiF3 (0 < x ≤ xmax ≈ 0.4) with an inverse perovskite structure analogous to that of BaLiF3 was synthesized by soft mechanical treatment of BaF2 and LiF together with SrF2 at ambient temperature. Ex as well as in situ X-ray powder diffraction (XRPD) measurements show that heat treatment at 393 K initiates the decomposition of the mixed phase into BaLiF3, LiF and (Sr,Ba)F2. Structural details of the metastable compound (Ba,Sr)LiF3 were investigated by ultrafast 19F magic angle spinning (MAS) nuclear magnetic resonance (NMR) spectroscopy. Interestingly, five magnetically inequivalent F sites were identified which correspond to fluorine anions coordinated by a variable number of Ba and Sr cations, respectively. Details from XRPD and NMR spectroscopy are discussed with respect to the formation mechanisms and thermal stability of the as prepared fluorides. Impedance spectroscopy is used to characterize (long-range) ionic transport properties. Results are compared with those obtained recently on mechanosynthesized BaLiF3.

AB - Highly metastable Ba1-xSrxLiF3 (0 < x ≤ xmax ≈ 0.4) with an inverse perovskite structure analogous to that of BaLiF3 was synthesized by soft mechanical treatment of BaF2 and LiF together with SrF2 at ambient temperature. Ex as well as in situ X-ray powder diffraction (XRPD) measurements show that heat treatment at 393 K initiates the decomposition of the mixed phase into BaLiF3, LiF and (Sr,Ba)F2. Structural details of the metastable compound (Ba,Sr)LiF3 were investigated by ultrafast 19F magic angle spinning (MAS) nuclear magnetic resonance (NMR) spectroscopy. Interestingly, five magnetically inequivalent F sites were identified which correspond to fluorine anions coordinated by a variable number of Ba and Sr cations, respectively. Details from XRPD and NMR spectroscopy are discussed with respect to the formation mechanisms and thermal stability of the as prepared fluorides. Impedance spectroscopy is used to characterize (long-range) ionic transport properties. Results are compared with those obtained recently on mechanosynthesized BaLiF3.

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