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Inorganics 2016, 4(4), 35; doi:10.3390/inorganics4040035

In Situ Studies and Magnetic Properties of the Cmcm Polymorph of LiCoPO4 with a Hierarchical Dumbbell-Like Morphology Synthesized by Easy Single-Step Polyol Synthesis

1
Synthesis and Characterization of Innovative Materials, Department of Chemistry, Technical University of Munich, Lichtenbergstraße 4, 85747 Garching, Germany
2
Chair of Inorganic Chemistry with Focus on Novel Materials, Department of Chemistry, Technical University of Munich, Lichtenbergstraße 4, 85747 Garching, Germany
3
BMW AG, Petuelring 130, 80788 München, Germany
These authors contributed equally to this work.
*
Author to whom correspondence should be addressed.
Academic Editor: Richard Dronskowski
Received: 6 October 2016 / Revised: 9 November 2016 / Accepted: 10 November 2016 / Published: 17 November 2016
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Abstract

LiCoPO4 (LCP) exists in three different structural modifications: LCP-Pnma (olivine structure), LCP-Pn21a (KNiPO4 structure type), and LCP-Cmcm (Na2CrO4 structure type). The synthesis of the LCP-Cmcm polymorph has been reported via high pressure/temperature solid-state methods and by microwave-assisted solvothermal synthesis. Phase transitions from both LCP-Pn21a and LCP-Cmcm to LCP-Pnma upon heating indicates a metastable behavior. However, a precise study of the structural changes during the heating process and the magnetic properties of LCP-Cmcm are hitherto unknown. Herein, we present the synthesis and characterization of LCP-Cmcm via a rapid and facile soft-chemistry approach using two different kinetically controlled pathways, solvothermal and polyol syntheses, both of which only require relatively low temperatures (~200 °C). Additionally, by polyol, method a dumbbell-like morphology is obtained without the use of any additional surfactant or template. A temperature-dependent in situ powder XRD shows a transition from LCP-Cmcm at room temperature to LCP-Pnma and finally to LCP-Pn21a at 575 and 725 °C, respectively. In addition to that, the determination of the magnetic susceptibility as a function of temperature indicates a long-range antiferromagnetic order below TN = 11 K at 10 kOe and 9.1 K at 25 kOe. The magnetization curves suggests the presence of a metamagnetic transition. View Full-Text
Keywords: polymorph; LiCoPO4-Cmcm; metamagnetic transition; in situ XRD; polyol; solvothermal; transition phase; hierarchical morphology polymorph; LiCoPO4-Cmcm; metamagnetic transition; in situ XRD; polyol; solvothermal; transition phase; hierarchical morphology
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MDPI and ACS Style

Alarcón-Suesca, C.; Ludwig, J.; Hlukhyy, V.; Stinner, C.; Nilges, T. In Situ Studies and Magnetic Properties of the Cmcm Polymorph of LiCoPO4 with a Hierarchical Dumbbell-Like Morphology Synthesized by Easy Single-Step Polyol Synthesis. Inorganics 2016, 4, 35.

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