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Open AccessArticle

Binary Alkali-Metal Silicon Clathrates by Spark Plasma Sintering: Preparation and Characterization

Max-Planck-Institut für Chemische Physik fester Stoffe, 01187 Dresden, Germany
Department of Physics, California Polytechnic State University, San Luis Obispo, CA 93407, USA
Department of Physics, University of South Florida, Tampa, FL 33620, USA
Authors to whom correspondence should be addressed.
Academic Editor: Javier Narciso
Materials 2016, 9(7), 593;
Received: 13 June 2016 / Revised: 12 July 2016 / Accepted: 13 July 2016 / Published: 19 July 2016
(This article belongs to the Special Issue Inorganic Clathrate Materials)
The binary intermetallic clathrates K8-xSi46 (x = 0.4; 1.2), Rb6.2Si46, Rb11.5Si136 and Cs7.8Si136 were prepared from M4Si4 (M = K, Rb, Cs) precursors by spark-plasma route (SPS) and structurally characterized by Rietveld refinement of PXRD data. The clathrate-II phase Rb11.5Si136 was synthesized for the first time. Partial crystallographic site occupancy of the alkali metals, particularly for the smaller Si20 dodecahedra, was found in all compounds. SPS preparation of Na24Si136 with different SPS current polarities and tooling were performed in order to investigate the role of the electric field on clathrate formation. The electrical and thermal transport properties of K7.6Si46 and K6.8Si46 in the temperature range 4–700 K were investigated. Our findings demonstrate that SPS is a novel tool for the synthesis of intermetallic clathrate phases that are not easily accessible by conventional synthesis techniques. View Full-Text
Keywords: spark plasma synthesis; Zintl phase; intermetallic clathrate spark plasma synthesis; Zintl phase; intermetallic clathrate
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MDPI and ACS Style

Veremchuk, I.; Beekman, M.; Antonyshyn, I.; Schnelle, W.; Baitinger, M.; Nolas, G.S.; Grin, Y. Binary Alkali-Metal Silicon Clathrates by Spark Plasma Sintering: Preparation and Characterization. Materials 2016, 9, 593.

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