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On the True Indium Content of In-Filled Skutterudites

Visnow, Eduard and Heinrich, Christophe P. and Schmitz, Andreas and de Boor, Johannes and Leidich, Patrick and Klobes, Benedikt and Hermann, Raphael P. and Müller, Eckhard and Tremel, Wolfgang (2015) On the True Indium Content of In-Filled Skutterudites. Inorganic Chemistry, 54 (16), pp. 7818-7827. ACS Publications. DOI: 10.1021/acs.inorgchem.5b00799 ISSN 0020-1669

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Abstract

The incongruently melting single-filled skutterudite InxCo4Sb12 is known as a promising bulk thermoelectric material. However, the products of current bulk syntheses contain always impurities of InSb, Sb, CoSb, or CoSb2, which prevent an unbiased determination of its thermoelectric properties. We report a new two-step synthesis of high-purity InxCo4Sb12 with nominal compositions x = 0.12, 0.15, 0.18, and 0.20 that separates the kieftite (CoSb3) formation from the topotactic filler insertion. This approach allows conducting the reactions at lower temperatures with shorter reaction times and circumventing the formation of impurity phases. The synthesis can be extended to other filled skutterudites. High-density (>98%) pellets for thermoelectric characterization were prepared by current-assisted short-time sintering. Sample homogeneity was demonstrated by potential and Seebeck microprobe measurements of the complete pellet surfaces. Synchrotron X-ray diffraction showed a purity of 99.9% product with traces (≤0.1%) of InSb in samples of nominal composition In0.18Co4Sb12 and In0.20Co4Sb12. Rietveld refinements revealed a linear correlation between the true In occupancy and the lattice parameter a. This allows the determination of the true In filling in skutterudites and predicting the In content of unknown AxCo4Sb12. The high purity of InxCo4Sb12 allowed studying the transport properties without bias from side phases. A figure of merit close to unity at 420 °C was obtained for a sample of a true composition of In0.160(2)Co4Sb12 (nominal composition In0.18Co4Sb12). The lower degree of In filling has a dramatic effect on the thermoelectric properties as demonstrated by the sample of nominal composition In0.20Co4Sb12. The presence of InSb in amounts of ∼0.1 vol% led to a substantially lower degree of interstitial site filling of 0.144, and the figure of merit zT decreased by 18%, which demonstrates the significance of the true filler atom content in skutterudite materials.

Item URL in elib:https://elib.dlr.de/100041/
Document Type:Article
Title:On the True Indium Content of In-Filled Skutterudites
Authors:
AuthorsInstitution or Email of AuthorsAuthors ORCID iD
Visnow, EduardInstitut für Anorganische Chemie und Analytische Chemie, Johannes Gutenberg-Universität, Duesbergweg 10-14, D-55099 Mainz, GermanyUNSPECIFIED
Heinrich, Christophe P.Institut für Anorganische Chemie und Analytische Chemie, Johannes Gutenberg-Universität, Duesbergweg 10-14, D-55099 Mainz, Germany and Graduate School Materials Science in Mainz, Johannes Gutenberg-Universität, Staudinger Weg 9, 55128 Mainz, GermanyUNSPECIFIED
Schmitz, AndreasGerman Aerospace Center, Institute of Materials Research, Köln, GermanyUNSPECIFIED
de Boor, JohannesGerman Aerospace Center, Institute of Materials Research, Köln, GermanyUNSPECIFIED
Leidich, PatrickInstitut für Anorganische Chemie und Analytische Chemie, Johannes Gutenberg-Universität, Duesbergweg 10-14, D-55099 Mainz, GermanyUNSPECIFIED
Klobes, BenediktJuelich Centre for Neutron Science und P. Gruenberg Inst. PGI, JARA-FIT, FZ Juelich, 52425UNSPECIFIED
Hermann, Raphael P.Peter Grünberg Institut and Jülich Centre for Neutron Science, JARA-FIT, Forschungszentrum Jülich GmbH, D-52425 Jülich, Germany and Faculte des Sciences, Universite de Liege, B-4000, Liege, BelgiumUNSPECIFIED
Müller, EckhardGerman Aerospace Center, Institute of Materials Research, Köln, Germany and Justus Liebig University Giessen, Institute of Inorganic and Analytical Chemistry, 35392 Giessen, GermanyUNSPECIFIED
Tremel, WolfgangInstitut für Anorganische Chemie und Analytische Chemie, Johannes Gutenberg-Universität, Duesbergweg 10-14, D-55099 Mainz, GermanyUNSPECIFIED
Date:17 August 2015
Journal or Publication Title:Inorganic Chemistry
Refereed publication:Yes
Open Access:No
Gold Open Access:No
In SCOPUS:Yes
In ISI Web of Science:Yes
Volume:54
DOI :10.1021/acs.inorgchem.5b00799
Page Range:pp. 7818-7827
Publisher:ACS Publications
ISSN:0020-1669
Status:Published
Keywords:filled skutterudites, thermoelectric material
HGF - Research field:Aeronautics, Space and Transport
HGF - Program:Transport
HGF - Program Themes:Terrestrial Vehicles (old)
DLR - Research area:Transport
DLR - Program:V BF - Bodengebundene Fahrzeuge
DLR - Research theme (Project):V - Fahrzeugenergiesystem III (old)
Location: Köln-Porz
Institutes and Institutions:Institute of Materials Research > Thermoelectric Materials and Systems
Deposited By: Zabrocki, Dr. Knud
Deposited On:27 Nov 2015 09:46
Last Modified:30 May 2019 22:07

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