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Zeitschrift für Kristallographie - Crystalline Materials

Editor-in-Chief: Pöttgen, Rainer

Ed. by Antipov, Evgeny / Bismayer, Ulrich / Boldyreva, Elena V. / Huppertz, Hubert / Petrícek, Václav / Tiekink, E. R. T.

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2196-7105
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Scaled-up solvothermal synthesis of nanosized metastable indium oxyhydroxide (InOOH) and corundum-type rhombohedral indium oxide (rh-In2O3)

Lukas Schlicker
  • Fachgebiet Keramische Werkstoffe/Chair of Advanced Ceramic Materials, Technische Universitat Berlin, Berlin, Germany
  • :
/ Maged F. Bekheet
  • Fachgebiet Keramische Werkstoffe/Chair of Advanced Ceramic Materials, Technische Universitat Berlin, Berlin, Germany
/ Aleksander Gurlo
  • Fachgebiet Keramische Werkstoffe/Chair of Advanced Ceramic Materials, Technische Universitat Berlin, Berlin, Germany
Published Online: 2017-01-28 | DOI: https://doi.org/10.1515/zkri-2016-1967

Abstract

Phase pure metastable indium oxyhydroxide (InOOH) with crystallite size in the range ca. 2–7 nm is synthesized by a nonaqueous solvothermal synthesis route in ethanol. The influence of synthesis parameters such as temperature, basicity (pH), synthesis time, and water content is carefully addressed. T-pH maps summarize the impact of synthesis temperature and pH and reveal that phase pure InOOH is obtained in water-free solutions at mild temperatures (150–180°C) in highly basic conditions (pH>12). Subsequent calcination of InOOH at 375–700°C in ambient air atmosphere results in metastable nanoscaled rhombohedral indium oxide (rh-In2O3). The synthesis protocol for phase pure nanocrystalline InOOH material was successfully upscaled allowing for obtaining ca. 3 g of phase-pure InOOH with a yield of ca. 78%. The upscaled InOOH and rh-In2O3 batches are now available for a detailed in-situ characterization of the mechanism of decomposition of InOOH to rh-In2O3 to c-In2O3 as well as for the characterization of the functional properties of InOOH and rh-In2O3 materials.

Keywords: indium oxide; metastable; nanocrystalline; scale-up; solvothermal synthesis


Received: 2016-06-02

Accepted: 2016-08-29

Published Online: 2017-01-28

Published in Print: 2017-02-01


Citation Information: Zeitschrift für Kristallographie - Crystalline Materials. Volume 232, Issue 1-3, Pages 129–140, ISSN (Online) 2196-7105, ISSN (Print) 2194-4946, DOI: https://doi.org/10.1515/zkri-2016-1967, January 2017

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