Journal
ZEITSCHRIFT FUR KRISTALLOGRAPHIE-CRYSTALLINE MATERIALS
Volume 232, Issue 1-3, Pages 129-140Publisher
WALTER DE GRUYTER GMBH
DOI: 10.1515/zkri-2016-1967
Keywords
indium oxide; metastable; nanocrystalline; scale-up; solvothermal synthesis
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Funding
- DFG [GU 992/12-1]
- Office of Science, Office of Basic Energy Sciences, of the U.S. Department of Energy [DE-AC02-05CH11231]
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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 degrees C) in highly basic conditions (pH > 12). Subsequent calcination of InOOH at 375-700 degrees 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.
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