Cubic Bixbyite‐Structured Phases of Yb6MoO12 and Y6MoO12 Prepared by the Solution Combustion Method at Low Temperatures. Issue 15 (25th April 2017)

• Record Type: Journal Article
• Authors: Schildhammer, Daniel; Fuhrmann, Gerda; Petschnig, Lucas; Partl, Gabriel; Götsch, Thomas; Penner, Simon; Schaur, Andreas; Saxer, Andreas; Schottenberger, Herwig; Huppertz, Hubert
• Is Part Of: European journal of inorganic chemistry. Issue 15(2017)
• Page Start: 2265
• Page End: 2269
• Publication Date: 2017-04-25
• Subjects: Rare earths -- Molybdenum -- Solution combustion -- Structure elucidation; Chemistry, Inorganic -- Periodicals; Organometallic chemistry -- Periodicals; Bioinorganic chemistry -- Periodicals; Solid state chemistry -- Periodicals; 546
• DOI: 10.1002/ejic.201700087
• Languages: English
• ISSNs: 1434-1948

Abstract

Abstract : For the first time, Yb6 MoO12 was synthesized in the cubic bixbyite structure type ( Ia 3 ) under low‐temperature conditions. The solution combustion method was used to prepare an amorphous precursor at a temperature of 400 °C. Subsequent calcination at around 600 °C initiated the crystallization process, accompanied by the decomposition of remnant organic material, leading to a carbonate precursor. Further increase of the temperature to 800 °C resulted in a decarboxylation of the precursor, converting it into a highly crystalline cubic phase. A second phase transition into a rhombohedral structure was observed at a temperature around 1000 °C. Detailed phase transition studies were performed by powder X‐ray diffraction (PXRD), thermal analysis (TG‐DTA), attenuated total reflection infrared spectroscopy (ATR‐IR), and X‐ray photoelectron spectroscopy (XPS) analysis. Furthermore, the analogous yttrium compound Y6 MoO12 was prepared by the same method. Contrary to previous reports, the structure analysis revealed that Y6 MoO12 crystallizes in the same highly symmetric cubic structure ( Ia 3 ). Due to the thermal stability differences of the corresponding rare earth oxides and molybdenum oxide, both cubic low‐temperature phases Yb6 MoO12 and Y6 MoO12 are presumably not attainable by classical solid‐state reactions. Abstract : A cubic low‐temperature phase of Yb6 MoO12 was synthesized for the first time by the solution combustion method. The new structure was solved by Rietveld refinement and characterized by XPS, DTA‐TG, and ATR‐IR spectroscopy. Additionally, a pre‐phase containing a carbonate unit was determined.