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Preparation of single-phase YbB6 by low-temperature solid-state reaction method using iodine

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Abstract

In this study, low-temperature solid-state synthesis of pure nanocrystalline ytterbium hexaboride (YbB6) employing iodine-based reduction method has been discussed. For the reduction reaction, the mechanically activated powder mixture of ytterbium oxide, boron oxide, magnesium, and iodine was heated up under Ar in a quartz tube to 85 °C. All reaction byproducts, viz. MgO, Mg3(BO3)2, and YbI2, were removed by hot acid leaching with 3 M HCl solution to form pure YbB6. The morphological and phase structure of the synthesized YbB6 powder were analyzed by X-ray diffractometry (XRD), high-resolution transmission electron microscopy (HRTEM), and Raman spectroscopy. The crystalline phases obtained were refined by multi-phase Rietveld refinement. XRD and Raman spectroscopy showed a contrast between the nano-YbB6 formed by the present low-temperature iodine-based reduction method versus mechanochemical method. The YbB6 produced by the low-temperature iodine reduction method is highly crystalline in nature, whereas YbB6 produced by mechanochemical method is less crystalline or conversely more amorphous in nature. The iodine-based reduction method indeed played a definitive role to allow the reaction to take place at a lower temperature enabling the formation of nanocrystalline YbB6.

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Acknowledgments

The author would like to thank Eti Maden Works General Managements for the used laboratory facilities and Dr. Arun K. Chattopadhyay of Uniformity Labs, California, for the critical reading and ungrudging assistance for preparing the manuscript, and the author is also thankful to the Middle East Technical University, Central Laboratory for sample analysis.

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  1. Department of Mechanical and Metal Technologies, Kırıkkale Vocational High School, Kırıkkale University, 71450, Kırıkkale, Turkey

    Tuncay Simsek

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Simsek, T. Preparation of single-phase YbB6 by low-temperature solid-state reaction method using iodine. J Aust Ceram Soc 57, 125–136 (2021). https://doi.org/10.1007/s41779-020-00521-w

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