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.

在这项研究中，讨论了基于碘的还原法低温固态合成纯纳米晶六硼化Y（YbB ₆）。对于还原反应，将氧化y，氧化硼，镁和碘的机械活化粉末混合物在石英管中的Ar下加热至85°C。所有反应副产物，即。通过用3 M HCl溶液进行热酸浸提法去除MgO，Mg ₃（BO ₃）₂和YbI ₂，以形成纯YbB ₆。合成的YbB ₆的形态和相结构通过X射线衍射（XRD），高分辨率透射电子显微镜（HRTEM）和拉曼光谱分析粉末。通过多相Rietveld精制来精制获得的结晶相。XRD和拉曼光谱显示通过当前基于碘的低温还原方法形成的纳米YbB ₆与机械化学方法之间的对比。所述YBB ₆通过低温还原碘法制造在性质上是高度结晶的，而YBB ₆通过机械化学方法制备的是较低结晶或相反地在性质上更无定形的。基于碘的还原方法确实起到了决定性的作用，使反应在较低的温度下发生，从而形成了纳米晶体YbB。₆。