Chemical analysis of metal impurity distribution of zone-refined mercuric iodide by ICP-AES and DSC

A mercuric iodide single crystal is being developed for X-ray and gamma-ray detector applications where high-purity starting material is required. Zone-refining processing has been proven to be an effective step in the purification of large amounts of mercuric iodide for crystal growth. In this study we used the Inductively Coupled Plasma-Atomic Emission Spectroscopy (ICP-AES) to identify and determine the distribution of impurity concentrations along the ampoule after zone-refining mercuric iodide. The results show that for Ag, Cu, Fe, Mg, Ca, Zn, Cr and Al, the zone-refining process does sweep the impurities to the last-to-freeze zone, due to an effective distribution coefficient, keff < 1. For Na, Ni, Cd, Mn and Pb the concentration gradient seems to be fairly independent of the position along the ingot. Differential Scanning Calorimetry was also employed to investigate the deviation from stoichiometry caused by the zone-refining process, and the results indicated that the first-to-freeze section is Hg-rich, and the middle section tends to become slightly Hg-rich, while the last-to-freeze section becomes I-rich.