Technical Notes - Purification of Antimony and Tin by a New Method of Zone Refining

THE purification of two metals, antimony and tin, by zone refining is described, and a reciprocating method of passing molten zones through a straight ingot, which effects a considerable economy of time and apparatus, is discussed. Antimony has been used extensively as a doping agent in germanium and silicon. More recently, it has become important in the preparation of new semiconducting compounds such as InSb, GaSb, and AlSb. High purity is especially necessary in this latter use, since the antimony may comprise as much as 80 pct by weight of the compound. Antimony is generally available in a commercial form of about 99.8 pct purity. Column 1 of Table I is a typical emission spectra analysis of commercially available 99.8 pct antimony. Zone refining has been quite successful in increasing the purity of such samples. Columns 2 to 4 of Table I are analyses of an ingot of the antimony of column 1 after the passage of seven molten zones in an atmosphere of nitrogen. The ingot length was 9 1/2 in.; the mean zone length was 2 in.; convection was the only means of stirring. The column headings are sample locations in inches from the leading end of the ingot. The results illustrate both the merit and a limitation of zone refining. It is seen that four of the five impurities—nickel, arsenic, lead,