Composition-tuning in a solid-state electrotransport furnace with active thermal expansion compensation

Rev Sci Instrum. 2016 Dec;87(12):123903. doi: 10.1063/1.4971300.

Abstract

A new solid-state electrotransport (SSE) apparatus for refining ultra-pure single crystals of metallic compounds under ultra-high vacuum is described. The setup employs a novel thermal expansion compensation mechanism to minimize mechanical stress on the sample during refinement with cold clamps for contamination-less purification at elevated temperatures. The apparatus is designed to tune the composition of initially slightly off-stoichiometric samples. The expansion compensation and stress-free operation were tested by recording the thermal expansion of elemental cerium in a treatment up to 655 °C. SSE refinement was then performed on a high-quality single crystal of U6Fe resulting in a 50% increase of its residual resistivity ratio to the highest value obtained for a single crystal to date.