Synthesis and Structural Characterization of Ca<sub>14</sub>Nb<i><sub>x</sub></i>In<sub>1<i>-</i></sub><i><sub>x</sub></i>As<sub>11</sub> (<i>x</i> ≈ 0.85)

Abstract

Single-crystals of the new compound Ca14NbxIn1–xAs11 have been obtained from a solid-state reaction in a sealed Nb ampoule. The initial experiment had been set up with the aim to investigate the effect of electron doping (via In) on the crystal structure and physical properties of Ca14MnAs11. Subsequent single-crystal X-ray diffraction and elemental analysis work suggested that instead of Ca14MnxIn1–xAs11, the major product of the reaction is the phase Ca14NbxIn1–xAs11. This supposition was corroborated when the title compound was synthesized from a reaction of Ca, In and As in a sealed Nb ampoule, proving that, 1) Mn metal is not included in the structure, and 2) that the inadvertent side reaction of As with the walls of the Nb container is the source of the niobium. The overall structure is isotypic with the tetragonal Ca14AlSb11 structure type (space group I41/acd), although some marked differences between the two must be noted. Current ongoing work is focused on the synthesis of phase pure polycrystalline samples and determination of the physical properties of this unusual transition metal Zintl phase.