Synthesis and characterization of a nanophase zirconium powder

The reaction of ZrI4 with LiH in diethyl ether at ambient temperature produced an initial mixture of nanophase zirconium powder and LiI. After removal of most of the LiI by washing with ether, the remaining powder was annealed at 527 °C, 600 °C, and 650 °C. The X-ray powder diffraction patterns of the annealed samples were consistent with the presence of Zr3O and ZrC. Transmission electron micrographs revealed that most of the sample annealed at 650 °C consisted of 6.3 nm particles, although some platelets as large as 100 nm across were present. The zirconium suboxide Zr3O was identified from lattice spacings and ZrC from electron diffraction. In combination with results from elemental analyses, it is concluded that the annealed sample contained 18 wt% ZrC, 44 wt% Zr3O, 9 wt% of a zirconium iodide, and 28 wt% Zr.