Structural and In Situ X-ray Diffraction Study of Hydrogenation of CaxMg1-xNi2 (0 ≤ x ≤ 1)

In the quasi-binary system CaNi2-MgNi2 solid-solutions CaxMg1-xNi2 (0 <= x <= 1) were prepared from the elements. They crystallize in the hexagonal Laves phase type (MgNi2, C36) for x <= 0.33 (P6(3)/mmc, a = 482.51(7) pm, c = 1582.1(3) pm for x = 0, a = 482.59(3), c = 1583.1(1) for x = 0.33) and in the cubic Laves phase type (MgCu2, C15) for 0.33 < x (Fd3m, a = 697.12(3) pm for x = 0.5, a = 705.11(2) pm for x = 0.67, a = 724.80(2) pm for x = 1). After hydrogenation in an autoclave the X-ray diffraction patterns changed completely. Reflections assigned to CaNiH3, and Ni and Rietveld refinement confirmed this. The hydrogenation properties of CaxMg1-xNi2 (0 <= x <= 1) compounds were also studied in situ by X-ray powder diffraction. In situ X-ray powder diffraction of CaxMg1-xNi2 (0 <= x <= 1) compounds under 0.3 MPa hydrogen gas flow (15 sccm), data collected on a Rigaku SmartLab diffractometer in an Anton Paar XRK 900 Reactor Chamber using Cu-K alpha 1 radiation. Scanning electron microscopy and EDX spectroscopy confirmed the entitled materials and elemental composition, respectively. From the Transmission electron microscopy and Selected area electron diffraction concluded that the CaxMg1-xNi2 (0 <= x <= 1) compounds were crystalline.

Automated summary

This study prepared solid solutions CaxMg1-xNi2 (0 <= x <= 1) in the quasi-binary system CaNi2-MgNi2 and investigated their crystal structures and hydrogenation properties. The results show significant changes in the crystal structure and hydrogenation properties of the compounds within different compositional ranges.