Kalisvaart, W.P.; Luber, E.J.; Poirier, E.; Harrower, C.T.; Teichert, A.; Wallacher, D.; Grimm, N.; Steitz, R.; Fritzsche, H.; Mitlin, D.: Probing the Room Temperature Deuterium Absorption Kinetics in Nanoscale Magnesium Based Hydrogen Storage Multilayers Using Neutron Reflectometry, X-ray Diffraction, and Atomic Force Microscopy. The Journal of Physical Chemistry C 116 (2012), p. 5868-5880
Magnesium hydride has high storage capacity (7.6 wt % H) but very slow sorption kinetics. Addition of catalytic phases on the surface as well as alloying with transition metals is known to improve the properties. In this study, the sorption kinetics of a 50-nm Mg layer and Mg-10%Cr-10%V layer, capped with a CrV/Pd bilayer catalyst, are compared using a combination of neutron reflectometry (NR), X-ray diffraction (XRD), and atomic force microscopy to elucidate the effects of alloying on the hydrogen storage properties of Mg at room temperature. From NR it is found that the Cr?V alloyed layer shows both a delay in expansion in the first absorption cycle and a delay in contraction in the first desorption, which indicates a delay in nucleation of MgD2 and formation of substoichiometric MgD2-δ, respectively. Compared to pure Mg, the kinetics are strongly improved as no blocking MgD2 layer is formed. XRD showed a strong reduction in the Mg grain size for the Cr?V alloyed layer after one cycle. For pure Mg, the grain size is almost unchanged although the film becomes nanocrystalline in the hydrided state. NR is shown to be highly sensitive to both the deuterium distribution as well as the layer thickness, which makes it a valuable tool for studying reaction mechanisms and quantification of the expansion of both crystalline and amorphous energy storage materials.