Microstructural characterization of catalyzed NaAlH4

A number of laboratories have now demonstrated that catalyst-assisted NaAlH4 can reversibly absorb and desorb hydrogen in the solid state at moderate temperatures. An understanding of the mechanisms by which bulk decomposition and reformation of the compound can occur in the presence of a surface catalyst is important to improving the kinetic and thermodynamic properties of alanates for use in hydrogen storage applications. Using scanning electron microscopy (SEM) and energy dispersive spectroscopy (EDS), we have examined the microstructure and elemental composition of Na alanate samples, doped using a liquid Ti/Zr catalyst precursor, for a number of conditions. First, microscopy and compositional analyses were performed at different stages of the decomposition process within the first desorption cycle. Second, the material was characterized after multiple absorption/desorption cycles (five cycles). Finally, the effects of the catalyst doping procedure on particle size, surface morphology and surface composition were examined. Significant changes in particle morphology and in elemental distribution were found to be induced by the desorption and cycling processes. Importantly, our measurements indicate that the initial dehydriding reactions were accompanied by significant enhancement of Al concentration toward the surface of particles and that elemental segregation occurred with repeated absorption/desorption cycles. (C) 2002 Published by Elsevier Science B.V.