Crystal structure and stability of LiAlD4 with TiF3 additive

LiAlD4 samples with TiF3 additives have been investigated by synchrotron X-ray diffraction, neutron diffraction and a Sieverts-type apparatus. Directly after ball milling there are no signs of any Ti-containing phases, and the unit-cell of LiAlD4 and Al give no indication of any solid solutions. Hence it is concluded that the Ti is in an amorphous state directly after ball milling. Furthermore, no LiF was observed in the samples. Based on Sieverts-type measurements the plateau pressure at 80 °C has been proved to be higher than 85 bar. Samples stored in a glove box are slowly desorbed, and after 6 months for a LiAlD4 + TiF3 sample, the reaction to LiD + Al is nearly finished.