%0 journal article %@ 0360-3199 %A Heere, M., Soerby, M.H., Pistidda, C., Dornheim, M., Hauback, B.C. %D 2016 %J International Journal of Hydrogen Energy %N 30 %P 13101-13108 %R doi:10.1016/j.ijhydene.2016.05.153 %T Milling time effect of Reactive Hydride Composites of NaF-NaH-MgB2 investigated by in situ powder diffraction %U https://doi.org/10.1016/j.ijhydene.2016.05.153 30 %X Light metal complex borohydrides have high hydrogen storage capacities but suffer from drawbacks of slow hydrogen sorption kinetics, poor reversibility and high thermodynamic stability. The NaF + 9NaH + 5MgB2 composite has a theoretical hydrogen capacity of 7.7 wt% H assuming the formation of 10NaBH3.9F0.1 + 5MgH2. Hydrogenation and dehydrogenation properties as well as the effect of different ball milling times have been investigated. The in situ hydrogenation is faster in the composite ball milled for 87 h than the 5 h milled composite. A boron-rich phase with space group Pa-3, a = 7.4124(5) Å was formed during hydrogenation at 325 °C and 50 bar hydrogen for both short and long milling times. In the long milled composite the boron-rich phase disappeared after 3 h of hydrogenation, whereas it became a major phase in the short milled composite after 1.5 h of hydrogenation. NaBH4 was formed at 206 °C. NaMgH1-xFx was formed at 290 °C instead of the assumed MgH2. The same phases formed at 268 °C and 325 °C, respectively, and only in minor amounts in the short milled composite. Ex situ hydrogenation in a Sieverts' type apparatus at the same temperature and hydrogen pressure conditions followed a different reaction pathway with formation of MgH2 in addition to NaBH4 and NaMgH3-xFx (0 ≤ x ≤ 1). The measured hydrogen uptake was 6.0 and 6.3 wt% for the long and short milled composites, respectively.