Abstract
Abstract Ball milling is an effective method for the synthesis and modification of light complex hydrides by changing the milling conditions. Using specially designed vials, in-situ variations of the hydrogen pressure and vial temperature taking place during the milling of LiAlH4, with and without dopants, and of LiBH4 + MgCl2 were monitored. This provided information about the efficiency of the reactions before removing the powder from the vial. The thermodynamic properties of the milled hydrides were analysed by differential scanning calorimetry and intelligent gravimetric analysis. Additional structural characterisation was carried out by X-ray diffraction and Raman spectroscopy. The results showed that the decomposition of LiAlH4 during milling is strongly affected by the use of TiCl3 as dopant. The partial formation of Mg(BH4)2 from LiBH4 + MgCl2 was demonstrated by Raman spectroscopy.
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