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The dehydriding process and hydrogen–deuterium exchange (H–D exchange) of xLiBH4 + (1 − x)Mg2FeD6 (x = 0.25, 0.75) composites has been studied in detail. For the composition with x = 0.25, only one overlapping mass peak of all hydrogen and deuterium related species was observed in mass spectrometry. This implied the simultaneous dehydriding of LiBH4 and Mg2FeD6, despite an almost 190 °C difference in the dehydriding temperatures of the respective discrete complex hydrides. In situ infrared spectroscopy measurements indicated that H–D exchange between [BH4]− and [FeD6]4− had occurred during ball-milling and was promoted upon heating. The extent of H–D exchange was estimated from the areas of the relevant mass signals: immediately prior to the dehydriding, more than two H atoms in [BH4]− was replaced by D atoms. For x = 0.75, H–D exchange also occurred and about one to two H atoms in [BH4]− was replaced by  D atoms immediately before the dehydriding. In contrast to the situation for x = 0.25, firstly LiBH4 and Mg2FeD6 dehydrided simultaneously with a special molar ratio = 1:1 at  x = 0.75, and then the remaining LiBH4 reacted with the Mg and Fe derived from the dehydriding of Mg2FeD6

Dehydriding Process and Hydrogen–Deuterium Exchange of LiBH4–Mg2FeD6 Composites