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Volume 151, 2011
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Hydride formation in Mg-based systems processed by reactive milling

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Abstract

The possibilities to produce quaternary Mg-based transition-metal complex hydrides have been explored. Mg2Mn1−xFex (x = 0.5, 0) elemental powder mixtures were ball milled in a reactive D2 atmosphere (about 5 MPa). The results were compared with the formation of Mg2(FeD6)0.5(CoD5)0.5 from Mg–Fe–Co powders. The changes of D2 pressure were monitored during milling and deuterium absorption was detected within the first 15 h of milling. Powder X-ray and neutron diffraction analysis for the as-milled Mg2Mn0.5Fe0.5 powder showed a large fraction of unreacted elemental Mn, as well as the formation of a cubic K2PtCl6-type phase (a = 6.452 Å). The latter could be identified as Mg2FeD6. Infrared spectroscopy confirmed the presence of [FeD6]4 anions (stretching band at 1261 cm−1) and ruled out the formation of [MnH6]5 complexes. As for the as-milled Mg2Mn, powder diffraction analysis showed the formation of MgD2 as the main reaction product. A small fraction of a cubic K2PtCl6-type phase (a = 6.526 Å) was also observed. This was identified as a Mg2FeD6-type compound. It was likely formed as a result of Fe impurities originating from the milling media and detected by EDX analysis. Infrared spectroscopy confirmed the presence of the [FeD6]4 complex (stretching band at 1259 cm−1) and showed an additional band at 1313 cm−1. The likelihood of this band arising from Mn–D bonds is discussed. Finally, deuterium desorption upon heating, was investigated for all systems by differential scanning calorimetry.

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Article information


Submitted
19 Feb 2011
Accepted
25 Feb 2011
First published
19 May 2011

Faraday Discuss., 2011,151, 315-326
Article type
Paper

Hydride formation in Mg-based systems processed by reactive milling

S. Deledda and B. C. Hauback, Faraday Discuss., 2011, 151, 315
DOI: 10.1039/C1FD00023C

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