In situ thermodiffraction to monitor synthesis and thermolysis of hydrazine borane-based materials
(2016) Journal of Alloys and Compounds — Vol. 659, n° 25 February 2016, p. 210-216 (2016)
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- Hydrazine borane N2H4BH3 (HB) and its alkali metal derivatives, i.e. sodium hydrazinidoborane NaN2H3BH3 (NaHB) and lithium hydrazinidoborane β-LiN2H3BH3 (β-LiHB), are novel materials under investigation for solid-state chemical hydrogen storage. Herein, we report in situ thermodiffraction experiments developed to monitor synthesis of NaHB at low temperatures (from -173 °C) and a thermolysis of each of the boranes, manifesting the following main observations. (i) Dehydrogenation of HB starts with the liquid phase and dehydrocoupling involves the formation of a crystalline intermediate (at 90-197 °C). (ii) NaHB forms from -38 °C, melts at ca. 60 °C, and decomposes upon melting at higher temperatures. (iii) β-LiHB dehydrogenates to a small extent starting from 40 °C, but mostly transforms to the high-temperature phase α-LiHB at 91 °C; up to around 150 °C, the two crystalline phases dehydrogenate according to a complex stepwise mechanism. Our results help in gaining insight in synthesis and thermolysis of the aforementioned novel hydrazine borane-based materials.
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Moury, R., Robeyns, K., Filinchuk, Y., Miele, P., & Demirci, U. B. (2016). In situ thermodiffraction to monitor synthesis and thermolysis of hydrazine borane-based materials. Journal of Alloys and Compounds, 659(25 February 2016), 210-216. https://doi.org/10.1016/j.jallcom.2015.11.052 (Original work published 2016)