Synthesis of LiNH₂ + LiH by reactive milling of Li₃N

Minella, C.B., Rongeat, C., Domènech-Ferrer, R., Lindemann, I., Dunsch, L., Sorbie, N., Gregory, D.H. and Gutfleisch, O. (2011) Synthesis of LiNH₂ + LiH by reactive milling of Li₃N. Faraday Discussions, 151, pp. 253-262. (doi: 10.1039/C1FD00009H)

Abstract

The hydrogen sorption properties of Li₃N under reactive milling conditions have been investigated <i>in</i>- and <i>ex-situ</i> as a function of polytype structure (α vs. β), focusing on the influence of the micro-structure and/or the crystal structure upon hydrogen uptake. LiNH₂ and LiH were synthesized by reactive milling of Li₃N at 20 bar hydrogen pressure for 4 h. Reactive milling represents a quick and effective technique to produce LiNH₂ by hydrogenation of Li₃N at low hydrogen pressure and without any need for heating. As to our knowledge, we present a full hydrogenation of Li₃N under the aforementioned conditions for the first time. The (de)hydrogenation and rehydrogenation behaviour of milled amides was evaluated using a combination of powder X-ray diffraction, differential scanning calorimetry, thermogravimetry and <i>in situ</i> Raman spectroscopy. <i>In situ</i> Raman spectroscopy showed a shift in the lithium amide stretching modes upon hydrogenation supporting a non-stoichiometric storage mechanism consistent with the literature. The microstructure and polytype composition of the Li₃N dehydrogenated materials had no effect on the hydrogenation products and only minor effects on the hydrogen uptake profile during milling.

• Item Type: Articles
• Status: Published
• Refereed: Yes
• Glasgow Author(s) Enlighten ID: Sorbie, Miss Natalie and Gregory, Professor Duncan
• Authors: Minella, C.B., Rongeat, C., Domènech-Ferrer, R., Lindemann, I., Dunsch, L., Sorbie, N., Gregory, D.H., and Gutfleisch, O.
• Subjects: Q Science > QD Chemistry
• College/School: College of Science and Engineering > School of Chemistry
• Journal Name: Faraday Discussions
• ISSN: 1359-6640
• ISSN (Online): 1364-5498