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Materials (Basel). 2013 Nov 21;6(11):5410-5426. doi: 10.3390/ma6115410.

Rapid Microwave Synthesis, Characterization and Reactivity of Lithium Nitride Hydride, Li₄NH.

Author information

1
WestCHEM, School of Chemistry, University of Glasgow, Glasgow G12 8QQ, UK. nuria.tapia@glasgow.ac.uk.
2
WestCHEM, School of Chemistry, University of Glasgow, Glasgow G12 8QQ, UK. natsor@chem.gla.ac.uk.
3
WestCHEM, School of Chemistry, University of Glasgow, Glasgow G12 8QQ, UK. nicolas.vache@ensccf.fr.
4
Ecole Nationale Supérieure de Chimie de Clermont-Ferrand, Université Blaise Pascal, BP 187, Aubière Cedex 63174, France. nicolas.vache@ensccf.fr.
5
WestCHEM, School of Chemistry, University of Glasgow, Glasgow G12 8QQ, UK. tuan.hoang@glasgow.ac.uk.
6
WestCHEM, School of Chemistry, University of Glasgow, Glasgow G12 8QQ, UK. Duncan.Gregory@glasgow.ac.uk.

Abstract

Lithium nitride hydride, Li₄NH, was synthesised from lithium nitride and lithium hydride over minute timescales, using microwave synthesis methods in the solid state for the first time. The structure of the microwave-synthesised powders was confirmed by powder X-ray diffraction [tetragonal space group I4₁/a; a = 4.8864(1) Å, c = 9.9183(2) Å] and the nitride hydride reacts with moist air under ambient conditions to produce lithium hydroxide and subsequently lithium carbonate. Li₄NH undergoes no dehydrogenation or decomposition [under Ar(g)] below 773 K. A tetragonal-cubic phase transition, however, occurs for the compound at ca. 770 K. The new high temperature (HT) phase adopts an anti-fluorite structure (space group Fm 3̅ m; a = 4.9462(3) Å) with N3- and H- ions disordered on the 4a sites. Thermal treatment of Li₄NH under nitrogen yields a stoichiometric mixture of lithium nitride and lithium imide (Li₃N and Li₂NH respectively).

KEYWORDS:

diffraction; hydride; hydrogen storage; microwaves; nitride; reactivity; structure; synthesis; thermal analysis

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