13 samples of Li
2+xNH (where
x = 0, 0.167, 0.333, 0.500, 0.667, 0.833, 1.000, 1.167, 1.333, 1.500, 1.667, 1.833, 2.000) were synthesised by the solid state reaction of lithium imide with
Lithium nitride–hydride according to the following reaction:
Lithium imide for the reaction was synthesised as for the Li
1+xNH
2−x samples (
x = 1.000).
Lithium nitride–hydride was synthesised by the reaction of
lithium hydride (Sigma Aldrich, 95%) and
Lithium nitride (Sigma Aldrich, >99.5%): The reactants were hand-ground and then milled according to the procedure outlined above. 0.5 g of the resultant mixture was pelletised using a
hand press (Pike Technologies, 7 mm diameter), and placed into a nickel crucible in a quartz boiling tube, sealed with a Young's tap T-piece. The sample was heated to 500 °C at 2 °C min
−1 and dwelled for 12 hours.
Synthesis of the mixed Li
2+xNH samples from lithium imide and
Lithium nitride–hydride was the same as for the other samples, except that the milling procedure used a rotation rate of 400 rpm, and the furnace temperature set point was 540 °C.
Makepeace J.W., Brittain J.M., Sukhwani Manghnani A., Murray C.A., Wood T.J, & David W.I. (2021). Compositional flexibility in Li–N–H materials: implications for ammonia catalysis and hydrogen storage. Physical Chemistry Chemical Physics, 23(28), 15091-15100.