Synthesis and characterization of Th2N2(NH) isomorphous to Th2N3

Inorganic Chemistry
G W Chinthaka SilvaKen R Czerwinski

Abstract

Using a new, low-temperature, fluoride-based process, thorium nitride imide of the chemical formula Th(2)N(2)(NH) was synthesized from thorium dioxide via an ammonium thorium fluoride intermediate. The resulting product phase was characterized by powder X-ray diffraction (XRD) analysis and was found to be crystallographically similar to Th(2)N(3). Its unit cell was hexagonal with a space group of P3m1 and lattice parameters of a = b = 3.886(1) and c = 6.185(2) Å. The presence of -NH in the nitride phase was verified by Fourier transform infrared spectroscopy (FTIR). Total energy calculations performed using all-electron scalar relativistic density functional theory (DFT) showed that the hydrogen atom in the Th(2)N(2)(NH) prefers to bond with nitrogen atoms occupying 1a Wyckoff positions of the unit cell. Lattice fringe disruptions observed in nanoparticle areas of the nitride species by high-resolution transmission electron microscopic (HRTEM) images also displayed some evidence for the presence of -NH group. As ThO(2) was identified as an impurity, possible reaction mechanisms involving its formation are discussed.

References

Jun 15, 1992·Physical Review. B, Condensed Matter·J P Perdew, Y Wang
Jun 13, 2009·Inorganic Chemistry·G W Chinthaka SilvaKenneth R Czerwinski
Oct 23, 2009·Inorganic Chemistry·G W Chinthaka SilvaKenneth R Czerwinski

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