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Study of Ammonolysis Reactions within SituX-Ray Diffraction: Detection and Crystal Structure of Li0.84W1.16N2

✍ Scribed by S. Kaskel; D. Hohlwein; J. Strähle

Book ID
102605348
Publisher
Elsevier Science
Year
1998
Tongue
English
Weight
424 KB
Volume
138
Category
Article
ISSN
0022-4596

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✦ Synopsis

The new ternary nitride Li 0.84 W 1.16 N 2 was found by an in situ X-ray diffraction study of the ammonolysis of a LiF-WO 3 mixture. The ammonolysis proceeds via Li 6 W 2 O 9 to LiWN 2 , which subsequently decomposes at 900°°C to form Li 0.84 W 1.16 N 2 . For a larger scale synthesis of Li 0.84 W 1.16 N 2 , the ammonolysis of a mixture of Li 2 CO 3 and WO 3 was performed at 900°°C. Li 0.84 W 1.16 N 2 crystallizes in the anti-TiP type structure with the space group P6 3 /mmc and a ‫؍‬ 2.8809(1) A s , c ‫؍‬ 10.3456(4) A s , and Z ‫؍‬ 2 as determined from simultaneous Rietveld refinement of X-ray and neutron powder diffraction data. The refinement converged with R(F 2 ) ‫؍‬ 7.0% for the X-ray data and 8.3% for the neutron data with a total reduced 2 ‫؍‬ 3.54. The structure consists of alternating layers of WN 6 trigonal prisms and MN 6 octahedra (M ‫؍‬ W, Li), with distances W-N ‫؍‬ 2.11 A s .

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