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Low‐Temperature Synthesis, Characterization, and Stability of Spinel‐Type Li 2 NiF 4 and Solid‐Solutions Li 2 Ni 1– x Co x F 4
Author(s) -
Kohl Julia,
Nakhal Suliman,
Ferro Noel,
Bottke Patrick,
Wilkening Martin,
Bredow Thomas,
Heitjans Paul,
Lerch Martin
Publication year - 2013
Publication title -
zeitschrift für anorganische und allgemeine chemie
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.354
H-Index - 66
eISSN - 1521-3749
pISSN - 0044-2313
DOI - 10.1002/zaac.201200455
Subject(s) - crystallite , spinel , lithium (medication) , cobalt , solid solution , characterization (materials science) , diffraction , x ray crystallography , materials science , ion , chemistry , crystallography , analytical chemistry (journal) , inorganic chemistry , nanotechnology , organic chemistry , physics , metallurgy , medicine , optics , endocrinology
A new synthesis route to Li 2 NiF 4 based on a fluorolytic process using Ni(acac) 2 or Ni(OAc) 2 · 4H 2 O as precursor is presented. Variation of the synthesis conditions allows crystallite size control of the obtained powders. 6 Li and 7 Li MAS NMR experiments were carried out to study local environments of the lithium ions. Several attempts were made to synthesize Li 2 CoF 4 , which are, unfortunately, hitherto not successful. Nevertheless, our studies clearly reveal that solid solutions Li 2 NiF 4 –Li 2 CoF 4 are stable up to ca. 30 % cobalt. High‐temperature X‐ray diffraction measurements also show no evidence for the existence of pure Li 2 CoF 4 . These findings are supported by quantum chemical calculations.