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Local Structure of Nanoscopic Magnesium Hydroxide Fluorides Studied by Natural Abundance 25 Mg Solid State NMR Spectroscopy
Author(s) -
Scholz Gudrun,
Heidemann Detlef,
Kemnitz Erhard
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.201200554
Subject(s) - magnesium , hydroxide , chemistry , fluorine , oxygen , nmr spectra database , inorganic chemistry , solid state nuclear magnetic resonance , spectroscopy , spectral line , crystallography , analytical chemistry (journal) , nuclear chemistry , nuclear magnetic resonance , organic chemistry , physics , astronomy , quantum mechanics
Along with X‐ray diffraction measurements, 25 Mg solid state NMR experiments were performed in natural abundance at 9.4 T on crystalline and mechanically milled samples of MgO, Mg(OH) 2 , MgF 2 , and magnesium hydroxide fluorides Mg(OH) x F 2– x prepared on mechanochemical and sol‐gel syntheses routes. In addition to single pulse and spin‐echo sequences, both static 1 H‐ 25 Mg CP and 19 F‐ 25 Mg CP measurements allowed the registration of 25 Mg spectra in attractive short measurement times. Although an assignment of different magnesium species in magnesium hydroxide fluorides is only hardly possible, position and line shapes of 25 Mg spectra of magnesium hydroxide fluorides reflect chemically reliable trends. All samples studied here show a sixfold fluorine, oxygen, or mixed fluorine / oxygen coordination of magnesium, also in highly disordered samples.