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Author Nava-Avendaño, Jessica ♦ Ayllón, José A. ♦ Frontera, Carlos ♦ Oró-Solé, Judith ♦ Estruga, Marc ♦ Molins, Elies ♦ Palacín, M. Rosa
Source United States Department of Energy Office of Scientific and Technical Information
Content type Text
Language English
Subject Keyword CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND SUPERFLUIDITY ♦ CONCENTRATION RATIO ♦ LATTICE PARAMETERS ♦ MICROWAVE RADIATION ♦ MONOCLINIC LATTICES ♦ MONOCRYSTALS ♦ ORTHORHOMBIC LATTICES ♦ OXYFLUORIDES ♦ SODIUM COMPOUNDS ♦ SYNTHESIS ♦ TEMPERATURE DEPENDENCE ♦ TITANIUM COMPOUNDS ♦ VALENCE ♦ VANADIUM COMPOUNDS ♦ VANADIUM IONS
Abstract Na{sub 5}Ti{sub 3}O{sub 3}F{sub 11} was prepared by the microwave assisted method, and presents a chiolite related structure with cell parameters a=10.5016(5), b=10.4025(5), and c=10.2911(5) Å and Cmca (no. 64) space group. From solvothermal synthesis at 100 °C the cryolite Na{sub 3−δ}VO{sub 1−δ}F{sub 5+δ} was prepared, which crystallizes in the monoclinic system with a=5.5403(2), b=5.6804(2), c=7.9523(2) Å, β=90.032(7)° cell parameters and P2{sub 1}/n (no. 14) space group. Under similar synthesis conditions but with higher HF concentration the chiolite-type phase Na{sub 5−δ}V{sub 3}F{sub 14} was achieved, which exhibits a=10.5482(2), b=10.4887(1) and c=10.3243(1) Å cell parameters and Cmc2{sub 1} (no. 36) space group. A single crystal also having the chiolite structure was synthesized at 200 °C which exhibits tetragonal symmetry (a=7.380(3) and c=10.381(11) Å and space group P4{sub 2}2{sub 1}2 (no. 94)). Bond valence sum indicates that it contains V{sup 4+} and therefore can be formulated as Na{sub 5}V{sub 3}O{sub 3}F{sub 11}. - Graphical abstract: Na{sub 5}M{sub 3}(O,F){sub 14} with M=Ti and V having chiolite structure and Na{sub 3−δ}VO{sub 1−δ}F{sub 5+δ} cryolite were prepared by means of microwave-assisted and solvothermal synthesis. - Highlights: • Na{sub 5}Ti{sub 3}O{sub 3}F{sub 11} chiolite was prepared by a microwave assisted method and characterized. • Na{sub 3−δ}VO{sub 1−δ}F{sub 5+δ} and Na{sub 5−δ}V{sub 3}F{sub 14} were prepared by solvothermal synthesis. • The compounds were structurally characterized by diffraction techniques. • O/F distribution was estimated by applying Pauling’s second rule.
ISSN 00224596
Educational Use Research
Learning Resource Type Article
Publisher Date 2015-03-15
Publisher Place United States
Journal Journal of Solid State Chemistry
Volume Number 226


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