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Synthesis and Characterization of Iron‐Doped ZrSiO 4 Solid Solutions from Gels
Author(s) -
Herrera G.,
Montoya N.,
Alarcón J.
Publication year - 2011
Publication title -
journal of the american ceramic society
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.9
H-Index - 196
eISSN - 1551-2916
pISSN - 0002-7820
DOI - 10.1111/j.1551-2916.2011.04808.x
Subject(s) - tetragonal crystal system , solid solution , amorphous solid , materials science , annealing (glass) , doping , zircon , solubility , analytical chemistry (journal) , crystallography , nuclear chemistry , crystal structure , chemistry , chromatography , metallurgy , paleontology , optoelectronics , biology
The mechanism of formation and the structural features of tetragonal Fe–ZrO 2 ‐amorphous silica composites and particulated Fe ‐doped ZrSiO 4 solid solutions were studied. A series of specimens with compositions Fe x –ZrSiO 4 , 0 ≤ x ≤ 0.10 were prepared by sol–gel techniques and thermally annealed over the range of temperature between 400°C and 1600°C. Results confirmed the formation of tetragonal Fe–ZrO 2 solid solution as first crystalline phase on the whole process leading to Fe ‐doped ZrSiO 4 solid solution. The annealing temperature for the preparation of Fe ‐containing ZrSiO 4 solid solutions was dependent on the nominal amount of iron. The Fe x –ZrSiO 4 solid solutions, with 0.02 < x < 0.08, were almost monophasic at 1100°C. The results of lattice parameter variation, energy‐dispersive X ‐ray ( EDX ) and diffuse reflectance ( DR ), showed that in the as‐prepared samples, Fe 3+ cations entered into the zircon structure being located mainly in tetrahedral sites replacing Si 4+ . The solubility limit of Fe 3+ in ZrSiO 4 at 1100°C was in the range 0.07–0.1 mol of iron per mol of zircon (approximately 3–4 wt% as Fe 2 O 3 ). This study opens new perspectives to the development of more ecological colored zircon‐based solid solution materials using mineralizer‐free synthetic procedures.