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Synthesis and Characterization of Iron‐Doped ZrSiO4 Solid Solutions from Gels

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The mechanism of formation and the structural features of tetragonal Fe–ZrO2‐amorphous silica composites and particulated Fe‐doped ZrSiO4 solid solutions were studied. A series of specimens with compositions Fe x –ZrSiO4, 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–ZrO2 solid solution as first crystalline phase on the whole process leading to Fe‐doped ZrSiO4 solid solution. The annealing temperature for the preparation of Fe‐containing ZrSiO4 solid solutions was dependent on the nominal amount of iron. The Fe x –ZrSiO4 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, Fe3+ cations entered into the zircon structure being located mainly in tetrahedral sites replacing Si4+. The solubility limit of Fe3+ in ZrSiO4 at 1100°C was in the range 0.07–0.1 mol of iron per mol of zircon (approximately 3–4 wt% as Fe2O3). This study opens new perspectives to the development of more ecological colored zircon‐based solid solution materials using mineralizer‐free synthetic procedures.

Document Type: Research Article


Publication date: December 1, 2011


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