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Phase Formation, Crystal Chemistry, And Properties In The System Bi2O3–Fe2O3–Nb2O5

Michael W. Lufaso, Terrell A. Vanderah, Ileana M. Pazos, I. Levin, Robert S. Roth, Juan Claudio Nino, Virgil Provenzano, Peter Karl Schenck
Published 2006 · Chemistry
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Subsolidus phase relations have been determined for the Bi{sub 2}O{sub 3}-Fe{sub 2}O{sub 3}-Nb{sub 2}O{sub 5} system in air (900-1075 deg. C). Three new ternary phases were observed-Bi{sub 3}Fe{sub 0.5}Nb{sub 1.5}O{sub 9} with an Aurivillius-type structure, and two phases with approximate stoichiometries Bi{sub 17}Fe{sub 2}Nb{sub 31}O{sub 106} and Bi{sub 17}Fe{sub 3}Nb{sub 30}O{sub 105} that appear to be structurally related to Bi{sub 8}Nb{sub 18}O{sub 57}. The fourth ternary phase found in this system is pyrochlore (A{sub 2}B{sub 2}O{sub 6}O'), which forms an extensive solid solution region at Bi-deficient stoichiometries (relative to Bi{sub 2}FeNbO{sub 7}) suggesting that {approx}4-15% of the A-sites are occupied by Fe{sup 3+}. X-ray powder diffraction data confirmed that all Bi-Fe-Nb-O pyrochlores form with positional displacements, as found for analogous pyrochlores with Zn, Mn, or Co iad of Fe. A structural refinement of the pyrochlore 0.4400:0.2700:0.2900 Bi{sub 2}O{sub 3}:Fe{sub 2}O{sub 3}:Nb{sub 2}O{sub 5} using neutron powder diffraction data is reported with the A cations displaced (0.43A) to 96g sites and O' displaced (0.29A) to 32e sites (Bi{sub 1.721}Fe{sub 0.190}(Fe{sub 0.866}Nb{sub 1.134})O{sub 7}, Fd3-bar m (no. 227), a=10.508(1)A). This displacive model is somewhat different from that reported for Bi{sub 1.5}Zn{sub 0.92}Nb{sub 1.5}O{sub 6.92}, which exhibits twice the concentration of small B-typemore » cations on the A-sites as the Fe system. Bi-Fe-Nb-O pyrochlores exhibited overall paramagnetic behavior with large negative Curie-Weiss temperature intercepts, slight superparamagnetic effects, and depressed observed moments compared to high-spin, spin-only values. The single-phase pyrochlore with composition Bi{sub 1.657}Fe{sub 1.092}Nb{sub 1.150}O{sub 7} exhibited low-temperature dielectric relaxation similar to that observed for Bi{sub 1.5}Zn{sub 0.92}Nb{sub 1.5}O{sub 6.92}; at 1MHz and 200K the relative permittivity was 125, and above 350K conductive effects were observed.« less

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