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The tetragonal rutile-type (FeSb)O 4  compound was synthesized reacting Fe 2 O 3  and Sb 2 O 3  in O 2 . Solid solubility in the pseudo-binary TiO 2 —(FeSb)O 4  (rutile — tripuhyite) system was investigated annealing powder mixtures characterized by different TiO 2 /(FeSb)O 4  molar ratios in an O 2  flux. Complete miscibility was found in the whole compositional range at 1373 K. The crystal structures of (FeSb)O 4  and selected terms of the (Ti 2x Fe 1–x Sb 1–x )O 4  solid solution (0 ≤  x  ≤ 1) were refined from X-ray powder diffraction data using the Rietveld method. Selective broadening of the X-ray lines was observed and analyzed by means of the Gaussian quadratic plot. Line broadening is probably related to a phase transformation taking place at low temperature, as suggested by the excess molar volume of the solid solution. As a result local chemical inhomogeneity and microstrain in the direction perpendicular to the 00 l  lattice planes for compositions 0.2 ≤  x  ≤ 0.6 are generated.

Solid state miscibility in the pseudo-binary TiO 2 —(FeSb)O 4 system at 1373 K