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Revealing phase boundaries by weighted parametric structural refinement.

Parametric Rietveld refinement from powder diffraction data has been utilized in a variety of situations to understand structural phase transitions of materials in situ. However, when analysing data from lower-resolution two-dimensional detectors or from samples with overlapping Bragg peaks, such transitions become difficult to observe. In this study, a weighted parametric method is demonstrated whereby the scale factor is restrained via an inverse tan function, making the phase boundary composition a refinable parameter. This is demonstrated using compositionally graded samples within the lead-free piezoelectric (BiFeO3)x(Bi0.5K0.5TiO3)y(Bi0.5Na0.5TiO3)1-x-y and (Bi0.5Na0.5TiO3)x(BaTiO3)1-x systems. This has proven to be an effective method for diffraction experiments with relatively low resolution, weak peak splitting or compositionally complex multiphase samples.