Effect of processing parameters on microstructural properties of lead magnesium niobates

The synchrotron powder X-ray diffraction (XRD) and subsequent detailed Rietveld analysis of lead magnesium niobate (PMN) samples were performed to study the microstructural properties of polar nanoregions (PNRs) of the R3m phase. PMN samples were synthesized under different sample processing conditions. The line profile broadening analysis of room-temperature synchrotron powder XRD patterns was performed using the multi-phase Rietveld refinement method for isotropic microstructural evaluation of different PMN samples. The two phases of perovskite PMN considered in the Rietveld refinement approach for satisfactorily fitting the XRD patterns are the paraelectric cubic phase (Pmm) and the local rhombohedral phase (R3m) which corresponds to the PNRs. It is observed that the contributions of the Gaussian component of size broadening of the polar rhombohedral phase (R3m) and the Lorentzian component of strain broadening of the paraelectric cubic phase (Pmm) are apposite for satisfactory Rietveld refinement of the synchrotron XRD data for all PMN samples. The volume-average crystallite size of PNRs (R3m phase) is almost invariant (approximately 12 nm) with increasing processing temperature while their weight percentage increases. The values of the apparent microstrain in the paraelectric cubic phase (Pmm) are larger for hot-pressed samples.