Phase transitions and interface phenomena in the cryogenic temperature domain of a niobate nanostructured ceramic

Abstract

Powder neutron diffraction and dielectric spectroscopy were used to investigate both crystallographic and dielectric permittivity properties of a Sr₂KNb₅O₁₅ single phase ferroelectric oxide with nanosized grains ranging from 35 nm to 90 nm. Measurements were carried out in the temperature range from 10 K (cryogenic) to 550 K. All neutron diffraction data were indexed on the basis of a tetragonal double unit cell. From 10 K to room temperature the space group of the Sr₂KNb₅O₁₅ ferroelectric phase was considered to be P4bm. The refinement of the paraelectric phase (at 550 K) was determined in the centrosymmetric space group P4/mbm. Dielectric spectroscopy measurements were performed in a thermal cycle. A set of four phase transitions non-related to symmetry changing was detected from Rietveld analysis of neutron powder diffraction data. During a thermal cycle, in the cryogenic temperature domain, strong thermal hysteresis is developed. Both phase transition and thermal hysteresis were correlated. These phenomena are associated with Nb-cation atomic displacements in the NbO₆ octahedra along the c-axis direction and of the domain with different frequencies involving grains as well as an excess of interfaces ascribed to the grain boundary. The bulk/grain boundary interfaces in nanostructured ceramics are correlated with the thermal stability phenomenon.