Optical and x-ray studies on the low-temperature phase transition of

Low-temperature phase transitions of with non-stoichiometric composition were investigated using a polarization microscope and x-ray diffractometer. Both apparatuses were equipped with a specially designed low-temperature cryostat which enabled us to measure the birefringence down to 4 K and x-ray reflections down to 20 K. Ferroelastic domain structure was observed to persist even at 4 K. Birefringence and pure shear show a peak at about 200 K and drop steeply at 110 K but do not vanish below 110 K. These facts indicate that the phase below 110 K is not re-entrant to the tetragonal 4 mm phase. The quite long relaxation process observed in birefringence and the appearance of a new reflection in the x-ray diffraction experiment indicate that the quasi-tetragonal region appears at 110 K and develops with long relaxation time.