Structural evolution of Ba8Ti3Nb4O24 from BaTiO3 using a series of Ba(Ti1−5xNb4x)O3 solid solutions

2014 
Abstract In this work, the structural evolution of hexagonal phase Ba 8 Ti 3 Nb 4 O 24 by adding Nb 2 O 5 to perovskite structure of BaTiO 3 was investigated. The compositions Ba(Ti 1-5x Nb 4x )O 3 ceramics, with 0.00025 ⩽  x  ⩽ 0.125 were prepared by the conventional solid state route in air atmosphere, the powders precursors, BaTiO 3 , BaCO 3 and Nb 2 O 5 , were mixed in stoichiometric proportions and ground in a ball mill using alumina balls and acetone. The mixed powders were calcined at temperatures up to 1500 °C. The phase transformation of Ba 8 Ti 3 Nb 4 O 24 from BaTiO 3 was studied by DRX, Raman spectroscopy, SEM, electrical measurements (relative permittivity and P – E hysteresis loops); Rietveld’s refinement was used to structurally characterize the samples. For the devices obtained capacitance was measured at 1 kHz; with these values we calculated the relative permittivity. The samples show typical P – E hysteresis loops at room temperature accompanied by saturation polarization (Ps) and remnant polarization (Pr). The DRX and Rietveld’s refinement results show x  ⩽ 0.01 has a ferroelectric behavior. When the doped level is increased x  ⩾ 0.02, a peak displacement is observed, this is due to the phase transformation of tetragonal to cubic into the unit cell. Finally, with x  = 0.125 the crystal structure transforms to the characteristic hexagonal phase Ba 8 Ti 3 Nb 4 O 24 which resonates at microwave frequencies.
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