Bi3Ni2Ta3O14 pyrochlores and related materials were prepared by solid state reaction at sintering temperatures ranging from 900°C to 1150°C. The BNT cubic pyrochlores could be represented by a general formula Bi3Ni2-xTa3O14-x and phase pure sample was obtained at temperature 1050°C with x = 0.6. This was confirmed by X-ray diffraction analysis and detailed lattice refinement. The single phase material crystallized in a cubic system, space group Fd3m with a = b = c = 10.5134 Å, α = β = γ = 90o, respectively. The sample was further characterized using a combination of techniques including Fourier-Transform infrared spectroscopy (FT-IR), differential thermal analysis (DTA), thermogravimetric analysis (TGA) and inductively coupled plasma – atomic emission spectrometry (ICP-AES). The material was thermally stable without any thermal events being observed. Electrical properties of the single phase material were studied by ac impedance spectroscopy starting from room temperature to 800 oC over a frequency range of 5 Hz to 13 MHz. The phase formation and solid solutions of cubic pyrochlores in the Bi2O3-NiO-Ta2O5 (BNT) ternary system were studied thoroughly via combination of characterization techniques.