The need for renewable energy sources has become an increasingly important issue in recent years. Thermoelectric materials are being investigated as one of many potential solutions to this problem because of their ability to convert waste heat into usable electrical energy. Unfortunately, current thermoelectric materials are inefficient and are made from toxic and expensive elements, so there is great effort devoted to developing new materials that are efficient, and made from less-toxic, and more abundant precursors. LaNiO₃ is one material of interest, and substitution of La for Bi has been shown to increase the thermoelectric performance. However, the cause of the increase is not understood. To learn why the performance is increasing, this study examines the effect of preparation and substitution of Bi followed by structural characterization to see if these aspects relate to the increase in thermoelectric performance.  . Bi_xLa_1-xNiO₃ (x = 0, 0.02, 0.05, 0.1, 0.2) was prepared by reverse co-precipitation followed by annealing at 600°C and 800°C. Powder X-ray diffraction (XRD) shows the material is pure-phase at lower concentrations of Bi; Bi cannot be incorporated into the unit cell past a concentration of 0.02 using these methods. Future work includes physical property measurements to determine their thermoelectric properties.