Nano-sized lead has many versatile applications that could be useful in daily life. In the present work, we report a comprehensive study for preparation of nanosized lead oxide using the co-precipitation method and optimization of reaction parameters to obtain lead oxide (PbO) nanoparticles with homogeneously distributed size, shape, and structure. When aqueous solution of lead(II) acetate was reacted with sodium hydroxide at elevated temperatures, the alpha form of lead oxide nanoparticles, with spherical shape were produced. Decreasing the ratio of sodium hydroxide to lead(II) acetate concentration at moderate temperatures resulted in a gradual change in crystal structure from quasi-spherical α-PbO nanoparticles and two dimensional nanoflakes of beta PbO with a thickness below 100 nm was synthesized for the first time. The particles obtained in both α and β forms were characterized by X-ray powder diffraction (XRD), dynamic light scattering equipment (Zetasizer), transmission electron microscopy (TEM), scanning electron microscopy (SEM) and Fourier transform infrared spectroscopy (FTIR) techniques. Finally, thin layers of freeze-dried α-PbO and β-PbO particle powder on glass and filter paper were formed by the help of nail polisher and conductivity measurements were performed using four-point probes method. Produced layers β-PbO particles of the size below 100 nm showed higher conductivity on both supports as compared to the ones produced from spherical α-PbO nanoparticles. This altered the conductivity of the material in the semiconducting zone, which is probably due to a more effective electron transfer facilitated by 2D alignment of the molecules, could increase the potential use of this material in voltaic and catalysis.