The nanostructured pyrophosphate Ni 0.25 Co 0.75 MnP 2 O 7 was prepared. The synthesis technique was based on the hydrothermal method at 150°C using poly-ethylene-glycol (PEG-10000) as surfactant with further calcination at 500°C. A structural analysis of Ni 0.25 Co 0.75 MnP 2 O 7 compound was carried out by applying X-ray diffraction (XRD) and using the Rietveld method. Morphological characterizations were performed using a scanning electron microscope (SEM) and transmission electron microscopy (TEM). A comparative study of the electrical conductivity of Mn 2 P 2 O 7 and Ni 0.25 Co 0.75 MnP 2 O 7 nanomaterials was carried out by impedance spectroscopy in the temperature range 500–680°C. The activation energies for MnP 2 O 7 and Ni 0.25 Co 0.75 MnP 2 O 7 were 2.00 and 0.88eV, respectively. Ni 0.25 Co 0.75 MnP 2 O 7 nanomaterial presents a good electric conductivity compared to Mn 2 P 2 O 7 , due to the substitution effect. The improvement of the electronic and ionic conductivity makes the Ni 0.25 Co 0.75 MnP 2 O 7 nanomaterial possible electrode materials for rechargeable batteries. The electrochemical behaviors of Ni 0.25 Co 0.75 MnP 2 O 7 were studied using cyclic voltammetry.