Graphite oxide (GO)/polypyrrole (PPy) nanocomposites (GPYs) were synthesized using in situ polymerization. The effect of the feeding ratios of pyrrole and GO on the structure and electrochemical performances of GPYs was investigated. The structure was characterized via Fourier-transform infrared spectroscopy, scanning electron microscopy, transmission electron microscopy and X-ray diffraction. The electrochemical performance was characterized via cyclic voltammetry, galvanostatic charge-discharge and electrochemical impedance spectroscopy. The results indicate that the more pyrrole is added to GO (with GO concentrations of 20% and 50%), the more agglomeration of both PPy and GO layers occurs. This is detrimental to the capacitance utilization of PPy. When the feeding ratio of GO : pyrrole is 80 : 20, PPys with nanofibrils are dispersed homogenously in/on the exfoliated layer of GO and the conductivity is enhanced. The capacitance utilization of PPy in a composite with a GO concentration of 80% (383 F/g) is higher than that of pure PPy (201 F/g), which indicates the presence of a synergistic effect between GO and PPy. Graphite oxide (GO) is a lamellar material which can be exfoliated into the graphene oxide by applying mechanical energy in highly polar solvents, such as water [1]. Recently, GO has received rapidly growing interest because of its unique structure and properties. GO sheets possess a number of hydroxyl and epoxide functional groups anchored onto the surface sp 3 -hybridized carbon atoms. Moreover, they have considerable amounts of sp 2 -hybridized carbon atom-containing carboxyl and carbonyl groups at their sheet edges. Thus, they can be readily dispersed in water [2][3][4][5][6]. Meanwhile, these oxygen-containing groups impart the GO sheets strong reactivity with small polar molecules and polymers, which form GO composites.Micrometer-or nanometer-sized conducting polymers and their composites have attracted great attention primarily because of their potential applications in batteries, sensors, capacitors, and field-emission applications [7][8][9][10][11][12][13]. Among the conducting polymers and composites that have been studied, polypyrrole (PPy) and its composites are among the most extensively studied. This is because they possess high electrical conductivity, interesting redox properties and relatively high environmental stability. Furthermore, PPy is easy to prepare via chemical or electrochemical processes. The electronegative groups of GO, especially carboxyl and hydroxyl groups, can act as the "active sites" for the polymerization of pyrrole [14]. The morphology of the obtained polymers is an oriented nanostructure, such as nanofibers or nanowires. Nanostructured materials often possess a combination of physical and mechanical properties not present in conventional composites, such as electrical conductivity or electrochemical activity. Previous research on GO/PPy nanocomposites (GPYs) has been primarily focused on the improvement of the conductivity and thermal stability of . Little att...