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The polyhedron-structured NiSe 2 @MoSe 2 (NMS) were magnificently produced through hydrothermal method, which makes the active electrode very effective in accessing the redox active sites in the charge/discharge process in supercapacitor applications. Systematic studies of the structural and morphological features of the unique polyhedron NMS were performed. Laser Raman spectra reported the vibrational and rotational modes of NMS. NMS exhibited a maximum 1000 F g -1 (138.8 mA h g -1 ) specific capacitance at 1 A g -1 and attained a capacity retention of 77.67% for 5000 stable cycles at 10 A g -1 using 1 M KOH as an electrolyte. The well assembled asymmetric supercapacitor NMS hydrolyzed for 18 h//AC demonstrated an outstanding electrochemical performance with an improved 305 F g -1 specific capacitance attained at 1 A g -1 with a good cycle life of 87.35% and a capacity retention of over 5000 cycles. Herein, the combined contribution of both the Ni and Mo ions offers a richer redox chemistry, which is beneficial to a higher electrochemical activity. The experimental results indicate that the NMS electrode could be used as a high-performance electrode., Competing Interests: There are no conflicts to declare., (This journal is © The Royal Society of Chemistry.)

So far, numerous metal oxides and metal hydroxides have been reported as an electrode material, a critical component in supercapacitors that determines the operation window of the capacitor. Among them, nickel and cobalt-based materials are studied extensively due to their high capacitance nature. However, the pure phase of hydroxides does not show a significant effect on cycle life. The observed XRD results revealed the phase structures of the obtained Ni(OH) 2 and Co-Ni(OH) 2 hydroxides. The congruency of the peak positions of Ni(OH) 2 and Co-Ni(OH) 2 is attributed to the homogeneity of the physical and chemical properties of the as-prepared products. The obtained results from XPS analysis indicated the presence of Co and the chemical states of the as-prepared composite active electrode materials. The SEM analysis revealed that the sample had the configuration of agglomerated particle nature. Moreover, the morphology and structure of the hydroxide materials impacted their charge storage properties. Thus, in this study, Ni(OH) 2 and Co-Ni(OH) 2 composite materials were produced via a hydrothermal method to obtain controllable morphology. The electrochemical properties were studied. It was observed that both the samples experienced a pseudocapacitive behavior, which was confirmed from the CV curves. For the electrode materials Ni(OH) 2 and Co-Ni(OH) 2 , the specific capacitance ( C s ) of about 1038 F g -1 and 1366 F g -1 , respectively, were observed at the current density of 1.5 A g -1 . The Ni-Co(OH) 2 composite showed high capacitance when compared with Ni(OH) 2 . The cycle index was determined for the electrode materials and it indicated excellent stability. The stability of the cell was investigated up to 2000 cycles, and the cell showed excellent retention of 96.26%., Competing Interests: There are no conflicts to declare., (This journal is © The Royal Society of Chemistry.)