In this study, for the first time, a new electrode of composite includes spherical nickel-selenide/ nickel sulfur carbon nanotubes (NiS 2 @NiSe 2 /CNT) was synthesized and used for high-performance supercapacitors in alkaline media. The crystalline nature, morphology and hollow interior of the microspheres were characterized by X-ray diffraction (XRD), scanning electron microscope (SEM), transmission electron microscopy (TEM) techniques, respectivly. Electrochemical evaluation of NiS 2 @NiSe 2 /CNT electrodes was performed by galvanostatic charge-discharge, cyclic voltammetry (CV) and electrochemical impedance spectroscopy (EIS). This composite shows a high specific capacitance (845 F g -1 at a current density of 1 A g -1 ), excellent good rate capability and stability (91% after 1000 cycles). In the second work, the CuCo 2 Se 4 yolk-shelled hollow microspheres (YS-CCSe) were santhesized with a facile self-templated method. The YS-CCSe properties were analysis by various technics such as energy dispersive x-ray (EDX), XRD, scanning electron microscopy (SEM) and TEM images. The YS-CCSe were examined as a high performance supercapacitors electrode material in alkaline media by various electrochemical methods. The results of three electrode testing show that, the YS-CCSe have a high specific capacitance (512 F g -1 at current density of 1 A g -1 ), excellent cycling stability (70.8 % retention at the current density of 16 A g -1 ), long cycling life (88.6 % capacitance retention after 1000 cycles) and good conductivity. Also, the YS-CCSe as an ASC device (two electrode testing) shows high energy density (9.45 Wh kg -1 ) at the power density of 170 W kg -1 . As a result, it is a promising candidate for supercomputers material in aqueous media.