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Development of electrochemical supercapacitor electrode is the best way to improve the performance and conductivity of the alone materials and support energy storage devices. In this work, cyanate anions have used as building blocks to build series of nanolayered materials based on Ti/Ni layered double hydroxides (LDHs). The structural and morphological characteristics of the prepared Ti/Ni LDHs were examined using different techniques. The electrochemical supercapacitive behavior of the prepared LDHs was observed in the three-assembly electrochemical cell. These results showed that the optimized ratio of the nickel and titanium plays an important role to enhance the electrochemical performance of the LDHs. The optimized Ti/Ni LDHs, which has the highest content of titanium, showed the highest specific capacitance (675 F/g) value. In this trend, this LDH also retain a high percentage of the cyclic retention after long cyclic charging-discharging process. The enhanced performance could be due to the double layer structure, enough interplanar distance between the layer, and large number of exposed active site within the double layer structure of the LDHs. Finally, although there are no reports for the electrochemical supercapacitive performance of Ti/Ni LDHs in the literature, it is interesting to produce a new candidate for energy storage applications.