obstacle to large-scale deployment. [11] From the equation, E = ½CV 2 , the energy density (E) of an electrochemical system is directly related to its specific capacitance (C) and the working voltage window (V) of SCs. [12,13] Therefore, designing an advanced SC with high capacitance as well as an enlarged voltage window is a potential strategy for the substantial improvement in its energy density property. Hybrid supercapacitors (HSCs) are a new class of SCs, which can be able to attain an improved energy density by sustaining their high-power density. These HSCs are typically composed of two different active materials, which exhibit battery-like (energy-source) and electric double-layered capacitor-like (power-source) materials, respectively. [14][15][16] Herein, battery-like materials typically exhibit high capacity performance by performing dominant reduction-oxidation (redox) reactions with electrolyte ions. [17,18] In contrast, capacitorlike materials store the charge through an adsorption/desorption process at an electrode/electrolyte interface. Therefore, developing novel battery-like materials with benefitted morphologies could greatly improve the energy density performance of SCs.Until now, distinct transition metal hydroxides/oxides, such as Ni 2 (OH) 2 CO 3 , CoMoO 4 , MnO 2 , NiAl LDHs, Co 3 O 4 , Ni(OH) 2 , etc., have been investigated as electrode materials for SCs due to their enriched redox chemistry, low cost, and multi-valence states of the involved elements. [19][20][21][22][23][24][25] However, metal oxides suffer from moderate electrochemical activity and low electrical conductivity. [26][27][28] Recently, transition metal sulfides have emerged as prominent electrode candidates for SCs owing to their two-order higher electrical conductivity than that of metal hydroxides/oxides. [29,30] Furthermore, replacing the oxygen atom in metal oxides with a low electronegativity of sulfur affords the structural deformation during intercalation/de-intercalation of foreign atoms. [31] Among the transition metal sulfides, especially nickel and cobalt sulfides, have attracted significant interest due to their several properties of high theoretical capacitance/capacity, enriched redox activity, high conductivity, multi-valence states, and natural abundance. So far, several researchers have studied the electrochemical performance of Transition bimetallic sulfides are exploited as high-capacity electrode materials in energy storage devices owing to their abundant electroactive sites and relatively high electrical conductivity compared with metal oxides. Here, an in situ conversion of metal ions into NiS 2 -CoMo 2 S 4 vertically aligned nanorod arrays on nickel foam (NS-CMS NRAs@NF) using a one-step hydrothermal technique to address the "dead-mass" limitation and multi-step preparation methods is reported. An in situ-converted NS-CMS NRAs obtained for 12 h of reaction time (NS-CMS NRAs-12 h@NF) delivers a superior areal capacity of 780 μAh cm −2 to the other NS-CMS electrodes synthesized for 6 h (543.1 μAh cm ...