The growing demand for fast, durable energy storage has intensified interest in pseudocapacitive electrodes that offer rapid redox kinetics and structural stability. In this work, a solvent-free thermal decomposition strategy is employed for the scalable synthesis of phase-pure monoclinic β-Ag2Mo2O7 silver dimolybdate nanostructures. Systematic optimization of thermal dwell time enables controlled phase formation and enhanced electrochemical performance. The optimized electrode exhibits a high specific capacitance of 937.5 Fg–1 at 1 Ag–1 and retains 92.8% of its initial capacitance after 10000 cycles. Kinetic analysis using Dunn’s method reveals a hybrid charge-storage mechanism arising from coupled diffusion-controlled redox reactions and surface-dominated pseudocapacitive processes associated with Ag0/Ag+ and Mo5+/Mo6+ couples. Symmetric and asymmetric coin-cell devices operate stably up to 1.5 V, delivering an energy density of 82 Wh kg–1 at 1172 W kg–1 with high Coulombic efficiency. Practical feasibility is demonstrated by powering an Arduino-based temperature sensor using series-connected asymmetric cells. These results demonstrate that thermally engineered β-Ag2Mo2O7 silver dimolybdate nanostructures are scalable and effective pseudocapacitive electrodes for high-performance supercapacitor applications.
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