Transition metal sulfide (TMS) materials exhibit significant potential as high-performance supercapacitor electrodes for rapid charge-discharge cycles. Compared to their oxide counterparts, TMS materials generally show superior electrical conductivities, with the incorporation of sulfur atoms boosting their ionic conductivities.The fabrication and control of the structure and morphology of TMS electrodes are crucial in determining their physical and electrochemical properties for energy storage applications. Typically, the electrochemical efficiency correlates with the interactions between the electrode materials and electrolyte ions at the electrode's surface. Hence, electrodes with an optimally structured morphology can demonstrate enhanced electrochemical performance due to their increased surface area, reduced ion transport distances, and structural integrity. These characteristics contribute to higher specific capacitance, enhanced ion diffusion kinetics, and extended cyclability.Electrochemically active electrode materials are typically created with various micro/nanostructures using different synthetic methods, such as solvo-/hydrothermal synthesis, thermolysis, microwave irradiation, chemical vapor deposition, sputtering, and electrodeposition. These synthetic processes often require extended synthesis times (approximately 12–24 hours), electrochemical deposition and additional heat treatment to transform chemical reactants (above 400°C). Such methods impose significant high-temperature input, voltage damage, or mechanical strain on substrates, rendering them impractical for the industrialization of supercapacitors and likely degrading the practicalbility of diverse substrates. Consequently, identifying an effective method to fabricate electrochemically active electrode materials without thermal heat treatment is important. The low-temperature solution-based synthetic approach has been investigated as a viable alternative for depositing active materials on metal substrates.In this study, we introduce a novel and efficient method for synthesizing hierarchically structured TMS electrodes using a direct exposure approach with a highly reactive sulfide solution. The essence of this synthesis technique lies in the swift interaction between the ammonium sulfide solution and transition metal, wherein the ammonium ions catalyze the liberation of transition metal ions. Subsequently, these released ions react with sulfur ions in the solution, resulting in the formation of TMS materials. By modulating the synthesis conditions, it is possible to engineer TMS electrodes with diverse structures, leading to varying electrochemical properties. This approach offers a simple yet effective pathway to fabricate scalable, hierarchical TMS structures, highlighting the innovative capabilities of the solution-based sulfur activation method for high performance and fast energy storage applications.
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