Systematic analysis of reaction parameters driving the hydrothermal growth of layered VS₂

Two-dimensional metallic vanadium disulfide (VS₂) has gained significant attention due to its excellent electrical and electrochemical properties, making it a promising candidate for energy storage and electronic applications. Despite the advantages of hydrothermal synthesis in producing VS₂ nanosheets, the underlying reaction pathways and critical synthesis parameters remain insufficiently understood. This study presents a systematic investigation of the key reaction variables influencing the hydrothermal growth of hierarchical VS₂ nanosheets on a three-dimensional substrate. By optimizing precursors' (NH₄VO₃ : TAA) molar ratios, reaction temperature, time, and ammonia concentration, we achieved precise control over the morphology and phase of VS₂. Our findings demonstrate that pure VS₂ nanosheets can be synthesized in just 5 hours, significantly reducing the conventional reaction time of 20 hours while maintaining phase purity and structural integrity. The parametric insights provided in this study establish a robust foundation for designing tunable VS₂ architectures with potential applications in catalysis, sensors, hydrogen evolution, and next-generation energy storage devices. © The Royal Society of Chemistry 2025.