LAUSR

Transition metal chalcogenides (TMCs) exhibit unique electronic, optical, and magnetic properties, making them highly promising for applications in electrocatalysis, energy storage, and spintronics. Among various synthesis methods, solution‐phase approaches are particularly attractive due to their scalability, cost‐effectiveness, and compatibility with emerging AI‐guided strategies for materials design. This review summarizes recent progress in the solution‐phase synthesis and optimization of TMCs, covering methods such as hydrothermal/solvothermal synthesis, colloidal routes, template‐assisted strategies, AI‐driven solution processing, and energy‐assisted liquid exfoliation. These techniques provide versatile routes to precisely tune structural, morphological, and compositional features, as well as construct heterostructures with enhanced performance. Special emphasis is placed on how solution‐phase methods enable property control and facilitate integration into practical devices. Key challenges, such as achieving environmentally sustainable processes, scalable fabrication, and rational AI‐assisted design, are also discussed. Future directions include green synthesis, innovative heterostructures, and advanced computational frameworks to accelerate discovery and application. Overall, this review aims to provide a concise and up‐to‐date resource for researchers exploring solution‐processed TMCs and their multifunctional applications.