Mechanochemistry has been recognized as an efficient and sustainable methodology to provide a unique driven force and reaction environments under ambient and neat conditions for the construction of functionalized materials possessing promising properties. Among them, highly porous conjugated scaffolds with attractive electronic conductivities and high surface areas are one of the representative categories exhibiting diverse task-specific applications, especially in electrochemical energy storage. In recent years, the mechanochemistry-driven procedures have been deployed to construct conjugated scaffolds with engineered structures and properties leveraging the tunability in chemical structures of building blocks and polymerization capability of diverse catalysts. Therefore, a thorough review of related works is required to gain an in-depth understanding of the mechanochemical synthesis procedure and property-performance relationship of the as-produced conjugated scaffolds. Herein, the mechanochemistry-driven construction of conjugated porous networks (CPNs), the carbon-based materials (e.g., graphite and graphyne), and carbon supported single atom catalysts (CS-SACs) are discussed and summarized. The electrochemical performance of the afforded conductive scaffolds as electrode materials in supercapacitors and alkali-ion batteries is elucidated. Finally, the challenges and potential opportunities related to the construction of conjugated scaffolds driven by mechanochemistry are also discussed and concluded.

High-entropy alloy nanoparticles (HEA-NPs) are highly underutilized in heterogeneous catalysis due to the absence of a reliable, sustainable, and facile synthetic method. Herein, we report a facile synthesis of HEA nanocatalysts realized via an ultrasound-driven wet chemistry method promoted by alcoholic ionic liquids (AILs). Owing to the intrinsic reducing ability of the hydroxyl group, AILs were synthesized and utilized as environmentally friendly alternatives to conventional reducing agents and volatile organic solvents in the synthetic process. Under high-intensity ultrasound irradiation, Au³⁺, Pd²⁺, Pt²⁺, Rh³⁺, and Ru³⁺ ions were co-reduced and transformed into single-phase HEA (AuPdPtRhRu) nanocrystals without calcination. Characterization results reveal that the as-synthesized nanocrystals are composed of elements of Au, Pd, Pt, Rh, and Ru as expected. Compared to the monometallic counterparts such as Pd-NPs, the carbon-supported HEA nanocatalysts show superior catalytic performance for selective hydrogenation of phenol to cyclohexanone in terms of yield and selectivity. Our synthetic strategy provides an improved and facile methodology for the sustainable synthesis of multicomponent alloys for catalysis and other applications.