Publication date: 15th December 2025
High-entropy nanomaterials offer a powerful platform for tuning catalytic and electronic properties through multi-metal synergy, yet scalable routes to monodisperse, compositionally complex nanoparticles remain limited. We present a unified set of low-temperature, colloidal synthesis strategies that enable precise control over both high-entropy oxides and high-entropy sulfides, as well as their ternary and quaternary spinel analogues. For oxide systems, we leverage Lewis-acid-catalyzed esterification and the intrinsically low solubility product (Ksp) of metal oxides to achieve <4 nm, <15% dispersity high-entropy spinel and rock-salt nanoparticles, the smallest and most uniform colloidal HEOs reported, while ensuring synchronized monomer generation for multi-cation incorporation. For sulfides, we develop scalable “heat-up” and amino-acid–assisted routes to produce monodisperse NixCo3–xS4 and multi-metal thiospinels, including five-metal high-entropy nanodiscs and star-like nanocrystals with tunable anisotropy. We further demonstrate in-situ and ex-situ formation of hybrid nanocrystal–nanosheet heterostructures that substantially enhance catalytic activity. Across these systems, we demonstrate homogeneous incorporation of 5–10 cations, gram-scale yields, and strong alkaline OER activity, with overpotentials as low as 283 mV at 10 mA/cm² and excellent cycling stability. Together, these results establish a general and scalable colloidal framework for designing uniform, phase-pure, compositionally complex nanocrystals—advancing both the fundamental understanding and applied performance of high-entropy materials in energy-conversion technologies.
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