Excessive-entropy perovskite fluoride (HEPF) has progressively attracted consideration within the discipline of electrocatalysis as a consequence of its distinctive properties. Though conventional co-precipitation strategies can effectively produce HEPF, the ensuing catalysts usually lack common morphology and have a tendency to combination extensively. Right here, nanocubic Okay(CuMgCoZnNi)F3 HEPF (HEPF-2) was efficiently ready on a gram-scale by a polyvinylpyrrolidone (PVP)-confined nucleation technique. Benefiting from its massive electrochemically energetic floor space and well-exposed energetic websites, the HEPF-2 demonstrates dramatically enhanced electrocatalytic exercise in electrocatalytic nitrate discount to ammonia, resulting in an improved ammonia yield charge (7.031 mg h−1 mgcat.−1), a excessive faradaic effectivity (92.8%), and glorious long-term stability, outperforming the irregular HEPF nanoparticles (HEPF-0) ready with out the help of PVP. Our work presents an environment friendly and facile methodology to synthesize perovskite fluorides with a well-defined construction, displaying nice promise within the discipline of high-performance electrocatalysis.