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During catalytic ozonation, Al₂O₃-supported catalysts usually have stable structures but relatively low surface activity, while carbon-supported catalysts are opposite. To encourage their synergisms, we designed a Ni-induced C-Al₂O₃-framework (_NiCAF) and reinforced it with a Cu–Co bimetal to create an efficient catalyst (CuCo/_NiCAF) with a core–multishell structure. The partial graphitization of carbon adjacent to Ni crystals formed a strong out-shell on the catalyst surface. The rate constant for total organic carbon removal of CuCo/_NiCAF (0.172 ± 0.018 min^–1) was 67% and 310% higher than that of Al₂O₃-supported catalysts and Al₂O₃ alone, respectively. The metals on CuCo/_NiCAF contributed to surface-mediated reactions during catalytic ozonation, while the embedded carbon enhanced reactions within the solid–liquid boundary layer and in the bulk solution. Moreover, carbon embedment provided a 76 …