In this work, a class of flake-shaped magnetic NiCo2O4 materials is fabricated by a facile hydrothermal reaction followed by calcination treatment process. The prepared flake-like NiCo2O4 displays porous features that endows a large specific surface area (142.48 m 2 g −1 ) and a narrow pore size distribution (3.70 nm). Furthermore, the NiCo2O4 samples were used as high-performance heterogeneous catalysts in the activation of peroxymonosulphate (PMS) to produce active radicals SO4 −• and HO • . Then, the produced SO4 −• and HO • can further attack and degrade organic dyes. The catalytic results show that magnetic flake-like NiCo2O4 catalyst can completely degrade Rhodamine B (RhB) dye within 30 min with the assistance of PMS. In addition, the catalysts could be magnetic recovered, which displayed high catalytic activity and excellent cycling stability. It was believed that the specific porous features, including high specific surface area and tailoring pore size distributions, and surface defects can ensure the high activation of PMS for the catalytic oxidation of RhB. More importantly, the present synthetic method is facile, controllable and scalable, which highlights its potential in energystorage, environmental treatment, and biology-related fields. nanoparticles (NPs) exhibited high catalytic performance, the MFe 2 O 4 NPs with high surface area and the unique magnetic properties always lead to their aggregation, resulting in lower catalytic efficiency. 24 To solve these issues, some carbonaceous materials with high electrical conductivity have been widely Graphitic abstract: A kind of porous flake-like NiCo 2 O 4 was prepared via simple hydrothermal reaction followed by a calcination treatment process. The prepared NiCo 2 O 4 as catalyst to activation of PMS for furthermore degradation of RhB. Results demonstrated that the NiCo 2 O 4 /PMS heterogeneous catalysts display high catalytic activity and excellent cycling durability (see Figure), which is superior to most previously reported results.