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Novel porous Co 3 O 4 cubes are prepared by a simple hydrothermal method and a Co 3 O 4 -based chemiluminescence (CL) sensor is fabricated. The samples are characterized by scanning electron microscopy (SEM), X-ray diffraction (XRD), transmission electron microscopy (TEM), selected area electron diffraction (ED), N 2 adsorption, CO-and O 2 -temperature programmed desorption (CO-and O 2 -TPD), etc.The CL properties of the sensors are measured, and the catalytic oxidation properties of the samples are also investigated. The results show that the Co 3 O 4 cubes are assembled from subunits of nanoparticles, which results in porous structure. Compared with the bulk Co 3 O 4 -based sensor, the porous Co 3 O 4 one has a higher CL intensity and a higher catalytic oxidation activity, which has been ascribed to the porous structure and the high surface area. Most importantly, the Co 3 O 4 assemblies-based sensor can be used as an effective method for judging catalyst activity or selecting excellent catalysts

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