The different morphologies of magnetic nickel cobaltate (NiCo2O4) electrocatalysts, consisting of nanoparticles (NiCo2O4-N), nanoplates (NiCo2O4-P) and microspheres (NiCo2O4-S) were fabricated. It was found that the electrocatalytic properties of the sensing materials were strongly dependent on morphology and specific surface area. The porous NiCo2O4 hexagonal nanoplates coupled with ILs as modified materials (ILs@NiCo2O4-P) for the simultaneous determination of thallium (TI+), lead (Pb2+) and copper (Cu2+), exhibited high sensitivity, long-time stability and good repeatability. The enhanced electrocatalytic activity was attributed to relatively large specific surface area, excellent electronic conductivity, and unique porous nanostructure. The analytical performance of the constructed electrode on detection of TI+, Pb2+ and Cu2+ was examined using differential pulse anodic stripping voltammetry (DPASV). Under optimal conditions, the electrode showed a good linear response to Tr+, Pb2+ and Cu2+ in the concentration range of 0.1-100.0, 0.1-100.0 and 0.05-100.0 mu g/L, respectively. The detection limits (S/N=3) were 0.046, 0.034 and 0.029 mu g/1. for TI+, Pb2+ and Cu2+, respectively. The fabricated sensor was successfully applied to detect trace TI+, Pb2+ and Cu2+ in various water and soil samples with satisfactory results. Hence, this work provided a promising material for electrochemical determination of cumulative toxic metals individually and simultaneously. (C) 2017 Elsevier B.V. All rights reserved.