A facile and low cost strategy for fabrication of a novel 3D honeycomb-like N-doped carbon nanosheet framework decorated with bismuth nanoparticles (3D Bi-NCNF) via co-pyrolysis of polyvinylpyrrolidone (PVP) and bismuth nitrate. As prepared 3D Bi-NCNF were characterized by a variety of techniques, i.e., field-emission scanning electron microscopy, transmission electron microscopy, X-ray diffraction, Raman spectroscopy, N-2 adsorption-desorption analysis, thermogravimetric analysis and X-ray photoelectron spectroscopy. Newly designed 3D Bi-NCNF nanocomposite possess porous network structures, high specific surface area and high nitrogen content dopant acts as an electrode-modification material for selective and sensitive electrochemical sensors for the assay of Cd2+ and Pb2+ by square wave anodic stripping voltammetry (SWASV). Under optimized conditions, Bi-NCNF modified glassy carbon electrodes (GCEs) exhibited excellent electroanalytical performance for the simultaneous detection of Cd2+ and Pb2+, a wide linear response ranges of 1-120 mu g L-1, with an ultralow detection limits of 0.02 and 0.03 mu g L-1 (S/N = 3) were observed, respectively. Moreover, excellent repeatability, reproducibility and stability, and reliable assays in tap water samples were realized with constructed sensors. Therefore, this study provides a novel strategy for fabrication of metal nanoparticles decorated nitrogen-doped carbon-based frameworks materials, which could be utility for constructing sensitive electrochemical sensors in the convenient and rapid detection of toxic metal ions. (c) 2018 Elsevier Ltd. All rights reserved.