Zinc aluminum antimony layered double hydroxides (ZnAlSb-LDH) are synthesized by hydrothermal method and investigated as an innovative anodic materials for Zinc-nickel secondary batteries. The X-ray diffraction (XRD) and scanning electron microscopy (SEM) results demonstrate the as-harvested samples are well-crystallized and flake structure. The electrochemical performances of ZnAlSb-LDH with different Zn/Al/Sb molar ration are parsed by the galvanostatic charge-discharge measurements, cyclic voltammograms (CV), electrochemical impedance spectroscopy (EIS), and Tafel polarization curves. Besides, the antimony scattered in the LDH after the introduced antimony ion is reduced, leading to form a conductive network, which advances the conductivity of the zinc electrode. What's more, the high overpotential of hydrogen evolution of antimony could boost the corrosion resistance of the zinc negative electrode. Compared with ZnAl-LDH, ZnAlSb-LDH with different Zn/Al/Sb molar rations, particularly the sample of Zn/Al/Sb = 3:0.8:0.2 have higher discharge capacity and more stable cycling performances. After 800 cycles, ZnAlSb-LDH retains a specific capacity of 328 mAh g(-1) with the retention rate was 92.7%. (c) The Author(s) 2017. Published by ECS. This is an open access article distributed under the terms of the Creative Commons Attribution Non-Commercial No Derivatives 4.0 License (CC BY-NC-ND, http://creativecommons.org/licenses/by-nc-nd/4.0/), which permits non-commercial reuse, distribution, and reproduction in any medium, provided the original work is not changed in any way and is properly cited. For permission for commercial reuse, please email: [email protected]. All rights reserved.