Al-substituted alpha-type nickel hydroxides (alpha-Ni(OH)(2)) containing different interlayer anions (NO3-, SO42-, Cl-, CO32-, OH-) are synthesized via a polyacrylamide (PAM) assisted two-step drying method. The effects of interlayer anions on the microstructure, morphology and electrochemical performance of AI-substituted alpha-Ni(OH)(2) are investigated by X-ray diffraction (XRD), infrared spectroscopy (IR), scanning electron microscope (SEM), cyclic voltammetry (CV), electrochemical impedance spectroscopy (EIS), and charge/discharge tests. The results demonstrate that the intercalated anions have a critical effect on the basal plane spacing, degree of crystallinity, and electrochemical properties of the end products. Especially, the intercalated anions have a marked impact on the activation process of the nickel electrodes. The Cl- intercalated alpha-Ni(OH)(2) sample exhibits better high-rate discharge ability and cycle stability than samples with other interlayer anions. This is attributed to the higher crystallinity, better exchange ability and smaller anion size of Cl-. The anion exchange ability and the size of anions also play an important role in the proton diffusion rate, which directly affects the electrochemical properties of alpha-Ni(OH)(2). The relationships between the specific capacity and basal spacing are also discussed in details for the five samples. (C) 2015 Elsevier B.V. All rights reserved.