Morphological control of the nanostructured alpha-Ni(OH)(2) is achievable via self-assembly of sodium dodecyl sulfate (SIDS) as templates accompanied with microwave-assisted homogeneous alkalization process. The synthesized alpha-Ni(OH)(2) can be 2-D hexagonal nano-sheets, macroporous micro-spheres or irregular-shaped platelets, depending on the SDS concentration. Further, the interlayer spacing of the synthesized alpha-Ni(OH)(2) crystalline was determined to be 2.47 nm, indicating the intercalation of DS- anions between brucite layers. The results explain the morphological change of the synthesized alpha-Ni(OH)(2) with SDS concentration, which provides a way to morphological control of metal hydroxides. The corresponding electrochemical properties for the alpha-Ni(OH)(2) Synthesized with and without SDS are characterized as well, showing the advantages of the 2-D hexagonal nano-sheets. (C) 2009 Elsevier Inc. All rights reserved.