Micro/nanostructured nickel borate (Ni-3(BO3)(2)) has been widely explored as advanced materials for energy conversion and non linear optical applications, fabricating one-dimensional micro-/nanostructures of Ni-3(BO3)(2) has thus become increasingly necessary. In this contribution, pure phase of rod-like micron Ni-3(BO3)(2) particles were synthesized via a facile flux NaCl and surfactant poly(oxyethylene)9 nonylphenol ether (NP-9) assisted thermal conversion route at 750-800 degrees C for 2.0 h. The introduction of NaCl and NP-9 was favorable for the formation of the Ni-3(BO3)(2) particles with rod-like morphology and smaller size, respectively. When calcined at 750 degrees C in the presence of 8.0 mL of NP-9 and with the molar ratio of Ni:B:Na = 3:8:3, high aspect ratio rod-like micron Ni-3(BO3)(2) particles were obtained. The FT-IR and UV-vis properties of the as-synthesized Ni-3(BO3)(2) particles were also presented. The as-synthesized Ni-3(BO3)(2) rod-like particles further enlarged the metal borate family, with corresponding potential applications in the areas of nanocomposites, catalysis, energy conversion and storage, etc. (C), 2012 Elsevier B.V. All rights reserved.