In this paper, we report on the facile synthesis method to obtain nickel titanate (NiTiO3) nanoparticles through pyrolysis of polymeric precursor. The pyrolysis behaviors of the polymer precursors prepared via the in situ polymerization of metal salts and acrylic acid were analyzed by simultaneous thermogravimetric and differential scanning calorimetry. The structural and morphological characteristics of the products were studied by powder X-ray diffraction and transmission electron microscope. The results reveal that ilmenite NiTiO3 nanoparticles with spherical-like shape are obtained through pyrolysis of Ni-Ti polyacrylate precursor at above 600 degrees C. The mean particle size of NiTiO3-600 degrees C and NiTiO3-800 degrees C is about 30 nm and 60 nm, respectively. Ultraviolet-visible (UV-vis) near infrared (NIR) reflectance spectra study show that the NiTiO3 nanoparticles have a high reflection peak of similar to 580 nm, which is associated with the deep and brilliant yellow color of this pigment. The average reflectance of NiTiO3-600 degrees C and NiTiO3-800 degrees C in NIR range are 62.1% and 58.8%, respectively. We have observed brilliant yellow color and high UV-vis-NIR reflectance of NiTiO3 nanoparticles. Moreover, these NiTiO3 nanoparticles have great potential in serving as cool pigment for building coating. (C) 2012 Elsevier B.V. All rights reserved.