Nano-sized Ni(OH)(2) was synthesized by a co-precipitation method. Peaks between 500 and 750 cm(-1) in Fourier transform infrared spectroscopy (FTIR) confirmed the presence of metal hydroxide stretching. Thermo gravimetric analysis inferred that 69 wt% residue remained above 750 A degrees C. High-resolution transmission electron microscopy analysis of Ni(OH)(2) revealed its size ranged from 80 to 110 nm with smooth morphology. Scanning electron microscopy inferred that pure Ni(OH)(2) has nano rod-like morphology and higher weight percentage of aniline-intercalated Ni(OH)(2) has agglomerated structure. UV-Vis spectrum detected the presence of Ni2+ ions at 210 nm and the existence of amino group in the basal spacing of Ni(OH)(2) was not clearly appeared in the spectrum. Photoluminescence (PL) inferred that aniline-intercalated Ni(OH)(2) showed higher PL intensity than the pristine poly(vinyl alcohol) its and nano composite.