A new preparation method of the fibrous organic-inorganic nanohybrids was established by the reaction of Zn(OH)(2) with various organic carboxylic acids. Interlayer spacings of the reaction products of Zn(OH)(2) with benzoic acid and p-phenyl azobenzoic acid were 1.46 and 2.04 nm, and these reaction products have layered structure. In IR spectra, new peaks of RCOO-Zn band appeared at around 1400 cm(-1) and 1550 cm(-1) indicating that hydroxyl groups reacted with organic carboxylic acids. SEM images of these reaction products showed fibrous morphology. The TEM image showed that the layer structure was constructed along the fiber direction.