Sol-gel, homogeneous precipitation and hydrothermal synthesis are three different preparation techniques have been used as an attempt to synthesize nano-zirconium vanadate with properties suitable to be used as ion exchangers. The impact of the synthetic preparation variables such as the reactant concentrations, reaction temperature and reaction time on the ion exchange capacity of the produced ion exchanger has been considered for each preparation technique. One sample from each preparation technique having the largest ion exchange capacity has been selected to be physically and chemically characterized using various analytical techniques such as XRD, TGA, DSC, pH titration, FTIR and SEM in order to determine the properties of the ion exchanger produced from each technique. For all the studied ZrV samples it can be presumed that they have the ion exchange affinity sequences for alkali metal ions K > Na > Li, the order for the alkaline earth metals is Ba > Ca > Mg and their affinity for radioactive metals follow Cs > Sr. Moreover, the prepared materials are of high thermal and radiation stabilities. Also they have high chemical stabilities toward wide concentration ranges of acid, basic as well as polar solvents. It has been deduced from the X-ray analysis that ZrV produced from the sol-gel technique has an amorphous structural. While those produced from the homogeneous precipitation and hydrothermal synthesis techniques, in the nano-scale have semi-crystalline structural. Furthermore. SEM confirms that particle size of the all studied prepared ZrV samples have nano-diameters of range 50-60 nm. Specific surface area of the three different prepared ion exchangers are found to be equal to 187, 192 and 320 m(2)/g for sol-gel, homogeneous precipitation and hydrothermal, respectively. A tentative structural formula of Zr(OH)(2)(HVO(4))(2)center dot 2H(2)O has been proposed for all studied samples on the basis of on FTIR, DSC and TGA results. (C) 2010 Elsevier Ltd. All rights reserved.