Highly dispersed zirconium phosphate was prepared by reacting Cel/ZrO 2 (ZrO 2 =6.7 wt%; 0.56 mmol g −1 of zirconium atom per gram of the material) with phosphoric acid. High power decoupling magic angle spinning (HPDEC-MAS) 31 P NMR and X-ray photoelectron spectroscopy data indicated that HPO 2− 4 is the species present on the fiber surface. The X-ray diffraction patterns showed that zirconium hydrogen phosphate particles were amorphous and had an ion-exchange capacity, determined by ammonia gas adsorption, of 0.30 mmol g −1 . The ion-exchange capacities for Li + , Na + , and K + ions were determined from ion-exchange isotherms at 298 K and showed the following values (in mmol g −1 ): Li + =0.01, Na + =0.23, and K + =0.30. The higher affinity of the surface hydrogen phosphate particles for Na + and K + is due to its lamelar structure which permits easier diffusion of these two ions whose hydrated radii are smaller than that of Li + .