Rh3+/H+ ion exchange in gamma-zirconium phosphate and in its intercalation compounds with organic diamine (2,2＇-bipyridyl, 1,10-phenanthroline, and 2,9-dimethyl-1,10-phenanthroline) has been investigated. Fully exchanged rhodium-zirconium phosphate has the composition gamma-Zr(PO4) (H0.86Rh0.38PO4). 2.3H(2)O and an interlayer distance of 15.2 Angstrom. The exchange of Rh3+ in intercalation compounds leads to phases in which the molar ratio Rh3+/diamine within the layers is about one. In some cases, a partial leaching of organic ligand during the Rh3+/H+ exchange has been observed. All the materials produced were characterized by their chemical compositions, X-ray powder diffraction patterns, and coupled TG/DTA analysis. In the presence of Rh3+ ions, the temperature of thermal deintercalation of diamine is lower than that observed in the pure intercalation compounds.