The layered composite gamma-TiPO4(H2PO4)pheno(0.48). 1.5H(2)O (phen = 1,10-phenanthroline) is able to exchange transition metal ions to give new intercalation compounds. The uptake of divalent cobalt, nickel and copper gives materials with interlayer distances unchanged in respect of the precursor, while with silver ions two new compounds are obtained with the interlayer spacing increased by about 3 Angstrom. The silver materials also exchange Co(II), Ni(II) and Cu(II) and bimetallic intercalation compounds are thus obtained, All the new phases submitted to TG-DTA experiments show specific behaviour depending on the nature and amount of metal ion present in the solids. Silver has a catalytic effect on phenanthroline elimination with temperature, since the process is the more pronounced the higher the silver content. During exchange with cobalt the silver materials undergo a redox process and metallic silver is present in the solids as prepared, Ag-0 is no longer observable when the two compounds are heated above 500 degrees C, a gain of weight of weight is detected in the TG curves, probably due to Ag2O formation, The redox process presumably also occurs in the Ni-Ag derivatives since, as for the Co-Ag analogues, the compounds are dark-grey coloured. After elimination of phen, the thermal treatment leads to the formation of AgTi2(PO4)3, transition metal-titanium double phosphates and pyrophosphates, processes always accompanied by exothermic effects in the DTA curves.