AbstractTransition metal oxide / phenylphosphonate hybrids with M/P ratios ranging from 1 to 5, (M= Ti, Zr) and metal phosphonates (M/P = 0.5) have been prepared by a sol-gel process involving in a first step the non-hydrolytic condensation between metal alkoxide and phosphonic acid leading to M-O-P bonds, followed by the hydrolysis-condensation of the remaining M-OR groups. The composition, texture and structure of the materials were investigated using EDX, TGA, XRD, IR and 31P NMR.