Phosphorus containing methacrylate hybrids were synthesized from 2-(methacryloyloxy)ethyl phosphate (EGMP) and 3-[(methacryloyloxy)-propyl] trimethoxysilane (MEMO) via dual-cure process involving sol-gel reaction and addition polymerization. The kinetics of the reactions, was established using spectroscopic techniques. Photoacoustic Fourier transform infrared spectroscopy (PA-FTIR) and X-ray photoelectron spectroscopy (XPS) confirm the formation of Si-O-Si, P-O-P and Si-O-P linkages and simultaneous polymerization of methacrylate groups leading to a dense networked structure. The presence of silicate/phospho-silicate network in the hybrid enhances its thermal stability. Nano-indentation measurements on thin films show enhanced hardness and modulus with increasing silicate network. Topographic and conductivity images obtained using micro-thermal analysis (mu TA) reveal a dense, homogenous and defect-free thin film formed on metallic substrate with a T-g of 93 degrees C. (C) 2007 Elsevier Ltd. All rights reserved.