MCM-41 materials were synthesized using alkyl(decosane, dodecyl)trimethyl ammonium bromide as structure directing surfactants. Xray diffraction (XRD) analysis and nitrogen adsorption measurements reveal that the pores are hexagonal with tunable textural properties through the choice of surfactant and experimental condition. Poly(diphenylamine), PDPA was entrapped into the pores of MCM-41 by initial sorption of diphenylamine (DPA, monomer) in a medium (napthalein sulfonic acid) that provides self-assembling of DPA inside the pores and subsequent oxidative of polymerization with peroxydisulphate. Clear presence of an additional peak (around 9-10degrees) in XRD pattern for the DPA loaded MCM-41 provides evidence for self-assembled structure. Upon polymerization the self-assembly of DPA molecules resulted tubular PDPA inside the pores of MCM-41. PDPA thus formed shows different electronic property than the PDPA prepared by conventional method. XRD and FTIR spectroscopic analysis of PDPA loaded MCM-41 clearly informs that PDPA are entrapped in channels of MCM-41. (C) 2005 Elsevier Ltd. All rights reserved.