Thermal stability on a mixture of triblock polymer (P123) and fluorocarbon surfactant (FC-4) in acidic media for synthesis of ordered mesoporous materials has been carefully investigated by NMR spectroscopy at various treated temperatures (RT-180 degrees C) and the templating mechanism of the mixture on high-temperature synthesis has been proposed. Accordingly, we have designed fluorocarbon-free templates for syntheses of ordered mesoporous silica materials at high temperatures. As expected, ordered mesoporous silica materials with high degree of silica condensation are synthesized at high temperatures from these designed templates. (C) 2007 Elsevier Inc. All rights reserved.