Structural characterization of some sol-gel derived phosphosilicate glasses

A comparative study of three phosphosilicate gels of the 90SiO(2)-10P(2)O(5) composition obtained from tetraethoxysilane and three phosphorous precursors: triethylphosphate (TEP), triethylphosphite (TEPI) and H3PO4 is performed. Si-29 and P-31 Magic Angle Spining NMR, X-ray Photoelectron, X-ray Fluorescence and Raman spectroscopies as well as TG analysis are used in order to establish phosphorous precursors and annealing influence on composition and structure of the outcome materials. Unlike the three dimensional silicate network made of Si(OSi)(x)(OH)(4-x) species, unreacted TEP (100% Q(1) condensed phosphorous units) from TEP derived gel and a large amount of isolated phosphorous species (39.7% Q(0)) in the H3PO4 derived gel are identified. Annealing at 700 degrees C of the three gels give similar structure with the 90SiO(2)- 10P(2)O(5) glass, excepting the triethylphosphate derived glass that has a much lower P content. Thus, the H3PO4 derived glass at 700 and 1000 degrees C shows 1.89 and 1.94 times higher P2O5/SiO2 ratios than in the case of the TEP derived one. (C) 2015 Elsevier B.V. All rights reserved.