TY - JOUR
T1 - Analysis of precursor residues in lithium aluminosilicate gels using XPS and RGA
AU - Ho, Shu Fang
AU - Klein, L. C.
AU - Caracciolo, R.
N1 - Funding Information:
The financial support of the Fiber Optic Materials Research Program and NSF Materials Chemistry Program (DMR 88-08234) is gratefully acknowledged.
PY - 1990/4/1
Y1 - 1990/4/1
N2 - Lithium aluminosilicate gels of composition 15 mol% lithia-2 mol% alumina-83 mol% silica were prepared by adding nitrates to tetraethyl-orthosilicate (TEOS) and going through the sol-gel process. Samples were prepared in thin film and bulk form. Dried and outgassed samples were studied with X-ray photoelectron spectroscopy (XPS) d residual gas analysis (RGA). XPS spectra show similar species in both thin film and bulk samples, but different relative quantities of each species. Some oxidation of organic groups by nitrate is evident in bulk samples which were heated to 70°C during the drying process. In both thin film and bulk samples, the O 1s spectra indicate oxygens associated with a silicate network and higher binding energy species such as -{A figure is presented}-O-. The C 1s spectra of bulk gels heated to 140° and 350°C in vacuum show some organics are vaporized at low temperature, while the oxidized-organic residues are decomposed to CO2 at high temperature. These species are also observed with residual gas analysis at the corresponding temperatures.
AB - Lithium aluminosilicate gels of composition 15 mol% lithia-2 mol% alumina-83 mol% silica were prepared by adding nitrates to tetraethyl-orthosilicate (TEOS) and going through the sol-gel process. Samples were prepared in thin film and bulk form. Dried and outgassed samples were studied with X-ray photoelectron spectroscopy (XPS) d residual gas analysis (RGA). XPS spectra show similar species in both thin film and bulk samples, but different relative quantities of each species. Some oxidation of organic groups by nitrate is evident in bulk samples which were heated to 70°C during the drying process. In both thin film and bulk samples, the O 1s spectra indicate oxygens associated with a silicate network and higher binding energy species such as -{A figure is presented}-O-. The C 1s spectra of bulk gels heated to 140° and 350°C in vacuum show some organics are vaporized at low temperature, while the oxidized-organic residues are decomposed to CO2 at high temperature. These species are also observed with residual gas analysis at the corresponding temperatures.
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U2 - 10.1016/0022-3093(90)90212-5
DO - 10.1016/0022-3093(90)90212-5
M3 - Article
AN - SCOPUS:0025416326
SN - 0022-3093
VL - 120
SP - 267
EP - 274
JO - Journal of Non-Crystalline Solids
JF - Journal of Non-Crystalline Solids
IS - 1-3
ER -