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The Pyrolytic Decomposition of Owens-Illinois Resin Gr650, an Organosilicon Compound

Published online by Cambridge University Press:  15 February 2011

B. G. Bagley
Affiliation:
Bell Communications Research, Inc., Murray Hill, NJ 07974;, Work done while at Bell Laboratories;
P. K. Gallagher
Affiliation:
AT&T Bell Laboratories, Murray Hill, NJ 07974;
W. E. Quinn
Affiliation:
Bell Communications Research, Inc., Murray Hill, NJ 07974;, Work done while at Bell Laboratories;
L. J. Amos
Affiliation:
Department of Chemistry, Princeton University, Princeton, NJ 08540;, Work done while at Bell Laboratories.
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Abstract

The pyrolytic conversion of an organosilsesquioxane (Owens-Illinois resin GR650) to SiO2 is characterized by ir spectroscopy, thermogravimetry and evolved gas analysis (line-of-sight mass spectroscopy). Scanning calorimetry, ramping at 10°C/min, on the as-received (room temperature annealed) resin indicates a glass transition temperature of 67°C which decreases to 58°C for an unrelaxed sample. The ir spectra have bands which can be assigned to Si-CH3 and Si-O-Si modes. For 30 minute isothermal anneals at temperatures above 420°C there is a continuous decrease in the bands associated with the Si-CH3 groups such that after 30 minutes at 650°C the ir spectrum has evolved to that for SiO2. Evolved gas analysis indicates that there are four major components evolving. Over the temperature range (ramping at 10°C/min) ∼180 to ∼500°C we observe C2H5OH and H2O, both of which are condensation reaction products from the curing reaction. Methane is a major evolving species over the temperature range ∼500 to ∼800°C and the thermal spectrum is double peaked which we attribute to CH3+ bound to the inside and outside of the polymer cage structures. The final major component detected was H2, over the temperature range ∼600 to ∼1100°C, which was attributed to pyrolysis of the organic components, both trapped and evolving. The features of the weight loss curve can be accounted for by the measured evolving species spectra.

Type
Research Article
Copyright
Copyright © Materials Research Society 1984

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References

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