The Pyrolytic Decomposition of Owens-Illinois Resin GR650, an Organosilicon Compound
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THE PYROLYTIC DECOMPOSITION ORGANOSILICON COMPOUND
OF OWENS-ILLINOIS
RESIN
GR650, AN
B. G. BAGLEY,* P. K. GALLAGHER,** W. E. QUINN,* AND L. J. AMOS*** *Bell Communications Research, Inc., Murray Hill, NJ 07974; Work done while at Bell Laboratories; **AT&T Bell Laboratories, Murray Hill, NJ 07974; ***Department of Chemistry, Princeton University, Princeton, NJ 08540; Work done while at Bell Laboratories. ABSTRACT The pyrolytic conversion of an organosilsesquioxane (Owens-Illinois resin GR650) to Si0 2 is characterized by ir spectroscopy, thermogravimetry and evolved gas analysis (line-of-sight mass spectroscopy). Scanning calorimetry, ramping at IOC/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-CH 3 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-CH 3 groups such that after 30 minutes at 650'C the ir spectrum has evolved to that for Si0 2. 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 C 2H 5OH and H20, 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 CH- bound to the inside and outside of the polymer cage structures. The final major component detected was H2, over the temperature range -600 to -1 100°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. INTRODUCTION There is much current interest in lowering ceramic fabrication temperatures. One applicable technique for doing this is via organometallic precursors which are subsequently converted to the inorganic ceramic. Some precursors are particularly attractive because their viscosities can be easily adjusted by temperature (at and above the glass transition) and/or by the use of solvents, thus making for easy forming; and the conversion to the inorganic ceramic then can be done conveniently by pyrolysis. Emphasis, thus far, on the use of this process for bulk material preparation has been centered on the carbides and nitrides [1-6] which are generally difficult to fabricate. Organosilicon compounds are currently of interest to the electronics industry where, again because of the ease of forming, they are being used for thin film (e.g. as dopant sources) and coating (encapsulant) applications. These materials are part of a group sometimes called collectively "spin-on glasses." In these electronic applications the material is used in its organometallic state or its conversion to the inorganic is incidental to its intended use (e.g. as when used in dopant sources). Owens-Illinois, one of several
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