Melt spinning and metal chloride vapor curing process on polymethylsilsesquioxane as SiOC fiber precursor

Abstract

Melt spinning process of polymethylsilsesquioxane (PMSQ) at 403-453 K was investigated as a SiAOAC fiber precursor in terms of averages and distributions of spun fiber diameters. Because of fusible character of PMSQ at low temperature, the spun fibers were exposed to vapors of various metal chlorides (SiCl 4 , Si(CH 3 )Cl 3 , TiCl 4 , and BCl 3 ) to promote the fiber curing. Cured fibers were investigated by FTIR and TG analyses.In a case of the fiber synthesized with SiCl 4 curing, tensile tests on the pyrolyzed fibers were performed. Exposure of the synthesized fiber at high temperature with a flame of an oxygen-gas burner was examined.

Processing of polysiloxane-derived porous ceramics: a review

“…SiC nanoparticles and Si O C fiber were produced from polymethylsilsesquioxane (PMSQ) precursors [119][120][121] by advanced cross-linking methods. For example, melt spinning on PMSQ at 130-180…”

“…• C followed by metal chloride (SiCl 4 , Si(CH 3 )Cl 3 , TiCl 4 or BCl 3 ) vapor curing yields Si O C C fibers [121]. This new technique can be applicable to the processing of porous polysiloxane-derived ceramics.…”

Synthesis of SiOC Base Fibers from Silicone Resin with Low Carbon Content and Control of Surface Functionality by Metal Chloride Treatment in Vapor

“…Detailed condition of the melt spinning was described in a previous article [4]. The averaged diameter of the spun fiber is 16.8 µm.…”

“…The averaged diameter of the spun fiber is 16.8 µm. The curing process of the spun fiber was performed by placing fiber bundles in a covered vat (800 cm 3 ) with 10ml of SiCl 4 or TiCl 4 in a Teflon dish for 1h. The curing procedure was performed in a glove bag with flowing nitrogen.…”

“…The obtained Si-O-C fiber was exposed to an air flow at high temperatures to estimate the oxidation resistance. The TiCl 4 cured fiber was placed in ambient for 1day to hydrolyze the incorporated TiCl 4 by humidity. The fiber was successively pyrolyzed in an air flow up to 873, 1073 or 1273K to obtain SiO 2 -TiO 2 fibers.…”