Novel Novolac-Phthalonitrile and Siloxane-Phthalonitrile Resins cured with low melting Novolac Oligomers for Flame Retardant Structural Thermosets

dc.contributor.authorHardrict, Shauntrece Nicoleen
dc.contributor.committeechairRiffle, Judy S.en
dc.contributor.committeememberEsker, Alan R.en
dc.contributor.committeememberMcGrath, James E.en
dc.contributor.departmentChemistryen
dc.date.accessioned2014-03-14T20:29:58Zen
dc.date.adate2004-01-15en
dc.date.available2014-03-14T20:29:58Zen
dc.date.issued2003-12-18en
dc.date.rdate2004-01-15en
dc.date.sdate2004-01-01en
dc.description.abstractThe chemical modification of low molecular weight novolac oligomers and siloxane/silane-containing monomers has led to novel phthalonitrile derivatives with low glass transition temperatures, ranging from -25 to 75 ºC. Multi-functional, low molecular weight phenol-formaldehyde novolac resins were blended with these novel phthalonitrile derivatives to achieve low viscosity resin blends. Moderate temperatures and rapid curing cycles were employed (200 ºC, 1 h and 225 ºC, 4h) to produce networks with high glass transition temperatures (> 250 ºC). A decrease in the sharp band at 2230 cm⁻¹, attributed to the nitrile functionality of the phthalonitrile resin, was monitored in FTIR studies and indicated the progress of the reactions. Ninety percent conversion was achieved within ~ 30 min. Thermal analysis of siloxane-phthalonitrile/novolac networks cured for 1h at 200 ºC and 4h at 225 ºC did not exhibit glass transition temperatures below 250 ºC. In dynamic TGA studies, 5% weight loss temperatures up to 418 ºC were observed, and the materials exhibited 50 to 56 % char at 800 ºC in nitrogen. Networks prepared from a resin blend containing 50 weight% of a phthalonitrile derivative of a 260 g mol⁻¹ novolac oligomer, 50 weight% of the 260 g mol⁻¹ novolac oligomer, and 1.5 mol % triphenylphosphine (based on novolac) (NOV/NOV/TPP) cured at 200 ºC for 1h, did not exhibit a Tg below 250 ºC via DSC. These networks exhibited a 5% weight loss temperature of 350 ºC, and 70 % char at 800 ºC in TGA studies under nitrogen. This degree of char formation makes these materials appealing for use in carbon-carbon composites. Post-curing these networks at 200 ºC for 1h, and then at 225 ºC for 4h, resulted in high thermo-oxidative stability, with a 5% weight loss observed at 447 ºC and 50 % char at 800 ºC. Blending tetramethyldisiloxane phthalonitrile monomers with 260 g mol⁻¹ novolac oligomers afforded prepolymer resins with low melt viscosities, 560 mPa s at 80 ºC. Such viscosities may allow these resins to be processed via vacuum assisted resin transfer molding (VARTM) at low temperatures and heated at elevated temperatures to produce flame resistant three-dimensional networks.en
dc.description.degreeMaster of Scienceen
dc.identifier.otheretd-01012004-153124en
dc.identifier.sourceurlhttp://scholar.lib.vt.edu/theses/available/etd-01012004-153124/en
dc.identifier.urihttp://hdl.handle.net/10919/9669en
dc.publisherVirginia Techen
dc.relation.haspartHardrict_MS_ETD.pdfen
dc.rightsIn Copyrighten
dc.rights.urihttp://rightsstatements.org/vocab/InC/1.0/en
dc.subjectnovolacen
dc.subjectphenolic networksen
dc.subjectphthalonitrileen
dc.subjectflame retardanceen
dc.subjectcomposite matrixen
dc.titleNovel Novolac-Phthalonitrile and Siloxane-Phthalonitrile Resins cured with low melting Novolac Oligomers for Flame Retardant Structural Thermosetsen
dc.typeThesisen
thesis.degree.disciplineChemistryen
thesis.degree.grantorVirginia Polytechnic Institute and State Universityen
thesis.degree.levelmastersen
thesis.degree.nameMaster of Scienceen

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