Phthalonitrile polymers offer promise as matrix materials for advanced composite applications. The phthalonitrile monomer is readily converted to a highly crosslinked thermosetting polymer in the presence of thermally stable organic amine catalysts. Rheometric studies were conducted to elucidate the optimum amine concentration for composite formulations. High quality composite panels were processed in an autoclave using unsized IM7 carbon fibers. Mechanical properties of the phthalonitrile/carbon composite are either better than or comparable to the state‐of‐the‐art PMR‐15 composites. Dynamic mechanical analysis reveal that samples postcured at elevated temperatures (375°C) do not exhibit a glass transition temperature up to 450°C and also retain °90% of their initial modulus at 450°C. Flame resistance of phthalonitrile/carbon composites, evaluated by cone calorimetric studies, excels over that of other polymeric composites for marine applications. The composites also show low water uptake, <1% after exposure to water for 16 months.
Phthalonitrile monomers can be polymerized thermally in the presence of small amounts of curing agents into thermosetting polymers. The thermosets exhibit outstanding thermo-oxidative stability, display good mechanical properties, and offer promise as matrices for composite applications. The phthalonitrile cure reaction is typically accomplished with an aromatic diamine, 1,3-bis(3-aminophenoxy)benzene (m-APB), added in the range of 1.5-2% by weight of the monomer in the melt phase. This article addresses the cure reaction with a sulfone-containing diamine, bis[4-(4-aminophenoxy)phenyl] sulfone ( p-BAPS), which shows lower volatility as determined from thermogravimetric studies (TGA) compared to m-APB at the processing temperatures typically employed for phthalonitrile cures. Rheometric studies conducted to monitor the viscosity increase during a cure reaction suggest that the cure reaction with m-APB is faster compared to the reaction with p-BAPS. Even though differences are seen in the initial cure rates, the final cured products are similar in terms of the glass transition temperatures and thermal and oxidative stabilities.
This article compares the cure behavior and properties of phthalonitrile polymers derived from three different monomers, namely, 4,4Ј-bis(3,4-dicyanophenoxy)biphenyl, 2,2-bis[4-(3,4-dicyanophenoxy)phenyl]hexafluoropropane and 2,2-bis[4-(3,4-dicyanophenoxy)phenyl]propane. Rheometric measurements with monomer melt in the presence of an aromatic diamine curing agent reveal that the rate of the cure reaction differs for the three monomers. The rate is dependent on the concentration of the curing agent. The glass transition temperature advances with increasing extent of cure and disappears upon postcure at temperatures in excess of 350°C. Based on thermogravimetric analysis, the thermal stability of all three polymers are comparable, whereas the fluorine-containing resin shows the best oxidative stability at elevated temperatures. Microscale calorimetric studies on all three polymers reveal that the char yields are high and the total heat release upon exposure to 50 kW/m 2 flux for each polymer is low, compared to other thermosets. Flexural strength ranges between 80 -120 MPa. The water uptake under ambient conditions is less than 3% by weight after submersion in water for seven months.
Phthalonitrile polymers, under development at the Naval Research Laboratory, offer promise as high temperature, high performance composite matrix materials. A fully cured resin shows outstanding thermal stability with no evidence of a glass transition temperature or Tg up to 450°C, good mechanical properties, and is easily processed into void‐free components. Phthalonitrile/glass fabric composite panels have been successfully fabricated by conventional consolidation of prepregged glass and by a more recently developed simplified process, resin infusion molding. Both processes can be used to produce panels with comparable mechanical properties. More important, flammability performance of these composites, evaluated in terms of specific optical density, combustion gases, heat release, and ignitability, excels over other state‐of‐the‐art polymer/glass composites. This finding is significant given that overcoming flammability obstacles has been the main limiting factor for use of composites in marine applications.
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