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Capillary rheometry is effectively used with thermosets. Most important is providing a uniform temperature in the barrel. This was successfully accomplished by using a circulating hot oil system. Standard capillary rheometry methods provide the dependence of thermoset apparent viscosity on shear rate, temperature and time. Such information is very useful in evaluating resin processability and in setting preliminary fabrication conditions.
The chemorheological behavior of the PRM-15 molding compounds were characterized, the range of suitable processing parameters for injection molding in a reciprocating screw injection molding machine was determined, and the effects of the injection molding processing parameters on the mechanical properties of molded PMR-15 parts were studied. The apparatus and procedures for measuring viscosity and for determining the physical response of the material during heating are described. Results show that capillary rheometry can be effectively used with thermosets if the equipment is designed to overcome some of the inherent problems of these materials. A uniform temperature was provided in the barrel by using a circulating hot oil system. Standard capillary rheometry methods can provide the dependence of thermoset apparent viscosity on shear rate, temperature, and time. Process conditions resulting in complete imidization should be carefully defined. Specification of controlled oven temperature is inadequate and can result in incomplete imidization. For completely imidized PMR-15 heat at 15 C/min melt flow without gas evolution occurs in the temperature range of 325 C to 400 C.
A method has been found for enhancing the melt flow of thermoplastic polyimides during processing. A high molecular weight 422 copoly(amic acid) or copolyimide was fused with approximately 0.05 to 5 pct by weight of a low molecular weight amic acid or imide additive, and this melt was studied by capillary rheometry. Excellent flow and improved composite properties on graphite resulted from the addition of a PMDA-aniline additive to LARC-TPI. Solution viscosity studies imply that amic acid additives temporarily lower molecular weight and, hence, enlarge the processing window. Thus, compositions containing the additive have a lower melt viscosity for a longer time than those unmodified.
A process for preparing polyimides having enhanced melt flow properties is described. The process consists of heating a mixture of a high molecular weight poly-(amic acid) or polyimide with a low molecular weight amic acid or imide additive in the range of 0.05 to 15 percent by weight of additive. The polyimide powders so obtained show improved processability, as evidenced by lower melt viscosity by capillary rheometry. Likewise, films prepared from mixtures of polymers with additives show improved processability with earlier onset of stretching by TMA.
A process for preparing polyimides having enhanced melt flow properties is described. The process consists of heating a mixture of a high molecular weight poly-(amic acid) or polyimide with a low molecular weight amic acid or imide additive in the range of 0.05 to 15 percent by weight of the additive. The polyimide powders so obtained show improved processability, as evidenced by lower melt viscosity by capillary rheometry. Likewise, films prepared from mixtures of polymers with additives show improved processability with earlier onset of stretching by TMA.
Pyrolytic conversion of polymeric precursors to ceramics is accompanied by loss of volatiles and large volume changes. Infiltration of a low viscosity polymer into a fiber preform will fill small spaces within fiber tows by capillary forces, but create large matrix cracks within large, intertow areas. One approach to minimizing shrinkage and reducing the number of required infiltration cycles is to use particulate fillers. In this study, Starfire allylhydridopolycarbosilane (AHPCS) was blended with a silicon carbide powder, with and without dispersant, using shear mixing. The polymer and polymer/particle interactions were characterized using nuclear magnetic resonance, differential scanning calorimetry, thermogravimetric analysis and rheometry. Polymer/particulate slurries and suspensions were used to infiltrate a figidized preform of an eight ply five harness satin CG Nicalon fiber having a dual layer BN/SiC interface coating, and the resulting composites characterized by optical and scanning electron microscopy.
The capability to manufacture large structures leads to weight savings and reduced risk relative to joining smaller components. However, manufacture of increasingly large composite components is pushing the out-time limits of epoxy/ carbon fiber prepreg. IM7/977-3 is an autoclave processable prepreg material, commonly used in aerospace structures. The out-time limit is reported as 30 days by the manufacturer. The purpose of this work was to evaluate the material processability and composite properties of 977-3 resin and IM7/977-3 prepreg that had been aged at room temperature for up to 60 days. The effects of room temperature aging on the thermal and visco-elastic properties of the materials were investigated. Neat resin was evaluated by differential scanning calorimetry to characterize thermal properties and change in activation energy of cure. Neat resin was also evaluated by rheometry to characterize its processability in composite fabrication. IM7/977-3 prepreg was evaluated by dynamic mechanical analysis to characterize the curing behavior. Prepreg tack was also evaluated over 60 days. The overall test results suggested that IM7/977-3 was a robust material that offered quality laminates throughout this aging process when processed by autoclave.