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Report describes preliminary attempts at dielectric monitoring of curing of graphite/epoxy and carbon/phenolic composites. Objective is to develop dielectric monitoring for optimizing curing process and reduce incidence of failures of produced composite structures.
The cure processes of TGDDM-based epoxy thermosets and polysulfone thermoplastic resins were monitored by means of computer-controlled dynamic dielectric measurements made at frequencies 5 Hz to 5 million Hz. The values of capacitance and conductance were recorded, and the data were used to calculate the complex permittivity, an intensive property which is characteristic of the material's state of cure and independent of the amount of material measured. The frequency dependence of the complex permittivity value was used to determine the conductivity and mean relaxation time. The conductivity which is also an intensive variable and is independent of sample size, was correlated with the viscosity in both the epoxy and polysulfone systems.
An epoxy and carbon fiber composite has been used to produce a light-weight rocket case for the Space Shuttle. A kinetic model is developed which can predict the extent of epoxy conversion during the winding and curing of the case. The model accounts for both chemical and physical kinetics. In the model, chemical kinetics occur exclusively up to the time the transition temperature equals the reaction temperature. At this point the resin begins to solidify and the rate of this process limits the rate of epoxy conversion. A comparison of predicted and actual epoxy conversion is presented for isothermal and temperature programmed cure schedules.
Kinetic model describes major features of curing process. Report describes investigation of curing of epoxy resin used in carbon-fiber/epoxy version of cases of Space Shuttle booster rockets.
The rate of cure and viscosity were measured for Hercules HBRF-55 resin. The rate of cure was measured by differential scanning calorimetry, while the viscosity was measured by a parallel disk and plate type apparatus. The data were fitted to analytic expressions to make them suitable for use in numerical calculations.
Dynamic dielectric analysis (DDA) is an effective in situ NDE method that can monitor the reaction status in thermosets and the phase changes in thermoplastics, including slow reactions occuring late in the cure cycle and recrystallization during annealing. The effects of moisture and resin history on reaction rate can also be determined, as can ionic and dipolar contributions. The ionic mobility parameter is noted to be an excellent monitor of viscosity above the glass transition temperature. The ability of DDA to monitor cure rate variations in a thick section during autoclaving has been demonstrated.
An analytical technique for controlling the curing process of fiber-reinforced composite materials that are formed using thermosetting resins. The technique is the percent gel method and involves development of a time-to-gel equation as s function of temperature. From this equation a rate-of-gel equation is then determined, and a percent gel is calculated which is the product of the rate-of-gel times time. Percent gel accounting is used to control the proper pressure application point in an autoclave cure process to achieve desired properties in a production composite part.
The development of infrared-transmitting optical fibers as sensors for monitoring the cure of advanced composite materials is reported. Fourier transform infrared spectra are presented which were remotely sensed during the cure of a high performance polyimide resin and a graphite/polyimide matrix prepreg using an 0.1 mm O.D. x 3 m chalcogenide optical fiber. A discussion of the fiber and sensor element, absorption mechanism and potential applications is presented.
Infrared-sensing optical fiber system developed to monitor principal infrared absorption bands resulting from vibrations of atoms and molecules as chemical bonds form when resin cured. System monitors resin chemistry more directly. Used to obtain Fourier transform infrared (FTIR) spectrum from graphite fiber/polyimide matrix resin prepreg. Embedded fiber optic FTIR sensor used to indicate state of cure of thermosetting composite material. Developed primarily to improve quality of advanced composites, many additional potential applications exist because principal of operation applicable to all organic materials and most inorganic gases. Includes monitoring integrities of composite materials in service, remote sensing of hazardous materials, and examination of processes in industrial reactors and furnaces.
Real-time in situ monitoring of the chemical states of epoxy resins was investigated during cure in an autoclave using infrared evanescent spectroscopy. Fiber evanescent sensors were developed which may be sandwiched between the plies of the prepreg sample. A short length of sapphire fiber was used as the sensor cell portion of the fiber probe. Heavy metal fluoride glass optical fiber cables were designed for connecting the FTIR spectrometer to the sensor fiber within the autoclave. The sapphire fibers have outstanding mechanical thermal properties which should permit their use as an embedded link in all thermoset composites. The system is capable of operation at a temperature of 250 C for periods up to 8 hours without major changes to the fiber transmission. A discussion of the selection of suitable sensor fibers, the construction of a fiber-optic interface, and the interpretation of in situ infrared spectra of the curing process is presented.
In an attempt to improve the thermal-oxidative stability (TOS) of PMR-type polymers, the use of 1,4-phenylenebis (phenylmaleic anhydride) PPMA, was evaluated. Two series of nadic end-capped addition curing polyimides were prepared by imidizing PPMA with either 4,4'-methylene dianiline or p-phenylenediamine. The first resulted in improved solubility and increased resin flow while the latter yielded a compression molded neat resin sample with a T(sub g) of 408 C, close to 70 C higher than PME-15. The performance of these materials in long term weight loss studies was below that of PMR-15, independent of post-cure conditions. These results can be rationalized in terms of the thermal lability of the pendant phenyl groups and the incomplete imidization of the sterically congested PPMA. The preparation of model compounds as well as future research directions are discussed.
Several models simulating plain weave, graphite/epoxy woven composites are presented, along with the effects that the simultaneous application of pressure and thermal loads have on their surfaces. The surface effects created by moisture absorption are also examined. The computational simulation consisted of using a two-dimensional finite element model for the composite. The properties of the finite element (FE) model are calculated by using the in-house composite mechanics computer code ICAN (Integrated Composite ANalyzer). MSC/NASTRAN is used for the FE analysis which yields the composite's top surface normalized displacements. These results demonstrate the importance of parameters such as the cure temperature (T sub o) and the resin content in the curing process of polymer-matrix composites. The modification of these parameters will help tailor the composite system to the desired requirements and applications.
Fourier-transform infrared spectroscopy applied in interior of specimen of material by bringing infrared light through specimen in optical fiber. Light interacts with material via evanescent-wave effect. Spectra obtained in this way at various times during curing process also combined with data from ultrasonic, thermographic, and dielectric-impedance monitoring, and other measurement techniques to obtain more complete characterization of progress of curing process.
In developed series of high-flow PMR-type polyimide resins, 2, 2'-bis(trifluoromethyl)-4, 4'-diaminobiphenyl (BTDB) substituted for 1, 4-pheylenediamine in PMR-II formulation. Polyimides designated either as PMR-12F when nadic ester (NE) end caps used, or as V-CAP-12F when p-aminostyrene end caps used. High-molecular-weight, addition-curing polyimides based on BTBD and HFDE highly processable high-temperature matrix resins used to make composite materials with excellent retention of properties during long-term exposure to air at 650 degrees F or higher temperature. Furthermore, 12F addition-curing polyimides useful for electronic applications; fluorinated rigid-rod polyimides known to exhibit low thermal expansion coefficients as well as low absorption of moisture.
Damped composite laminates were fabricated by co-curing viscoelastic damping film with graphite/epoxy prepreg plies. The dynamic response of the damped plates was measured using an impulse response technique and compared with the response of similar undamped laminates. Modal damping was computed from the frequency response data. Micrographs of the damped laminates showed that the damping layers retained their integrity during the fabrication process. The layers significantly increased the damping in the composite laminates. The use of the constrained viscoelastic film as an integral part of composite structures appears to be a feasible approach to passive vibration control. Composite plates manufactured with co-cured damping layers may have commercial applications in cases where light weight, strength, and vibration and noise reduction are important considerations.
Several models simulating plain weave, graphite/epoxy woven composites are presented, along with the effects that the simultaneous application of pressure and thermal loads have on their surfaces. The surface effects created by moisture absorption are also examined. The computational simulation consisted of using a two-dimensional finite element model for the composite. The properties of the finite element (FE) model are calculated by using the in-house composite mechanics computer code ICAN (Integrated Composite ANalyzer). MSC/NASTRAN is used for the FE analysis which yields the composite's top surface normalized displacements. These results demonstrate the importance of parameters such as the cure temperature (T sub o) and the resin content in the curing process of polymer-matrix composites. The modification of these parameters will help tailor the composite system to the desired requirements and applications.
Anabolic agents like parathyroid hormone and postagladin E-like substances were studied in dogs and rats to determine their effectiveness in the prevention and cure of bone loss due to immobilization. It was determined that postagladin E2 administration prevented immobilization while at the same time it added extra bone in a dose responsive manner. Although bone mass returns, poor trabecular architecture remains after normal ambulation recovery from immobilization. Disuse related bone loss and poor trabecular architecture were cured by post-immobilization postagladin E2 treatment.
With the expanding use of polymeric materials as composite matrices, adhesives, coatings and films, the need to develop low cost, automated fabrication processes to produce consistently high quality parts is critical. Essential to the development of reliable, automated, intelligent processing is the ability to continuously monitor the changing state of the polymeric resin in-situ in the fabrication tool. This final report discusses work done on developing dielectric sensing to monitor polymeric material cure and which provides a fundamental understanding of the underlying science for the use of frequency dependent dielectri sensors to monitor the cure process.