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NASA NTRS1984

Chemoviscosity modeling for thermosetting resins - I

A new analytical model for chemoviscosity variation during cure of thermosetting resins was developed. This model is derived by modifying the widely used WLF (Williams-Landel-Ferry) Theory in polymer rheology. Major assumptions involved are that the rate of reaction is diffusion controlled and is linearly inversely proportional to the viscosity of the medium over the entire cure cycle. The resultant first order nonlinear differential equation is solved numerically, and the model predictions compare favorably with experimental data of EPON 828/Agent U obtained on a Rheometrics System 4 Rheometer. The model describes chemoviscosity up to a range of six orders of magnitude under isothermal curing conditions. The extremely non-linear chemoviscosity profile for a dynamic heating cure cycle is predicted as well. The model is also shown to predict changes of glass transition temperature for the thermosetting resin during cure. The physical significance of this prediction is unclear at the present time, however, and further research is required. From the chemoviscosity simulation point of view, the technique of establishing an analytical model as described here is easily applied to any thermosetting resin. The model thus obtained is used in real-time process controls for fabricating composite materials.

Hou, T. H.↗

NASA NTRS1987

Studies on chemoviscosity modeling for thermosetting resins

A new analytical model for simulating chemoviscosity of thermosetting resins has been formulated. The model is developed by modifying the well-established Williams-Landel-Ferry (WLF) theory in polymer rheology for thermoplastic materials. By introducing a relationship between the glass transition temperature Tg(t) and the degree of cure alpha(t) of the resin system under cure, the WLF theory can be modified to account for the factor of reaction time. Temperature dependent functions of the modified WLF theory constants C sub 1 (t) and C sub 2 (t) were determined from the isothermal cure data. Theoretical predictions of the model for the resin under dynamic heating cure cycles were shown to compare favorably with the experimental data. This work represents progress toward establishing a chemoviscosity model which is capable of not only describing viscosity profiles accurately under various cure cycles, but also correlating viscosity data to the changes of physical properties associated with the structural transformation of the thermosetting resin systems during cure.

Bai, J. M.↗

NASA NTRS1985

Chemoviscosity modeling for thermosetting resins, 2

A new analytical model for simulating chemoviscosity of thermosetting resin was formulated. The model is developed by modifying the Williams-Landel-Ferry (WLF) theory in polymer rheology for thermoplastic materials. By assuming a linear relationship between the glass transition temperature and the degree of cure of the resin system under cure, the WLF theory can be modified to account for the factor of reaction time. Temperature dependent functions of the modified WLF theory constants were determined from the isothermal cure data of Lee, Loos, and Springer for the Hercules 3501-6 resin system. Theoretical predictions of the model for the resin under dynamic heating cure cycles were shown to compare favorably with the experimental data reported by Carpenter. A chemoviscosity model which is capable of not only describing viscosity profiles accurately under various cure cycles, but also correlating viscosity data to the changes of physical properties associated with the structural transformations of the thermosetting resin systems during cure was established.

Hou, T. H.↗

NASA NTRS1980

Oxygen index tests of thermosetting resins

The flammability characteristics of nine thermosetting resins under evaluation for use in aircraft interiors are described. These resins were evaluated using the Oxygen Index (ASTM 2863) testing procedure. The test specimens consisted of both neat resin and glass reinforced resin. When testing glass-reinforced samples it was observed that Oxygen Index values varied inversely with resin content. Oxygen values were also obtained on specimens exposed to temperatures up to 300 C. All specimens experienced a decline in Oxygen Index when tested at an elevated temperature.

Gilwee, W. J., Jr.↗

NASA NTRS1985

NASA/aircraft industry standard specification for graphite fiber toughened thermoset resin composite material

A standard specification for a selected class of graphite fiber/toughened thermoset resin matrix material was developed through joint NASA/Aircraft Industry effort. This specification was compiled to provide uniform requirements and tests for qualifying prepreg systems and for acceptance of prepreg batches. The specification applies specifically to a class of composite prepreg consisting of unidirectional graphite fibers impregnated with a toughened thermoset resin that produce laminates with service temperatures from -65 F to 200 F when cured at temperatures below or equal to 350 F. The specified prepreg has a fiber areal weight of 145 g sq m. The specified tests are limited to those required to set minimum standards for the uncured prepreg and cured laminates, and are not intended to provide design allowable properties.

Source record↗

NASA NTRS1985

Chemoviscosity modeling for thermosetting resins

A chemoviscosity model, which describes viscosity rise profiles accurately under various cure cycles, and correlates viscosity data to the changes of physical properties associated with structural transformations of the thermosetting resin system during cure, was established. Work completed on chemoviscosity modeling for thermosetting resins is reported.

Tiwari, S. N.↗

NASA NTRS1978

Rapid viscosity measurements of powdered thermosetting resins

A rapid and inexpensive method of obtaining processing-related data on powdered thermosetting resins has been investigated. The method involved viscosity measurements obtained with a small specimen (less than 100 mg) parallel plate plastometer. A data acquisition and reduction system was developed which provided a value of viscosity and strain rate about 12-13 second intervals during a test. The effects of specimen compaction pressure and reduction of adhesion between specimen and parallel plates were examined. The plastometer was used to measure some processing-related viscosity changes of an addition polyimide resin, including changes caused by pre-test heat treatment, test temperature, and strain rate.

Price, H. L.↗

NASA NTRS1986

Modeling the curing process of thermosetting resin matrix composites

A model is presented for simulating the curing process of a thermosetting resin matrix composite. The model relates the cure temperature, the cure pressure, and the properties of the prepreg to the thermal, chemical, and rheological processes occurring in the composite during cure. The results calculated with the computer code developed on the basis of the model were compared with the experimental data obtained from autoclave-curved composite laminates. Good agreement between the two sets of results was obtained.

Loos, A. C.↗

NASA NTRS1988

Chemoviscosity modeling for thermosetting resin systems, part 3

A new analytical model for simulating chemoviscosity resin has been formulated. The model is developed by modifying the well established Williams-Landel-Ferry (WLF) theory in polymer rheology for thermoplastic materials. By introducing a relationship between the glass transition temperature (T sub g (t)) and the degree of cure alpha(t) of the resin system under cure, the WLF theory can be modified to account for the factor of reaction time. Temperature-dependent functions of the modified WLF theory parameters C sub 1 (T) and C sub 2 (T) were determined from the isothermal cure data. Theoretical predictions of the model for the resin under dynamic heating cure cycles were shown to compare favorably with the experimental data. This work represents a progress toward establishing a chemoviscosity model which is capable of not only describing viscosity profiles accurately under various cure cycles, but also correlating viscosity data to the changes of physical properties associated with the structural transformations of the thermosetting resin systems during cure.

Hou, T. H.↗

NASA NTRS1979

Advanced thermoset resins for fire-resistant composites

The thermal and flammability properties of some thermoset polymers and composites are described. The processing and evaluation of composites fabricated from currently used resins and advanced fire-resistant resins are also described. Laboratory test methodology used to qualify candidate composite materials includes thermochemical characterization of the polymeric compounds and evaluation of the glass reinforced composites for flammability and smoke evolution. The use of these test methods will be discussed in comparing advanced laminating resins and composites consisting of modified epoxies, phenolics and bismaleimide, with conventional baseline materials consisting of epoxy.

Kourtides, D. A.↗

NASA NTRS1982

Fabricating Thin-Film High-Temperature Thermoset Resins

To prepare an epoxy thin film, quantity of uncured epoxy to be cast placed in vacuum oven and heated to melting temperature. Vacuum of about 30 mm Hg is applied to deaerate epoxy charge. Pressure is cycled with each foaming until all air and excess volatiles are revoved. thermoset (cross-linked) resin is cast between thin, flexible, releasing substrate films. Films less than 0.025 mm in thickness are made routinely with this facility.

Dickerson, G. E.↗

NASA NTRS1978

Characterization of flammability properties of some thermoplastic and thermoset resins

The thermochemical and flammability properties of some thermally stable polymers considered for use in aircraft interiors are described. The properties studied include: (1) thermomechanical properties such as glass transition and melt temperature; (2) dynamic thermogravimetric analysis in anaerobic environment; (3) flammability properties such as oxygen index, flame spread, and smoke evolution; and (4) selected physical properties. The thermoplastic polymers evaluated included polyphenylene sulfide, polyaryl sulfone, 9,9-bis(4-hydroxyphenyl)-fluorene polycarbonate-poly(dimethylsiloxane) and polyether sulfone. The thermoset polymers evaluated included epoxy, bismaleimide, a modified phenolic and polyaromatic melamine resin. These resins were primarily used in the fabrication of glass reinforced prepregs for the construction of experimental panels. Test results and relative rankings of some of the flammability parameters are presented and the relationship of the molecular structure, char yield, and flammability properties of these polymers are discussed.

Kourtides, D. A.↗

NASA NTRS1984

Free Volume Considerations in Thermoplastic and Thermosetting Resins

The direct measurement of physical aging and of the volume changes which go on during the course of this aging is discussed. Data on PMMA showing its physical aging as measured by its stress relaxation response and the accompanying volume changes are presented. An indication of how one can measure the free volume both directly from the volume change itself and relatively directly via a new technique is given. The application of this new technique (electron spin resonance spectroscopy) to other polymer systems is demonstrated.

Landel, R. F.↗

NASA NTRS1989

Chemoviscosity modeling for thermosetting resin systems, 4

An experimental study on the changes of chemorheological properties has been conducted and analyzed on commercial Hercules 3501-6 resin system cured under several isothermal conditions between 375 and 435 K. For the cure temperatures equal to or greater than 385 K, the storage modulus curing curves, G prime (t), exhibited abrupt changes in slope which occurred at various times depending on the curing temperatures and were attributed to the onset of gelation reactions. The crossover points between G prime (t) and G double prime (t) curves were observed for curing temperatures equal to or greater than 400 K. The gelation and the crossover points obtained from the chemorheological measurements, therefore, defined two characteristic resin states during cure. Approximately the same value for the degree of cure was reached by the advancement of the reaction at each of these states. The temperature dependency of the viscosities for the characteristic resin states and the rate constants of increase in moduli at different stages of curing were analyzed. Various G prime (t) and G double prime (t) isothermal curing curves were also shown to be capable of being superimposed on one another by the principle of time-temperature superposition. The resultant shift factors a sub t(t) and a Eta(T) were shown to follow the Arrhenius type relationship. Values of the activation energy suggested that the reaction kinetics, instead of the diffusion mechanism, was the limiting step in the overall resin advancement for the cure at temperatures equal to or greater than 385 K.

Hou, T. H.↗

NASA NTRS1989

A predictive model for failure properties of thermoset resins

A predictive model for the three-dimensional failure behavior of engineering polymers has been developed in a recent NASA-sponsored research program. This model acknowledges the underlying molecular deformation mechanisms and thus accounts for the effects of different chemical compositions, crosslink density, functionality of the curing agent, etc., on the complete nonlinear stress-strain response including yield. The material parameters required by the model can be determined from test-tube quantities of a new resin in only a few days. Thus, we can obtain a first-order prediction of the applicability of a new resin for an advanced aerospace application without synthesizing the large quantities of material needed for failure testing. This technology will effect order-of-magnitude reductions in the time and expense required to develop new engineering polymers.

Caruthers, James M.↗

NASA NTRS1990

Acetylene-chromene terminated resins as high temperature thermosets

A novel phase transfer catalyzed process for the preparation of propargyl ethers has been developed. The propargyl ethers serve as precursors to a new class of thermosetting resins called acetylene-chromene terminated (ACT) resins. Heat treatment of a solution of propargyl ethers with various catalysts, followed by removal of solvent leads to the ACT resins via partial conversion of the propargyl ether groups to chromenes. This process reduces the energy content of the resin systems and reduces the amount of shrinkage found during cure. Due to the presence of the solvent the process is safe and gives rise to low viscosity products suitable for resin transfer molding and filament winding type applications. Due to the high glass transition temperature, high modulus, and low moisture uptake the cured resins display better than 232 C/wet performance. The thermal stability of the ACT resins in air at 204 C is superior to that of conventional bismaleimide resins. The resins also display excellent electrical properties.

Godschalx, J. P.↗

NASA NTRS2023

Dynamic Crush Performance of Thermoplastic and Resin Infused Thermoset Triaxially Braided Composite Structures

Dynamic crush tests were conducted on triaxially braided composite tubes and C-channel structural elements to measure their relative energy absorbing characteristics. The elements were manufactured from triaxially braided [0/+60/-60] T700 fiber preforms with two different resin systems, a PR520 thermoset resin and a LM-PAEK thermoplastic resin. T700/PR520 composite tubes and C-channel elements were manufactured using a resin infusion process. T700GC/LMPAEK composite tubes were manufactured by braiding slit tape prepreg onto cylindrical mandrels. Consolidation pressure was applied through thermally activated shrink tape in an oven. The energy absorbing characteristics of the composite elements were measured using a pneumatically actuated sled with a flat-faced impacting mass, which provided several independent measurements of force, displacement, and energy absorption. The parameter primarily used for comparison between the systems was the specific energy absorption (SEA), a measure of energy absorbed per unit crushed length. The T700/LMPAEK tubes performed slightly better than T700/PR520 tubes, with an approximately 9% higher SEA. T700/PR520 tubes had over 20% higher SEA than C-channels made from the same material. Additional tests were conducted on tubes using a tapered-conical impactor to force the tubes to fail in circumferential tension. This type of impact significantly reduced the energy absorption.

Composite Materials↗

NASA NTRS2023

Dynamic Crush Performance of Thermoplastic and Resin Infused Thermoset Triaxially Braided Composite Structures

Composite Materials↗