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An alert was issued because of the arc-tracking possibilities of installed polyimide wire harnesses. MSFC undertook a program to try to enhance the safety and reliability of these harnesses. Photographs are presented showing the need for inspections of installed wiring harnesses.
Disclosed is a thermally-stable SnO2-surfaced polyimide film wherein the electrical conductivity of the SnO2 surface is within the range of about 3.0 x 10(exp -3) to about 1 x 10(exp -2) ohms(exp -1). Also disclosed is a method of preparing this film from a solution containing a polyamic acid and SnCl4 (DMSO)2.
Diamines containing pendent ethynyl and substituted ethynyl groups are synthesized. These diamines are reacted with dianhydrides to form polyamide acids, which are chemically or thermally cyclodehydrated to form polyimides and copolyimides with pendent ethynyl groups. Upon heating, the pendent ethynyl groups react to form crosslinked resins that are useful as adhesives, composite matrices, coatings, moldings, and films.
Offset stoichiometries and end-capping agents impart desired properties. Semicrystalline polyimides synthesized from 3,3',4,4' benzophenonetetracarboxylic dianhydride (BTDA) and 1,3-bis(4-aminophenoxy-4'-benzoyl)benzene (1,3-BABB) modified to increase melt flow. Modified versions more amenable to compression molding, processing to form adhesive bonds, and use as matrices in matrix/fiber composite materials.
Linear aromatic polyimides containing cyclobutene-3,4,-dione moieties synthesized in experiments. Polymers exhibit high thermal and thermo-oxidative stabilities, making them useful in structural components exposed to hot and/or oxidative environments, as in jet engines and on outer surfaces of supersonic aircraft. Electrons in cyclobutene-3,4-dione moieties readily excited to states of higher energy upon exposure to ultraviolet light, giving rise to electronic properties with potential utility in photovoltaic, photoconductive, and/or photoemissive devices.
Report describes experimental study of permeabilities, by each of five gases, of membranes made of four different polyimides. Conducted to gain understanding of effects of molecular structures of membranes on permeabilities and to assess potential for exploitation of selective permeability in gas-separation processes. Gases used: H2, O2, N2, CO2, and CH4.
Thermoset polyimides have great potential for successfully meeting tough stress and temperature challenges in the advanced aircraft development program. However, studies of structure-property relationships in these materials have not been very successful so far. Positron lifetime spectroscopy (PLS) has been used to investigate free volumes and associated parameters in a series of variable, segmental molecular weight samples. The free volume correlates well with the molecular weight M(sub c), the cross-link density v, and the coefficient of thermal expansion (CTE) of these materials. Currently, no other techniques are available for direct measurement of these parameters, particularly for polymers in solid phase. Experimental results and their interpretations are presented.
When a thin film of polymer is coated on to a quartz crystal microbalance (QCM), the QCM can be used to detect the rate of increase in weight of the polymer film as the volatile penetrant diffuses into the polymer. From this rate information the diffusion coefficient of the penetrant into the polymer can be computed. Calculations requiring this diffusion coefficient lead to values which approximate the monomeric friction coefficient of the polymer. This project has been concerned with the trial of crystal oscillating circuits suitable for driving polymer coated crystals in an atmosphere of penetrant. For these studies done at room temperature, natural rubber was used as an easily applied polymer that is readily penetrated by toluene vapors, qualities anticipated with polyimides when they are tested at T(g) in the presence of toluene. Three quartz crystal oscillator circuits were tested. The simplest circuit used +/- 5 volt dc and had a transistor to transistor logic (TTL) inverter chip that provides a 180 deg phase shift via a feed back loop. This oscillator circuit was stable but would not drive the crystal when the crystal was coated with polymer and subjected to toluene vapors. Removal of a variable resistor from this circuit increased stability but did not otherwise increase performance. Another driver circuit tested contained a two stage differential input, differential output, wide band video amplifier and also contain a feed back loop. The circuit voltage could not be varied and operated at +/- 5 volts dc; this circuit was also stable but failed to oscillate the polymer coated crystal in an atmosphere saturated with toluene vapors. The third oscillator circuit was of similar construction and relied on the same video amplifier but allowed operation with variable voltage. This circuit would drive the crystal when the crystal was submerged in liquid toluene and when the crystal was coated with polymer and immersed in toluene vapors. The frequency readings obtained when using this oscillating circuit are highly variable. This circuit requires further modification to stabilize frequency readings before its use in studies to determine the diffusion coefficient of penetrant molecules into a polymer film coated on a QCM.
Experimental polyimides relatively rigid synthesized in effort to exploit some of advantages of rodlike polymers, while alleviating disadvantages. Polymers used to make colorless fibers and transparent films for optical and electronic application.
Experiments show thin surface coats of silicon dioxide on thin undercoats of aluminum oxide retards thermooxidative degradation of polyimide-matrix/carbon-fiber composite materials.
Thermoset polyimides have great potential for successfully meeting tough stress and temperature challenges in the advanced aircraft development program. However, studies of structure/property relationships in these materials have not been very successful so far. Positron annihilation spectroscopy has been used to investigate free volumes and associated parameters. It has been noted that the free volume correlates well with the molecular weight, cross-link density and thermal coefficient of expansion of these materials. Currently no other techniques are available for direct measurement of these parameters. Experimental results and their interpretations will be discussed.
In this work a series of polyimides are investigated which exhibit a strong piezoelectric response and polarization stability at temperatures in excess of 100 C. This work was motivated by the need to develop piezoelectric sensors suitable for use in high temperature aerospace applications.
Composite IM7-K3B was subjected to a simulated high speed aircraft thermal environment to determine the effects of microcracking on the change in CTE. IM7-K3B is a graphite fiber reinforced polyimide laminate, manufactured by Dupont. The lay-up for the material was (0.90((Sub 3)(Sub s))). The specimens were placed in a laser-interferometric dilatometer to obtain thermal expansion measurements and were then repeatedly cycled between -65 F and 350 F up to 1000 cycles. After cycling they were scanned for microcracks at a magnification of 400x. The material was expected not to crack and to have a near zero CTE. Some microcracking did occur in all specimens and extensive microcracking occurred in one specimen. Further testing is required to determine how closely the CTE and microcracking are related.
The techniques necessary for the fabrication of a complex three-dimensional tubular form using a PMR-type resin have been developed to allow for the construction of several tubes with good physical and mechanical properties. Employing established resin transfer molding practices, the relatively non-hazardous AMB-21 in acetone formulation was used to successfully impregnate four layers of AS4 braided graphite fiber preform previously loaded around an aluminum cylindrical core in an enclosed mold cavity. Using heat and vacuum, the solvent was evaporated to form a prepreg followed by a partial imidization and removal of condensation products. The aluminum core was replaced by a silicone rubber bladder and the cure cycle continued to the final stage of 550 F with a bladder internal pressure of 200 lbs/sq in while simultaneously applying a strong vacuum to the prepreg for removal of any additional imidization products. A combination of several modifications to the standard resin transfer molding methodology enabled the mold to 'breathe', allowing the imidization products a pathway for escape. AMB-21 resin was chosen because of the carcinogenic nature of the primary commercial polyimide PMR-15. The AMB-21 resin was formulated using commercially available monomers or monomer precursors and dissolved in a mixture of methyl alcohol and acetone. The viscosity of the resulting monomer solution was checked by use of a Brookfield rheometer and adjusted by adding acetone to an easily pumpable viscosity of about 600 cP. In addition, several types of chromatographic and thermal analyses were of the braids, and excess handling of the preforms broke some of the microscopic fibers, needlessly decreasing the strength of the finished part. In addition, three dimensional braided preforms with fibers along the length of the tube will be significantly stronger in tension than the braided preforms used in this study.
As an ongoing effort to develop structural adhesives for high performance aerospace applications, recent work has focused on phenylethynyl terminated imide (PETI) oligomers. The work reported herein involves the synthesis and characterization of a series of phenylethynyl containing oligomers designated LARC (TM) MPEI (Modified Phenylethynyl Terminated Polyimide). These oligomers contain mixtures of linear, branched and star-shaped molecules. The fully imidized polymers exhibited minimum melt viscosity as low as 600 poise at 335 C. Ti/Ti lap shear specimens processed at 288 C under 15 psi showed tensile shear strength of approx. 6000 psi and 5200 psi at ambient and 350 F temperatures, respectively. The chemistry and properties of these new MPEIs are presented and compared to an optimized linear PETI, LaRC(Tm) -PETI-5.
The durability of polymer matrix composites exposed to harsh environments is a major concern. Surface degradation and damage are observed in polyimide composites used in air at 125-300 C. It is believed that diffusion of oxygen into the material and oxidative chemical reactions are responsible. Previous work has characterized and modeled diffusion behavior, and thermogravimetric analyses (TGAS) have been carried out in nitrogen, air, and oxygen to provide quantitative information on thermal and oxidative reactions. However, the model developed using these data did not successfully extrapolate TGA data down to conditions seen in service. A test program that focuses on lower temperatures and makes use of isothermal tests was undertaken to achieve a better understanding of the degradation reactions under use conditions. A new, low-cost technique was developed to collect chemical degradation data for isothermal tests lasting over 200 hours in the temperature range 125-300 C. Results indicate complex behavior not captured by the previous model, including the presence of weight-adding reactions. Weight gain reactions dominated in the 125-225 C temperature range, while weight loss reactions dominated beyond 225 C. The data obtained from isothermal tests and earlier TGAs is used to develop an advanced model of the material behavior.
Experimental results are presented on the erosion characteristics of the polyimide Kapton H, which serves as a blanket material in solar arrays. This polymer has a number of characteristics that make it a suitable choice for both terrestrial and space applications. In this paper attention is focused on the durability of protected Kapton when exposed to atomic oxygen (AO) in a plasma asher. A strip of 0.025-mm thick Kapton film, coated on both sides with SiO2, was studied during a 1306 hour exposure. The erosion, located at defect sites in the protective coating and measured optically, is described in terms of volume loss as a function of AO fluence. Three simple geometric profiles are used to generate a useful array of cavity shapes to model erosion evolution. These models connect the volume erosion rate to the observed lateral expansion of the developing cavities via their diameters, measured adviacent to the upper and lower protective film, and fitted by least-squares regression to simple power law functions of fluence. The rationale for the choice of models is discussed. It was found that lateral growth in cavity size evolves less than linearly with fluence.
The oxidative degradation of PMR (for polymerization of monomeric reactants) polyimides at elevated temperatures was followed by cross-polarized magic angle spinning (CP-MAS) NMR. Labeling of selected sites in the polymers with C-13 allowed for direct observation of the transformations arising from oxidation processes. The formation of several degradation products has been proposed to be occurring in the cross-links derived from the nadic end caps on oxidation. Model compounds have been synthesized and characterized by CPMAS NMR with both normal and delayed decoupling to distinguish between protonated and unprotonated carbons. Comparison of these spectra to predicted chemical shifts of proposed products for the aged polymer provides further insight to degradation occurring in the cross-linked moieties.