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NASA NTRS1992

Isothermal aging effects on PMR-15 resin

Specimens of PMR-15 polyimide neat resin were aged in air at temperatures of 288, 316, and 343 C. Weight losses and dimensional changes were monitored during the course of the exposure time. Physical changes were also observed by optical and electron microscopy. It was found that polyimide polymer degradation occurred within a thin surface layer that developed and grew during thermal aging. The cores of the polymer specimens were protected from oxidative degradation, and they were relatively unchanged by the thermal treatment. Surface cracking was observed at 343 C and was probably due to an interaction between voids and stresses that developed in the surface layer.

Bowles, Kenneth J.↗

NASA NTRS1993

Isothermal aging effects on PMR-15 resin

Bowles, Kenneth J.↗

NASA NTRS1998

Comparison of Graphite Fabric Reinforced PMR-15 and Avimid N Composites After Long Term Isothermal Aging at Various Temperatures

Extensive effort is currently being expended to demonstrate the feasibility of using high-performance, polymer-matrix composites as engine structural materials over the expected operating lifetime of the aircraft, which can extend from 18,000 to 30,000 hr. The goal is to develop light-weight, high-strength, and high-modulus materials for use in higher temperature sections of advanced 21 st century aircraft propulsion systems. To accomplish this goal, it is necessary to pursue the development of thermal and mechanical durability models for graphite-fiber-reinforced, polymer-matrix composites. Numerous investigations have been reported regarding the thermo-oxidative stability (TOS) of the polyimide PMR-15 (1-5). A significant amount of this work has been directed at edge and geometry effects, reinforcement fiber influences, and empirical modeling of high-temperature weight loss behavior. It is yet to be determined if the information obtained from the PMR-15 composite tests is applicable to other polyimide-matrix composites. The condensation-curing polymer Avimid N is another advanced composite material often considered for structural applications at high temperatures. Avimid N has better thermo-oxidative stability than PMR-15 (6), but the latter is more easily processed. The most comprehensive study of the thermo-oxidative stability of Avimid N neat resin and composites at 371 (infinity)C is found in Salin and Seferis (7). The purposes of the work described herein were to compare the thermal aging behavior of these two matrix polymers and to determine the reasons for and the consequences of the difference in thermal durability. These results might be of some use in improving future polymer development through the incorporation of the desirable characteristics of both polyimides.

Bowles, Kenneth J.↗

NASA NTRS1972

Effect of aging at 1040 C (1900 F) on the ductility and structure of a tantalum alloy, T-111

The post-aging embrittlement of T-111 (tantalum - 8-percent tungsten - 2-percent hafnium) following exposure for up to about 10,000 hours at 1040 C in either vacuum or liquid lithium was investigated for sheet and tubing samples. This thermal aging was shown to greatly increase the sensitivity of T-111 to hydrogen embrittlement during subsequent room temperature specimen processing or testing. The hydrogen embrittlement problem can be avoided by preventing exposure to the T-111 to moisture during post-aging processing or testing. Aging at 1040 C also resulted in formation of HfO2 particles at grain boundaries, which may contribute to the observed embrittlement.

Watson, G. K.↗

NASA NTRS1993

Lifetime prediction of materials exposed to the natural space environment

The goal of this study is to model the lifetime of different types of seal materials based on results obtained from accelerated experiments. A semi-mechanistic approach was taken. Thermal aging data were taken from the literature whereas experiments were conducted at Auburn under this contract for selected environments. The seal materials of interest are Silicone 383, Silicone 650, Viton 835, and Viton 747. The relevant conditions include thermal, oxygen, inert gas, vacuum, and gamma radiation. Compression set data available from NASA were used to examine the thermal effect. Experiments were conducted at Auburn University and at NASA to isolate the role of thermal, oxygen, inert gas, vacuum, gamma irradiation, and proton irradiation. A simple discrete stress relaxation method was developed to determine the relaxation response of the elastomers. Dynamic mechanical thermal analysis was also used to characterize the mechanical response of the specimens. These provide a more meaningful correlation between mechanisms and degradation.

Zee, Ralph↗

NASA NTRS2007

High Thermal Conductivity Polymer Matrix Composites (PMC) for Advanced Space Radiators

High temperature polymer matrix composites (PMC) reinforced with high thermal conductivity (approx. 1000 W/mK) pitch-based carbon fibers are evaluated for a facesheet/fin structure of large space radiator systems. Significant weight reductions along with improved thermal performance, structural integrity and space durability toward its metallic counterparts were envisioned. Candidate commercial resin systems including Cyanate Esters, BMIs, and polyimide were selected based on thermal capabilities and processability. PMC laminates were designed to match the thermal expansion coefficient of various metal heat pipes or tubes. Large, but thin composite panels were successfully fabricated after optimizing cure conditions. Space durability of PMC with potential degradation mechanisms was assessed by simulated thermal aging tests in high vacuum, 1-3 x 10(exp -6) torr, at three temperatures, 227 C, 277 C, and 316 C for up to one year. Nanocomposites with vapor-grown carbon nano-fibers and exfoliated graphite flakes were attempted to improve thermal conductivity (TC) and microcracking resistance. Good quality nanocomposites were fabricated and evaluated for TC and durability including radiation resistance. TC was measured in both in-plan and thru-the-thickness directions, and the effects of microcracks on TC are also being evaluated. This paper will discuss the systematic experimental approaches, various performance-durability evaluations, and current subcomponent design and fabrication/manufacturing efforts.

Shin, E. Eugene↗

NASA NTRS1994

Microstructural analysis of cracks generated during welding of 2195 aluminum-lithium alloy

This research summarizes a series of studies conducted at Marshall Space Flight Center to characterize the properties of 2195 Al-Li alloy. 2195 Al-Li alloy, developed by Martin Marietta laboratories, is designated as a replacement of 2219 Al-Cu alloy for the External Tank (E.T.) of the space shuttle. 2195 Al-Li alloy with its advantage of increased strength per weight over its predecessor, 2219 Al-Cu alloy, also challenges current technology. 2195 Al-Li has a greater tendency to crack than its predecessor. The present study began with the observation of pore formation in 2195 Al-Li alloy in a thermal aging process. In preliminary studies, Talia and Nunes found that most of the two pass welds studied exhibited round and crack-like porosity at the weld roots. Furthermore, the porosity observed was associated with the grain boundaries. The porosity level can be increased by thermal treatment in the air. A solid state reaction proceeding from dendritic boundaries in the weld fusion zone was observed to correlate with the generation of the porosity.

Talia, George E.↗

NASA NTRS1992

Effect of fiber reinforcement on thermo-oxidative stability and mechanical properties of polymer matrix composites

A number of studies have investigated the thermooxidative behavior of polymer matrix composites. Two significant observations have been made from these research efforts: (1) fiber reinforcement has a significant effect on composite thermal stability; and (2) geometric effects must be considered when evaluating thermal aging data. The polyimide PMR-15 was the matrix material used in these studies. The control composite material was reinforced with Celion 6000 graphite fiber. T-4OR graphite fibers, along with some very stable ceramic fibers were selected as reinforcing fibers because of their high thermal stability. The ceramic fibers were Nicalon (silicon carbide) and Nextel 312 (alumina-silica-boron oxide). The mechanical properties of the two graphite fiber composites were significantly different, probably owing to variations in interfacial bonding between the fibers and the polyimide matrix. Three oxidation mechanisms were observed: (1) the preferential oxidation of the Celion 6000 fiber ends at cut surfaces, leaving a surface of matrix material with holes where the fiber ends were originally situated; (2) preferential oxidation of the composite matrix; and (3) interfacial degradation by oxidation. The latter two mechanisms were also observed on fiber end cut surfaces. The fiber and interface attacks appeared to initiate interfiber cracking along these surfaces.

Bowles, K. J.↗

NASA NTRS1995

Evaluation of Rhenium Joining Methods

Coupons of rhenium-to-Cl03 flat plate joints, formed by explosive and diffusion bonding, were evaluated in a series of shear tests. Shear testing was conducted on as-received, thermally-cycled (100 cycles, from 21 to 1100 C), and thermally-aged (3 and 6 hrs at 1100 C) joint coupons. Shear tests were also conducted on joint coupons with rhenium and/or Cl03 electron beam welded tabs to simulate the joint's incorporation into a structure. Ultimate shear strength was used as a figure of merit to assess the effects of the thermal treatment and the electron beam welding of tabs on the joint coupons. All of the coupons survived thermal testing intact and without any visible degradation. Two different lots of as-received, explosively-bonded joint coupons had ultimate shear strengths of 281 and 310 MPa and 162 and 223 MPa, respectively. As-received, diffusion-bonded coupons had ultimate shear strengths of 199 and 348 MPa. For the most part, the thermally-treated and rhenium weld tab coupons had shear strengths slightly reduced or within the range of the as-received values. Coupons with Cl03 weld tabs experienced a significant reduction in shear strength. The degradation of strength appeared to be the result of a poor heat sink provided during the electron beam welding. The Cl03 base material could not dissipate heat as effectively as rhenium, leading to the formation of a brittle rhenium-niobium intermetallic.

Reed, Brian D.↗

NASA NTRS1989

Predictive aging of polymers

A method of predicting aging of polymers operates by heating a polymer in the outdoors to an elevated temperature until a change of property is induced. The test is conducted at a plurality of temperatures to establish a linear Arrhenius plot which is extrapolated to predict the induction period for failure of the polymer at ambient temperature. An Outdoor Photo Thermal Aging Reactor (OPTAR) is also described including a heatable platen for receiving a sheet of polymer, means to heat the platen, and switching means such as a photoelectric switch for turning off the heater during dark periods.

Cuddihy, Edward F.↗

NASA NTRS1990

Predictive aging of polymers

A method of predicting aging of polymers operates by heating a polymer in the outdoors to an elevated temperature until a change of property is induced. The test is conducted at a plurality of temperatures to establish a linear Arrhenius plot which is extrapolated to predict the induction period for failure of the polymer at ambient temperature. An Outdoor Photo Thermal Aging Reactor (OPTAR) is also described including a heatable platen for receiving a sheet of polymer, means to heat the platen and switching means such as a photoelectric switch for turning off the heater during dark periods.

Cuddihy, Edward F.↗

NASA NTRS2024

Preliminary Measurements of Partial Discharge Inception Voltage Degradation with Constant Temperature Aging of Magnet Wire Twisted Pairs for Electric Aircraft Motors

Electric aircraft require high reliability electric motors to meet the stringent safety standards of the aviation industry. Motor winding insulation lifetime and reliability models for electric aircraft applications are needed to enable design of high reliability and high-performance electric motors for aviation applications. Three primary stresses effect the lifetime of motor winding insulation: thermochemical, mechanical, and electrical. This paper presents preliminary experiments on twisted pairs of magnet wire targeting understanding the thermo-chemical degradation of motor winding insulation through constant temperature thermal aging. Three types of magnet wire twisted pairs where tested: polyimide insulated magnet wire, epoxy coated polyimide insulated magnet wire, and epoxy potted polyimide magnet wire. The degradation of the samples over time at temperature was tracked using partial discharge inception voltage measurements. These initial experiments were used for development of procedures and expertise in partial discharge testing and thermo-chemical aging to inform future testing. The preliminary nature of these experiments should be noted when viewing the results. Lessons learned from the experiments are documented.

Thomas Tallerico↗

NASA NTRS1991

Development and testing of a superconducting link for an IR detector

The development and testing of a ceramic superconducting link for an infrared detector is summarized. Areas of study included the materials used, the electrical contacts, radiation and temperature cycling effects, aging, thermal conductivity, and computer models of an ideal link. Materials' samples were processed in a tube furnace at temperatures of 840 C to 865 C for periods up to 17 days and transition temperatures and critical current densities were recorded. The project achieved better quality high superconducting transition temperature material through improved processing and also achieved high quality electrical contacts. Studies on effects of electron irradiation, temperature cycling, and aging on superconducting properties indicate that the materials will be suitable for space applications. Various presentations and publications on the study's results are reported.

Caton, R.↗

NASA NTRS1991

Effect of fiber reinforcements on thermo-oxidative stability and mechanical properties of polymer matrix composites

A number of studies have investigated the thermo-oxidative behavior of polymer matrix composites. Two significant observations have been made from these research efforts: (1) fiber reinforcement has a significant effect on composite thermal stability; and (2) geometric effects must be considered when evaluating thermal aging data. A compilation of some results from these studies is presented, and this information shows the influence of the reinforcement fibers on the oxidative degradation of various polymer matrix composites. The polyimide PMR-15 was the matrix material that was used in these studies. The control composite material was reinforced with Celion 6000 graphite fiber. T-40R graphite fibers, along with some very stable ceramic fibers were selected as reinforcing fibers because of their high thermal stability. The ceramic fibers were Nicalon (silicon carbide) and Nextel 312 (alumina-silica-boron oxide). The mechanical properties of the two graphite fiber composites were significantly different, probably owing to variations in interfacial bonding between the fibers and the polyimide matrix. The Celion 6000/PMR-15 bond is very tight but the T-40/PMR-15 bond is less tight. Three oxidation mechanisms were observed: (1) the preferential oxidation of the Celion 6000 fiber ends at cut surfaces, leaving a surface of matrix material with holes where the fiber ends were originally situated; (2) preferential oxidation of the composite matrix; and (3) interfacial degradation by oxidation. The latter two mechanisms were also observed on fiber end cut surfaces. The fiber and interface attacks appeared to initiate interfiber cracking along these surfaces.

Bowles, Kenneth J.↗

NASA NTRS1983

High-temperature molten salt thermal energy storage systems for solar applications

Experimental results of compatibility screening studies of 100 salt/containment/thermal conductivity enhancement (TCE) combinations for the high temperature solar thermal application range of 704 deg to 871 C (1300 to 1600 F) are presented. Nine candidate containment/HX alloy materials and two TCE materials were tested with six candidate solar thermal alkali and alkaline earth carbonate storage salts (both reagent and technical grade of each). Compatibility tests were conducted with salt encapsulated in approx. 6.0 inch x 1 inch welded containers of test material from 300 to 3000 hours. Compatibility evaluations were end application oriented, considering the potential 30 year lifetime requirement of solar thermal power plant components. Analyses were based on depth and nature of salt side corrosion of materials, containment alloy thermal aging effects, weld integrity in salt environment, air side containment oxidation, and chemical and physical analyses of the salt. A need for more reliable, and in some cases first time determined thermophysical and transport property data was also identified for molten carbonates in the 704 to 871 C temperature range. In particular, accurate melting point (mp) measurements were performed for Li2CO3 and Na2CO3 while melting point, heat of fusion, and specific heat determinations were conducted on 81.3 weight percent Na2CO3-18.7 weight percent K2CO3 and 52.2 weight percent BaCO3-47.8 weight percent Na2CO3 to support future TES system design and ultimate scale up of solar thermal energy storage (TES) subsystems.

Petri, R. J.↗

NASA NTRS1973

Evaluation of polyimide/glass fiber composites for construction of light weight pressure vessels for cryogenic propellants

The application of polyimide resin as a matrix for glass filament-wound thin metal-lined pressure vessels was studied over a temperature range of (minus) 320 to 600 F. Keramid 601 polyimide was found to perform quite well over the entire range of temperature. Hoop stress values of 425 ksi were determined at 75 F which is equivalent to epoxy resin in similar structures. At -320 and 600 F, 125 and 80% of this strength was retained. Thermal ageing at 500 F for up to 50 hours was studied with severe reduction in strength, but there is evidence that this reduction could be improved. Another polyimide resin studied was P10PA which was found to have processing characteristics inappropriate for filament-winding. NOL ring tensile and shear data was determined from both resins with S-glass. Pressure vessel design, fabrication and test procedures are described in detail.

Petker, I.↗

NASA NTRS1974

Creep behavior of tantalum alloy T-222 at 1365 to 1700 K

High vacuum creep tests on the tantalum T-222 alloy at 0.42 to 0.52 T sub m show that the major portion of the creep curves, up to at least 1 percent strain, can be best described by an increasing creep rate, with strain varying linearly with time. Correlation and extrapolation of the creep curves on the basis of increasing creep rates results in more accurate engineering design data than would use of approximated linear rates. Based on increasing creep rates, the stress for 1 percent strain in 10,000 hours for T-222 is about four times greater than for the Ta-10W alloy. Increasing the grain size results in increased creep strength. Thermal aging prior to testing caused precipitation of the hexagonal close packed (Hf,Ta) sub 2 C, which initially increased creep strength. However, this dimetal carbide was converted during creep testing to face-centered cubic (Hf,Ta)C.

Titran, R. H.↗

NASA NTRS1974

Interdiffusion behavior of tungsten or rhenium and group 5 and 6 elements and alloys of the periodic table. Part 2A: Appendices A-G

Arc cast W, CVD, W, CVD Re, and powder metallurgy Re materials were hot isostatically pressure welded to ten different refractory metals and alloys and thermally aged at 10 to the minus 8th power torr at 1200 C, 1500 C, 1630 C, 1800 C, and 2000 C for 100 hours to 2000 hours. Electron beam microprobe analysis was used to characterize the interdiffusion zone width of each couple system as a function of age time and temperature. Each system was least squares fitted to the equation: In (delta X sq/t) = B/T + A, where delta X is net interdiffusion zone width, t is age time, and T is age temperature. Detailed descriptions of experimental and analytical procedures utilized in conducting the experimental program are provided. For Vol. 1, see N74-34046.

Arcella, F. G.↗