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At least 1,117 records · Page 62
All sourcesNASA NTRSDOE OSTI
DOE OSTI2022

A New Perspective of Post-Weld Baking Effect on Al-Steel Resistance Spot Weld Properties through Machine Learning and Finite Element Modeling

The root cause of post-weld baking on the mechanical performance of Al-steel dissimilar resistance spot welds (RSWs) has been determined by machine learning (ML) and finite element modeling (FEM) in this study. A deep neural network (DNN) model was constructed to associate the spot weld performance with the joint attributes, stacking materials, and other conditions, using a comprehensive experimental dataset. The DNN model positively identified that the post-weld baking reduces the joint performance, and the extent of degradation depends on the thickness of stacking materials. A three-dimensional finite element (FE) model was then used to investigate the root cause and the mechanism of the baking effect. It revealed that the formation of high thermal stresses during baking, from the mismatch of thermal expansion between steel and Al alloy, causes damage and cracking of the brittle intermetallic compound (IMC) formed at the interface of the weld nugget during welding. This in turn reduces the joint performance by promoting undesirable interfacial fracture when the welds were subjected to externally applied loads. The FEM model further revealed that increase in structural stiffness, because of increase in steel sheet thickness, reduces the thermal stresses at the interface caused by the thermal expansion mismatch and consequently lessens the detrimental effect of post-weld baking on the joint performance.

36 MATERIALS SCIENCE↗
NASA NTRS2026

Microstructural Evolution and Mechanical Properties of LP-DED NASA HR-1 – A Hydrogen Resistant AM Superalloy for Space Propulsion Applications

The National Aeronautics and Space Administration (NASA) has actively pursued metal additive manufacturing (AM) technologies for spaceflight applications since the late 2000s. AM offers transformative advantages in cost, schedule, part consolidation, and design flexibility. Among the various AM techniques, laser powder directed energy deposition (LP-DED) is particularly well suited for fabricating complex geometries with fine feature resolution. In propulsion systems that utilize high-pressure gaseous hydrogen—such as liquid hydrogen rocket engines—hydrogen environment embrittlement (HEE) presents a serious threat to material performance 1,2 . Mechanical property degradation under these conditions can compromise component reliability, especially under cyclic loading. To address this challenge, NASA developed NASA HR-1 (Hydrogen Resistant-1) as a solution for liquid rocket engine components operating in hydrogen-rich environments, using the LP-DED technique 3-9 . A key component in a liquid rocket engine is the exhaust nozzle, which is typically regeneratively cooled (regen) due to the high heat flux. NASA HR-1 was specifically developed for regen nozzle applications using hydrogen as a propellant, providing resistance to HEE, a critical issue for many materials. The AM version of NASA HR-1 was also formulated to achieve high ultimate tensile strength, along with high yield strength and ductility in this environment 5,6 . Low-cycle fatigue (LCF) is another important consideration in nozzle design, as components are expected to endure multiple starts and missions. Additionally, the LP-DED version of the alloy exhibits improved thermal conductivity compared to its wrought counterpart, which benefits nozzle cooling. Overall, NASA HR-1 offers an excellent balance of high strength, HEE resistance, LCF performance, thermal conductivity, and ductility to meet the demanding requirements of channel-cooled nozzles and other components used with hydrogen and other propellants. The LP-DED–processed NASA HR-1 requires several post-processing heat treatment steps to achieve the material properties desirable for its intended application 6 . These steps include stress relief, homogenization, solution annealing, and aging for precipitation hardening. The stress relief treatment mitigates residual stresses accumulated during the LP-DED process and minimizes the potential for distortion. Homogenization, a common step for AM materials, reduces elemental segregation and promotes recrystallization to develop a more equiaxed grain structure. The subsequent solution annealing treatment heats the part to a solid solution temperature to dissolve the undesirable η-phase that forms during cooling from homogenization, followed by rapid cooling to retain an η-phase–free microstructure. Finally, aging promotes precipitation of the strengthening γ′ phase in the alloy. The integration of compositional design and optimized thermal processing enables high-quality LP-DED NASA HR-1 components with excellent microstructural and mechanical stability. Improved chemical and microstructure homogeneity enhances ductility and fatigue resistance—both critical for safe and reliable operation in high-pressure hydrogen environments. NASA has successfully fabricated and hot-fire tested multiple subscale and full-scale channel wall nozzles using LP-DED NASA HR-1 5,6, 9-14 . These efforts included process refinements to support thin-wall construction and various channel geometries. Throughout development, several key observations emerged. After homogenization, the as-built columnar grain structure transforms into a fully equiaxed microstructure. However, subsequent treatments—such as solution annealing and aging—result in changes that are more difficult to track. The grain structure remains largely unchanged, and the γ′ precipitates, typically 5–10 nm in diameter, are beyond the resolution of scanning electron microscopy (SEM). While transmission electron microscopy (TEM) can resolve these fine precipitates, TEM sample preparation is time-consuming and difficult for LP-DED material. As an alternative, differential scanning calorimetry (DSC) offers a useful, qualitative approach to monitor precipitate evolution throughout different stages of heat treatment. The overall goal is to improve the understanding of how heat treatment affects the microstructure and mechanical performance of LP-DED NASA HR-1. This paper presents heat treatment design considerations, microstructural characterization, mechanical testing – including tensile and LCF testing in both air and hydrogen environments.

Superalloy↗
DOE OSTI2025

Processing behavior evolution of recycled polypropylene: An integrated experimental and Computer-Aided engineering simulation study

Polypropylene (PP) comprises 21% of global plastics production and 18% of plastics waste, yet less than 1% of solid-waste PP is recycled in the United States (U.S.), representing significant environmental and economic challenges. Mechanical recycling, the most prevalent recycling method, subject's materials to thermomechanical stresses, which typically degrade polymer properties, affecting the quality of polymer products. This study replicates the impact of mechanical recycling through multiple extrusion cycles to examine the effects on PP's processing behavior. Dynamic scanning calorimetry (DSC) measurements showed stable melting behavior across all processing conditions, while crystallization analysis exhibited consistent shifts in kinetic parameters. Rheological characterization demonstrated progressive viscosity reductions through successive cycles, particularly pronounced at elevated reprocessing temperatures. Here, the integration of this experimental data into injection molding simulations showed that recycled PP maintains viable processing characteristics. Our findings establish quantitative correlations between processing history and material behavior, enabling optimization of processing parameters directly rather than relying on trial-and-error approaches. While these results reflect idealized recycling conditions with minimal contamination, they provide a framework for understanding fundamental property evolution during mechanical recycling.

42 ENGINEERING↗
NASA NTRS1979

Radiation damage in high-voltage silicon solar cells

Three types of open circuit high voltage solar cells were tested to determine their performance after exposure to 1 MeV electron irradiations. The cells with a relatively deep n-type emitter were more susceptible to radiation damage than other high open circuit high voltage cells. The use of diffused or ion implanted junctions leads to open circuit high voltage cell designs that are less susceptible to radiation damage. These latter two types of cells show degradations that are typical of the 0.1 ohm-cm material from which they are fabricated. Furthermore, exposure to ionizing radiation causes oxide degradation and decreased cell performance in cells that depend on a charged oxide to achieve significant cell properties. Hence, the combination of a charged oxide and a relatively deep n-type emitter is not recommended for incorporation into a cell designed for use in the particulate radiation environment of space.

Weinberg, I.↗
DOE OSTI2020

Graphite Licensing (ASME) and Testing (ASTM) Technical Assistance

DOE ART Graphite R&D program is currently involved in developing the structural code for licensing the new High Temperature Reactor (HTR) designs through the ASME Boiler Pressure Vessel Code (BPVC). The basic structural design code for graphite core components has been written, approved, and within the BPVC since 2012. However, several areas within the graphite code remain to be improved, specifically the addition of material property changes resulting from environmental degradation (neutron flux and oxidation). The incorporation of this data, which can significantly affect the graphite components and alter the structural integrity of the core during operation, is proving to be an important activity. How this data will be incorporated within the code and how it will be used for license applications will be critical to a number of HTR applicants in the future. These modifications to the code must take into account the unique irradiation and oxidation response of the wide spectrum of available nuclear graphite grades currently under consideration for HTR applications. Additionally, the ASME BPVC requires material property testing within the expected operational conditions of the HTR core including neutron radiation flux, elevated temperatures, and after chronic/acute oxidation of the graphite components. Currently, no standardized graphite testing methods are approved for these environmental conditions. New American Society for Testing and Materials (ASTM) standardized tests for elevated temperature testing, small sample testing, and testing after oxidation must be developed to support the requirements within the ASME code.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
DOE OSTI2026

Toward Sustainable Lithium Recovery: A Universal Hydrothermal Approach for Lithium Extraction

The rapid growth of lithium-ion battery (LIB) deployment presents critical challenges in sustainable end-of-life management and raw material recovery. Conventional pyrometallurgical and hydrometallurgical methods suffer from high energy demand, lithium loss, and complex wastewater treatment. This study established a universal, highly efficient, and sustainable hydrothermal route for lithium extraction and material recovery from various spent lithium-ion battery cathodes using 1,2,4,5-benzenetetracarboxylic acid (BTCA). The optimized process achieved over 99% lithium leaching efficiency for lithium iron phosphate (LFP) and LiNi x Mn y Co 1–x–y O 2 (NMC), with transition metal coleaching below 1%. It was also broadly applicable to lithium manganese oxide, lithium cobalt oxide, and black mass, achieving 98.5%, 98.95%, and 94.06% leaching efficiencies, respectively. The extracted lithium was directly converted into battery-grade lithium sources, while transition metals were recovered as oxides. Unreacted BTCA was efficiently regenerated and reused without degradation. Electrochemical evaluation confirmed that cathode materials synthesized with recovered lithium exhibit comparable performance to commercial products. Compared to conventional hydrometallurgy, the BTCA-based process increased revenue by over 40% and reduced greenhouse gas emissions by up to 39%. This closed-loop, chemistry-agnostic strategy offered a scalable and economically viable solution for industrial LIB recycling, enabling resource circularity and reducing dependency on primary critical materials.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
NASA NTRS1987

Soft x ray window encapsulant for HgI2 detectors

HgI2 is an excellent semiconductor material for a low energy, room temperature x-ray spectrometer. The high values of the atomic numbers for its constituent elements gives high x-ray and gamma ray stopping power. The band gap of HgI2 is significantly higher than other commonly used semiconductors. Owing to the large value band gap, the leakage current for HgI2 devices is smaller, thus allowing low noise performance. Devices fabricated from HgI2 crystals have demonstrated energy resolution sufficient to distinguish the x-ray emission from the neighboring elements on the periodic table. Also the power requirements of HgI2 are very low. These characteristics make a HgI2 spectrometer an ideal component in a satellite based detection system. Unfortunately, HgI2 crystals tend to deteriorate with time, even if protected by standard semiconductor encapsulants. This degradation ruins the performance of the device in terms of its energy resolution and pulse amplitude. The degrading mechanism is believed to be material loss occurring from below the electrodes, due to high vapor pressure of HgI2 at room temperature. To address this major obstacle to rapid expansion of HgI2 technology, a research program aimed at improving device stability by encapsulation with inert polymeric materials was carried out. The program focused specifically on optimizing the encapsulant materials and their deposition techniques. The principal objectives for this program were device encapsulation, device testing, and accelerated testing to ensure very long term stability of these high resolution sensors. A variety of encapsulants were investigated with the selection criteria based on their chemical diffusion barrier properties, mechanical stability, reactivity, and morphology of encapsulant films. The investigation covered different classes of encapsulants including solvent based encapsulants, vapor deposited encapsulants, and plasma polymerized encapsulants. A variety of characterization techniques were employed to examine their effectiveness in stabilizing HgI2 devices; these included permeability evaluation, vacuum and heat testing, scanning electron microscopy (SEM) as well as studying the detector performance of coated detectors. The plasma polymerized films appear to have entirely solved the HgI2 degradation problem. Another achievement of this program was the development of an accelerated testing technique which correlates extremely well with long term tesing.

Entine, G.↗
NASA NTRS2002

Fatigue Crack and Porosity Measurement in Composite Materials by Thermographic and Ultrasonic Methods

Many nondestructive methods exist for the detection of localized material anomalies in an otherwise good composite structure. The problem arises when the material system as a whole has degraded during service or was improperly manufactured. Porosity and intra-ply microcracking are two such conditions that in unlined composite pressure vessels can be very troublesome to detect and when linked through the thickness can be critical to mission success. These leak paths may lead to loss of pressure/propellant, increased risk of explosion and possible cryo-pumping. Research sought nondestructive methods for quantifying porosity and microcracking in composite tankage. Both thermographic and resonance ultrasound methods have been utilized with artificial neural network and statistical approaches to analyze the data. Resonant ultrasound spectroscopy provides measurements, which are sensitive to fine details in the materials character, such as micro-cracking and porosity. Here, the higher frequency (shorter wavelength) components of the signal train provide more significant interaction with the defects causing the spectral characteristics to shift toward lower amplitudes at the higher frequencies. As the density of the defects increases more interactions occur and more drastic amplitude changes are observed. From a thermal perspective, the higher the defect density the lower the through thickness thermal diffusivity will be. Utilizing a point heat source, and thermographically recording the heat profile with time, diffusivity calculations can be made which in turn can be related to the relative quality of the material. Preliminary experiments to verify the measurable effect on the resonance spectrum of the ultrasonic data to detect microcracking and for porosity detection thermographically are presented. Methods involving supervised and unsupervised artificial neural networks as well as other clustering algorithms are developed for signal identification.

Walker, James L.↗
DOE OSTI2023

Layer-Dependent Magnetism and Spin Fluctuations in Atomically Thin van der Waals Magnet CrPS 4

van der Waals (vdW) magnets, an emerging family of two-dimensional (2D) materials, have received tremendous attention due to their rich fundamental physics and significant potential for cutting-edge technological applications. In contrast to the conventional bulk counterparts, vdW magnets exhibit significant tunability of local material properties, such as stacking engineered interlayer coupling and layer-number dependent magnetic and electronic interactions, which promise to deliver previously unavailable merits to develop multifunctional microelectronic devices. As a further ingredient of this emerging topic, here we report nanoscale quantum sensing and imaging of atomically thin vdW magnet chromium thiophosphate CrPS 4 , revealing its characteristic layer-dependent 2D static magnetism and dynamic spin fluctuations. We also show a large tunneling magnetoresistance in CrPS 4 -based spin filter vdW heterostructures. Here, the excellent material stability, robust strategy against environmental degradation, in combination with tailored magnetic properties highlight the potential of CrPS 4 in developing state-of-the-art 2D spintronic devices for next-generation information technologies.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2025

Electrochemical Oxidation in Garnet-Type Solid Electrolyte by Formation of Point Defects

All-solid-state batteries hold greater promise for improving safety and energy density over conventional battery technology employing organic liquid electrolytes. One of the required features of a Li + conducting solid electrolyte is electrochemical stability, attained thermodynamically or kinetically, within the targeted operating voltage and temperature ranges. Therefore, understanding of the oxidative or reductive degradation mechanism is important to allow the design of stable solid electrolyte materials. This work contributes to building an understanding of the oxidative degradation mechanism in lithium solid electrolytes at cell operating conditions. Here, we have focused on resolving the oxidative decomposition mechanism of Al-doped lithium garnet Li 6.28 Al 0.24 La 3 Zr 2 O 12 (LLZO) as a state-of-the-art inorganic ceramic electrolyte. By combining experimental and computational analyses, we show that oxidation of LLZO occurs by simultaneous loss of oxygen and lithium from the structure, resulting in substoichiometric LLZO, at a moderate temperature (80 °C) and a high electrode potential (4.3 V vs Li/Li + ). Based on X-ray absorption and diffraction analyses, we find that the zirconium coordination shells in LLZO contract while the crystal structure experiences positive chemical strain upon electrochemical oxidation. The results from ex situ structural characterization of both the local structure and crystal symmetry are supported by a substoichiometric LLZO with lithium and oxygen vacancies, modeled by density functional theory (DFT) calculations. These chemical and structural changes in LLZO suppress effective lithium-ion conductivity by an order of magnitude. Formation of lithium and oxygen vacancies in LLZO upon electrochemical oxidation is different from prior thermodynamic predictions of phase decomposition of LLZO. The difference here is that the experiments were conducted at near-room temperature, which can hinder the kinetics of phase separation, and thus, the resultant LLZO solid electrolyte is still single-phase but substoichiometric in Li and O. In conclusion, these findings contribute an important degradation mechanism of the electrolyte, relevant for practical operational conditions of solid-state batteries.

36 MATERIALS SCIENCE↗
DOE OSTI2024

A thermodynamic perspective on electrode poisoning in solid oxide fuel cells

A critical challenge to the commercialization of clean and high-efficiency solid oxide fuel cell (SOFC) technology is the insufficient stack lifespan caused by a variety of degradation mechanisms, which are associated with cell components and chemical feedstocks. Cell components related degradation refers to thermal/chemical/electrochemical deterioration of cell materials under operating conditions, whereas the latter regards impurities in feedstocks of oxidant (air) and reductant (fuel). This article provides a thermodynamic perspective on the understanding of the impurities-induced degradation mechanisms in SOFCs. The discussion focuses on using thermodynamic analysis to elucidate poisoning mechanisms in cathodes by impurity species such as Cr, CO 2 , H 2 O, and SO 2 and in the anode by species such as S (or H 2 S), SiO 2 , and P 2 (or PH 3 ). The author hopes the presented fundamental insights can provide a theoretical foundation for searching for better technical solutions to address the critical degradation challenges.

25 ENERGY STORAGE↗
DOE OSTI2023

Determination of Thermal Damage Threshold in THz Photomixers Using Raman Spectroscopy

The increase of device lifetime and reliability of THz photomixers will play an essential role in their possible future application. Therefore, their optimal work conditions/operation range, i.e., the maximal incident optical power should be experimentally estimated. We fabricated and tested THz photomixer devices based on nitrogen-implanted GaAs integrated with a Bragg reflector. Raman spectroscopy was applied to investigate the material properties and to disclose any reversible or irreversible material changes. The results indicate that degradation effects in the photomixer structures/material could be avoided if the total optical power density does not exceed levels of about 0.7 mW/µm 2 for 100 min of operation. Furthermore, the investigations performed during 1000 min of optical exposure on the photomixer devices’ central region comprising interdigitated metal-semiconductor-metal (MSM) structures suggest a reversible “curing” mechanism if the power density level of ~0.58 mW/µm 2 is not exceeded. Long-term operation (up to 1000 h) reveals that the photomixer structures can withstand an average optical power density of up to ~0.4 mW/µm 2 without degradation when biased at 10 V. Besides the decrease of the position of the A1g (LO) Raman mode from ~291 cm -1 down to ~288 cm -1 with increasing optical power density and operation time, broad Raman modes evolve at about 210 cm -1 , which can be attributed to degradation effects in the active photomixer/MSM area. In addition, the performed carrier lifetime and photomixer experiments demonstrated that these structures generated continuous wave sub-THz radiation efficiently as long as their optimal work conditions/operation range were within the limits established by our Raman studies.

36 MATERIALS SCIENCE↗
DOE OSTI2022

Degradation in Photovoltaic Encapsulant Transmittance: Results of the Second PVQAT TG5 Artificial Weathering Study

The optical degradation of encapsulants from ultraviolet (UV) radiation has historically resulted in a significant loss in performance throughout the life of a photovoltaic (PV) module. IEC test methods have recently been developed to screen for PV encapsulants prone to loss in optical performance. The present study was performed to benchmark polymeric packaging materials relative to IEC 62788-1-4 (covering the measurement of optical transmittance) and IEC 62788-1-7 (on the durability of transmittance), provide feedback toward improvement of the methods, and develop insight regarding optical degradation. Contemporary materials were examined, including: poly(ethylene-co-vinyl acetate) (EVA), thermoplastic polyolefin (TPO), polyolefin elastomer (POE), and polyvinyl butyral (PVB) encapsulants; a poly(ethene-co-tetrafluoroethene)/poly(ethylene terephthalate) (ETFE/PET) transparent backsheet; and a polystyrene (PS) working reference material. The use of silica-, specialty-, and rolled-glass was also compared in laminated coupons. Specimen size was separately examined from 2.5 cm to 12.5 cm. Weathering was performed with a xenon source, using IEC TS 62788-7-2 methods A2, A3, A4, and A5 (chamber temperature of 55 Degrees C, 65 Degrees C, 75 Degrees C, or 85 Degrees C), respectively. Characterizations were made using a UV-VIS-NIR spectrophotometer (transmittance and reflectance, with and without an integrating sphere), a UV-VIS fluorescence spectrophotometer, a camera, and an optical microscope. Performance was analyzed, including solar weighted transmittance, yellowness index, UV cut-off wavelength, and haze (scattering). Separate Arrhenius analyses were performed to assess retention of transmittance and changes in yellowness index. The activation energy for both characteristics was found to range from 15 kJ?mol-1-80 kJ/mol-1, with an average of 48 kJ/mol-1, similar to the average of 45 kJ/mol-1 identified in the previous international PV Quality Assurance Task Force (PVQAT) Task Group 5 (TG5) study of more traditional encapsulants. The separate degradation modes of discoloration and scattering were distinguished in the encapsulants using a comprehensive spectral characterization. Based on these results, the IEC 62788-1-7 pass/fail criteria of 5% change in transmittance was confirmed to identify a known bad encapsulant.

durability↗
DOE OSTI2024

Voltage and temperature effects on low cobalt lithium-ion battery cathode degradation

Degradation of low cobalt lithium-ion cathodes was tested using a full factorial combination of upper cut-off voltage (4.0 V and 4.3 V vs. Li/Li + ) and operating temperature (25 °C and 60 °C). Half-cell batteries were analyzed with electrochemical and microstructural characterization methods. Electrochemical performance was assessed with galvanostatic cycling, cyclic voltammetry (CV), and electrochemical impedance spectroscopy (EIS) supported by distribution of relaxation times (DRT) analysis. Electrode microstructure was characterized with scanning electron microscopy (SEM), X-ray diffraction (XRD), and X-ray absorption near edge structure (XANES) imaging. Higher cut-off voltage cycling shows presence of NiO x formation, a low diffusivity rock-salt phase, in both CV and XRD data. XRD patterns confirmed that the rock-salt phase was beginning to form at the low cut-off voltage at high temperature, but in much lower intensity than at the high cut-off voltage. Higher temperature accelerates degradation processes at both voltages. Degradation factors at high temperature include NiO x formation, cathode material dissolution, and electrolyte decomposition. SEM analysis suggests that supporting phases may isolate and disconnect active material particles reducing capacity retention and battery life cycle. DRT analysis and XANES imaging show that both high temperature samples revealed a NiO x phase based on an increased diffusive impedance and a visible shift in the XANES spectra. The low cut-off voltage, high temperature sample showed a split peak and shift to lower energies indicating early formation of the NiO x phase. The diffusive impedance, which hinders intercalation and deintercalation, is driven by the formation of the NiO x phase. While primarily driven by cut-off voltage, elevated temperature also contributes to this degradation mechanism.

electrochemical impedance spectroscopy↗
DOE OSTI2024

Understanding Formation of Irradiation-Induced Defects through 4D-STEM, Electron Tomography, and WBDF-STEM

A major challenge in advancing nuclear materials for next-generation fission and proposed fusion reactors is to comprehensively understand the formation of irradiation-induced defects. Here it is essential to correlate the evolution of irradiation-induced defects and the degradation of mechanical properties, as they collectively dictate the material's lifespan and ensure nuclear safety. Scanning transmission electron microscopy (STEM) based techniques have emerged as indispensable tools for irradiation-induced defect characterization, offering high spatial resolution imaging and chemical analysis, such as electron energy loss spectroscopy (EELS) and energy dispersive X-ray spectroscopy (EDXS). These techniques have been effectively used to obtain an atomic-scale view of the defect structure. Recent advances in electron microscopy, particularly in 4D-STEM, offer detailed insight into microstructural evolution by capturing full 2D diffraction patterns at every pixel position. Using high-speed direct electron detectors, this technology generates a four-dimensional dataset, overcoming the limitations of traditional STEM imaging.

36 MATERIALS SCIENCE↗
NASA NTRS2001

Long-Term Durability of a Matrix for High-Temperature Composites Predicted

Polymer matrix composites (PMC's) are being increasingly used in applications where they are exposed for long durations to harsh environments such as elevated temperatures, moisture, oils and solvents, and thermal cycling. The exposure to these environments leads to the degradation of structures made from these materials. This also affects the useful lifetimes of these structures. Some of the more prominent aerospace applications of polymer matrix composites include engine supports and cowlings, reusable launch vehicle parts, radomes, thrust-vectoring flaps, and the thermal insulation of rocket motors. This demand has led to efforts to develop lightweight, high-strength, high-modulus materials that have upper-use temperatures over 316 C. A cooperative program involving two grants to the Massachusetts Institute of Technology and in-house work at the NASA Glenn Research Center was conducted to identify the mechanisms and the measurement of mechanical and physical properties that are necessary to formulate a mechanism-based model for predicting the lifetime of high-temperature polymer matrix composites. The polymer that was studied was PMR-15 polyimide, a leading matrix resin for use in high-temperature-resistant aerospace composite structures such as propulsion systems. The temperature range that was studied was from 125 to 316 C. The diffusion behavior of PMR-15 neat resin was characterized and modeled. Thermogravimetric analysis (TGA) was also conducted in nitrogen, oxygen, and air to provide quantitative information on thermal and oxidative degradation reactions. A new low-cost technique was developed to collect chemical degradation data for isothermal tests lasting up to 4000 hr in duration. In the temperature range studied, results indicate complex behavior that was not observed by previous TGA tests, including the presence of weight-gain reactions. These were found to be significant in the initial periods of aging from 125 to 225 C. Two types of weight loss reactions dominated at aging temperatures above 225 C. One was concentrated at the surface of the polymer and was very active at temperatures above 225 C. The second was observed to dominate in the latter stages of aging at temperatures below 260 C. This three-reaction model satisfactorily explains past findings that the degradation mechanism of PMR-15 appears to change around 316 C. It also indicates that the second weight gain mechanism is a significant factor at temperatures below 204 C. On the basis of these results, a predictive model was developed for the thermal degradation of PMR-15 at 316 C. A comparison of data generated by this model with actual experimental data is shown in the following figure.

Bowles, Kenneth J.↗
NASA NTRS1985

Mass loss of shuttle space suit orthofabric under simulated ionospheric atomic oxygen bombardment

Many polymeric materials used for thermal protection and insulation on spacecraft degrade significantly under prolonged bombardment by ionospheric atomic oxygen. The covering fabric of the multilayered shuttle space suit is composed of a loose weave of GORE-TEX fibers, Nomex and Kevlar-29, which are all polymeric materials. The complete evaluation of suit fabric degradation from ionospheric atomic oxygen is of importance in reevaluating suit lifetime and inspection procedures. The mass loss and visible physical changes of each test sample was determined. Kapton control samples and data from previous asher and flight tests were used to scale the results to reflect ionospheric conditions at about 220 km altitude. It is predicted that the orthofabric loses mass in the ionosphere at a rate of about 66% of the original orthofabric mass/yr. The outer layer of the two-layer orthofabric test samples shows few easily visible signs of degradation, even when observed at 440X. It is concluded that the orthofabric could suffer significant loss of performance after much less than a year of total exposure time, while the degradation might be undetectable in post flight visual examinations of space suits.

Miller, W. L.↗