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Search indexed NASA NTRS and DOE OSTI research on propulsion, heat transfer, battery materials and energy systems. Follow report and document links to the original sources.

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At least 91 records · Page 5

Organometallic Polymeric Conductors

For aerospace applications, the use of polymers can result in tremendous weight savings over metals. Suitable polymeric materials for some applications like EMI shielding, spacecraft grounding, and charge dissipation must combine high electrical conductivity with long-term environmental stability, good processability, and good mechanical properties. Recently, other investigators have reported hybrid films made from an electrically conductive polymer combined with insulating polymers. In all of these instances, the films were prepared by infiltrating an insulating polymer with a precursor for a conductive polymer (either polypyrrole or polythiophene), and oxidatively polymerizing the precursor in situ. The resulting composite films have good electrical conductivity, while overcoming the brittleness inherent in most conductive polymers. Many aerospace applications require a combination of properties. Thus, hybrid films made from polyimides or other engineering resins are of primary interest, but only if conductivities on the same order as those obtained with a polystyrene base could be obtained. Hence, a series of experiments was performed to optimize the conductivity of polyimide-based composite films. The polyimide base chosen for this study was Kapton. 3-MethylThiophene (3MT) was used for the conductive phase. Three processing variables were identified for producing these composite films, namely time, temperature, and oxidant concentration for the in situ oxidation. Statistically designed experiments were used to examine the effects of these variables and synergistic/interactive effects among variables on the electrical conductivity and mechanical strength of the films. Multiple linear regression analysis of the tensile data revealed that temperature and time have the greatest effect on maximum stress. The response surface of maximum stress vs. temperature and time (for oxidant concentration at 1.2 M) is shown. Conductivity of the composite films was measured for over 150 days in air at ambient temperature. The conductivity of the films dropped only half an order of magnitude in that time. Films aged under vacuum at ambient temperature diminished slightly in conductivity in the first day, but did not change thereafter. An experimental design approach will be applied to maximize the efficiency of the laboratory effort. The material properties (initial and long term) will also be monitored and assessed. The experimental results will add to the existing database for electrically conductive polymer materials. Attachments: 1) Synthesis Crystal Structure, and Polymerization of 1,2:5,6:9,10-Tribenzo-3,7,11,13-tetradehydro(14) annulene. 2) Reinvestigation of the Photocyclization of 1,4-Phenylene Bis(phenylmaleic anhydride): Preparation and Structure of (5)Helicene 5,6:9,10-Dianhydride. 3) Preparation and Structure Charecterization of a Platinum Catecholate Complex Containing Two 3-Ethynyltheophone Groups. and 4) Rigid-Rod Polymers Based on Noncoplanar 4,4'-Biphenyldiamines: A Review of Polymer Properties vs Configuration of Diamines.

Youngs, Wiley J.↗

Multi-scale experimental study of creep-fatigue failure initiation in a 709 Stainless Steel alloy using high resolution digital image correlation. Final report

This report discusses the efforts made towards the multi-scale study of the creep-fatigue response of stainless steel 709. Multiple experimental techniques, including digital image correlation (DIC) and electron backscatter diffraction (EBSD), were used in assessing the evolution of damage accumulation during fatigue, creep-fatigue, and thermomechanical fatigue of alloy 709. The role of microstructural features, hold times, temperature, and loading profiles were quantified and the interchangeability of temperature and time was investigated. Finally, a thermomechanical fatigue model was shown to predict well the failure of samples with varying loading profiles. Results indicate that strain accumulation in 709 steel happens primarily near grain boundaries (GBs) with the strains around GBs being inversely proportional to their measured residual burgers vector. Furthermore, hot-spots for strain accumulation were shown to be the locations of eventual microcrack nucleation. The introduction of hold times to the periodic loading cycle increases the damage accumulation rate and thus shortens the fatigue life of samples–this was true for both room temperature and high temperature. Thermomechanical cycling was shown to have little effect on the end life of samples, with the damage accumulation rate for in-phase and out-of-phase cycling being similar to isothermal fatigue. The interchangeability of time and temperature was shown to be possible within the studied load, time, and temperature ranges, since deformation mechanisms driving strain accumulation did not change with temperature (up to 650°C). The Neu-Sehitoglu thermomechanical fatigue model, with constants obtained from the literature and in part from our experimental results, was applied to predict failure of isothermal creep-fatigue samples. The main objectives of this work were to:(a) Perform high-resolution digital image correlation measurements (HiDIC) for alloy 709; (b) Quantify and assess damage accumulation at the microstructure under fatigue, TMF, and creep-fatigue conditions of 709; (c) Study of the role of hold times, i.e., adding a creep component, to: Room temperature cycling, High temperature cycling, Failure; (d) Study the mechanisms of thermomechanical fatigue in this alloy; (e) Investigate the existence of a time-temperature interchangeability criterion to aid in accelerated creep-fatigue testing; (f) Establish the validity of a combined creep-fatigue model for life prediction for 709. This report is structured with each subsequent section detailing the efforts, results, and conclusions related to each of the objectives described, mostly in chronological order.

36 MATERIALS SCIENCE↗

The accelerated characterization of viscoelastic composite materials

Necessary fundamentals relative to composite materials and viscoelasticity are reviewed. The accelerated characterization techniques of time temperature superposition and time temperature stress superposition are described. An experimental procedure for applying the latter to composites is given along with results obtained on a particular T300/934 graphite/epoxy. The accelerated characterization predictions are found in good agreement with actual long term tests. A postcuring phenomenon is discussed that necessitates thermal conditioning of the specimen prior to testing. A closely related phenomenon of physical aging is described as well as the effect of each on the glass transition temperature and strength. Creep rupture results are provided for a variety of geometries and temperatures for T300/934 graphite/epoxy. The results are found to compare reasonably with a modified kinetic rate theory.

Griffith, W. I.↗

White Paper: Research & Development for the Time at Temperature Approach

Recent advancements in nuclear power research are greatly improving reactor safety and performance through the development of Accident Tolerant Fuel (ATF) and Low-Enriched Uranium Plus (LEU+). These innovations can address Departure from Nucleate Boiling (DNB) margins, which are vital for reactor safety. DNB happens when the coolant switches to film boiling, significantly decreasing heat transfer and posing a risk of fuel cladding failure. The U.S. Nuclear Regulatory Commission (NRC) employs conservative DNB criteria, which can potentially restrict the operational flexibility and efficiency of reactors. The Time at Temperature (TaT) approach could provide a more detailed and adaptable operational guideline by establishing acceptable time-temperature limits, accounting for the duration a material can withstand elevated temperatures without losing its integrity. This method allows reactors to operate more efficiently and safely, offering additional operational margins, faster power adjustments, and improved fuel cycle economics. TaT criteria allow for higher power levels and more flexible responses to operational transients, particularly applicable for anticipated operational occurrences (AOOs) that result in short durations of post-DNB conditions. It enhances plant operational flexibility, allows faster startup times, and enables quicker power level adjustments, optimizing fuel loading patterns and improving fuel cycle economics. Implementing TaT limits reduces core design constraints, lowers fuel usage, and reduces costs, essential for the long-term sustainability of Light Water Reactors (LWRs). TaT maximizes the use of advanced fuel technologies like ATF and LEU+, further enhancing their economic and environmental benefits. To apply the TaT approach in existing LWRs, collaborative research activities among various DOE-sponsored programs are essential. These efforts should incorporate fuel experiments, physics-based high-fidelity modeling, ML-based surrogate modeling, and optimization techniques. This whitepaper proposes four research and development areas: 1) Investigation of the feasibility of new operations of LWR with updated safety limits; 2) Assessment of reactor operation limits through uncertainty reduction; 3) Evaluation of power uprate in virtual environment; and 4) Lattice and reactor core design for power uprate. Each area includes why this research is in need and a suggested scope of work. These comprehensive research areas ensure practical and beneficial advancements for existing reactors, translating innovations in nuclear fuel and cladding technology into improved reactor performance and safety.

42 - ENGINEERING↗

Accelerated Creep Testing of Inconel 718 Using the Stepped Isostress Method (SSM)

This paper demonstrates the stepped isostress method (SSM); an accelerated creep test (ACT) for the rapid assessment of metallic materials. The SSM test is based on the time-temperature-stress superposition principle (TTSSP) where temperature and/or stress are step increased to accelerate the time-to-rupture. The SSM test has proven successful for the ACT of polymers and polymeric composites but has yet to be proven for metallic materials. In this study, new test matrix design rules for the SSM of metals are established based on deformation mechanism, time-temperature transformation, and time-temperature precipitation maps. A test matrix of SSM and conventional creep tests (CCTs) are executed for alloy Inconel 718 at 750°C (1382°F) with stress levels ranging from 100 to 350 MPa. Validation CCT data is gathered from the Japan National Institute of Material Science (NIMS). Material constants for the Sine-hyperbolic (Sinh) constitutive model are calibrated using the SSM data and employed to predict the conventional creep response. Here, when blindly compared to the CCT data, the SSM calibrated Sinh model can accurately predict the conventional creep response across logarithmic decades and thus accelerate the capture of conventional creep data. Fractography indicates ductile fracture by transgranular microvoid coalescence (TMVC) with the same fracture mode observed in both SSM and CCT specimens. Creep cavitation is indicated by the population, smoothness, and size of microvoids.

36 MATERIALS SCIENCE↗

Effect of post cure time and temperature on the properties of two phenolic-fiber composites

Some effects of post-cure time and temperature on the physicomechanical properties of a phenolic-asbestos and a phenolic-glass composite are studied. The molding and post-curing procedures are discussed along with physical and mechanical test results. It is found that the specific gravity of the panels tested decreased slightly but the hardness always increased with post cure, and that the mechanical properties had different patterns of response to increasing post-cure time and temperature. For tensile properties, strength decreased, modulus increased, and elongation at break exhibited little change. In general, the phenolic-asbestos showed more positive response to post cure than did the phenolic-glass. Mold venting is found to impart better properties to the composites concerned.

Lucy, M. H.↗

Quantifying Properties for a Mechanistic, Predictive Understanding of Aqueous Impact on Aging of Medium and Low Voltage AC and DC Cabling in Nuclear Power Plants

To address the gap in knowledge in understanding degradation in relevant service conditions, this project aimed to develop a mechanistic, predictive model of medium and low voltage cable failure based on the primary environmental degradation parameters of aqueous immersion time, temperature, and the oxidation extent. To do so, we took a two-fold approach toward evaluating degradation as related to the aqueous condition. First, we evaluated the chemical, mechanical, and electrical properties of polymers that comprise the cabling insulation under varied aqueous conditions at different temperatures. Secondly, we evaluated the performance of insulation materials under similar accelerated aging conditions in addition to the dielectric breakdown of the cabling under submersion conditions. Thermal oxidation and immersion of LDPE thin films were done using a Parr vessel and the extent of oxidation was monitored using the carbonyl index from ATR-FTIR spectrum, a ratio quantifying the carbonyl functionality produced on the LDPE film surface. Increasing the temperature, oxidation time, and oxygen pressure increased the water-vapor permeability and the carbonyl content. Thermogravimetric analysis of the films confirmed that there is indeed an initial weight loss of the smaller molecular weight molecules and volatiles. At higher temperatures, there is a secondary mass loss. Up to 70°C, the mass loss curves were similar until 80°C, when the aged films decreased at a much greater rate with respect to increasing temperature. This was seen in the 10, 50, 90% weight loss temperatures. The mechanical properties of sheet PP and HDPE as well as injection molded LDPE, HDPE, HDPP dog bones were plotted with respect to the time spent in the Parr vessel during thermal oxidation. For the sheet PP and HDPE, the UTS and the modulus of elasticity decreased while the elongation increased. The injection-molded LDPE, HDPE, and HDPP dog bones experienced a similar trend where the changes in the properties were within experimental uncertainty. This analysis of LDPE in dry and immersive oxygen-rich environments is an important baseline for future experiments looking at other degradation mechanisms. A predictive aging model for low-density polyethylene insulative cable housings was developed. This model revealed a combination of physical and chemical processes which lead to an increase in permeability and a decrease in strength of the insulator. In creating this predictive model, a gap of knowledge in the literature was revealed in two areas: understanding how the crystallinity of a polymer changes with time and visualizing the predicted pores formed through the insulator which leads to failure. Developing and using an adapted ATR-FTIR method, crystallinity was monitored and compared to bulk crystallinity found via DSC. Inhomogeneity in crystallinity changes were observed but the FTIR method but was found to be less reliable. Pore visualization was found utilizing electrical impedance spectroscopy saturated aged polyethylene films with synthesized citrate-capped gold nanoparticles, and chloroauric acid precursor. results indicate a decreasing impedance of the polyethylene films caused by the transport of ions through the film. SEM imaging was then performed for elemental analysis of the films and counter electrodes for the presence of ions. Chloride and gold ions were detected; however, no nanoparticles were found. This gives an estimated pore size of at least 0.3 nm through the aged film. Cyclic submergence of polyethylene and polypropylene in aqueous solutions of copper sulfate and Harrison’s solution were examined. It was discovered that aging in these mixed conditions and at 90°C did cause a small, yet significant increase to tensile strength for both unaged polyethylene and polypropylene. The PE and PP in cycled and submerged conditions did not have tensile strengths significantly different from dry-aged after 16 weeks. For both solutions, it was determined that capacitance increases with both water tree depth and cable temperature and is relatively independent of changing water tree AR. As for resistance, there is no apparent change between depth percentages of 10 and 80 for both solutions. This is because the water tree has not yet entered the conductor and thus there is no shorting current flowing through the tree yet. Between 80 and 100% water tree depth, it is observed that for both solutions there is a rapid decrease in resistance because the tree is now impacting the conductor shield and allowing shorting current to flow through it. The relationship between resistance and temperature was found to be inversed. As temperature increases, resistance decreases for both water tree solutions with distilled water having the most apparent difference across the range of temperatures simulated. With regards to water tree AR, resistance was found to be relatively independent at depth percentages of 10, 50, and 70, but there was some relationship at 100% depth for both solutions. At this depth, as water tree AR increased, resistance was found to also increase. Through the examination of voltage and electric field distribution plots, it was confirmed for EPR cables that increasing water tree depth leads to increasing distortion. The increase in shorting current at 100% depth for aqueous copper sulfate compared to distilled water was also visualized. Lastly, the relationship between shorting current and temperature for narrow water trees was visualized and validated using the distribution plots. This study has led to a better understanding of the effect of cable temperature, water tree solution, and geometry of the tree region on cable degradation. Furthermore, this study has documented simulation results of water tree degradation in EPR MV cables, which had been previously lacking in information. Future work in this area will add frequency into the mix and examine what effect it has on the rate of cable degradation as a result of water treeing. To compliment the work being carried by UMD on different polymer chemistries, harvested medium voltage (MV) cables were selected for accelerated aging study at ORNL. These medium voltage cables are representative of the vintages and materials that are currently in use at existing nuclear power plants (NPPs). These cables were immersed in water at 90°C and energized for a period of two years at elevated voltage. Partial discharge was measured during this period of time to track potential degradation. Unfortunately, due to the absence of failure, the extent of integration between the UMD techniques and the harvested MV insulation was limited. However, based on the findings and from the UMD research in the previous sections on polyethylene and polypropylene, follow-on characterization for harvested MV cable insulation should focus on sample preparation to take advantage of the UMD techniques to better understand mechanistic degradation in MV cable insulations. This would include: 1.) Utilization of solutions and impedance measurement insulation to track permeability in harvested and accelerated aging insulation samples, 2.) Adaptation of gold nanoparticle synthesis for electrical impedance spectroscopy with supporting SEM characterization to study pore formation in harvested and accelerated aged insulation samples, & 3.) ATR-FTIR crystallinity with multiple temperature dependent harvested MV cable insulation under different air and submerged accelerated aging. In addition, low voltage dielectric spectroscopy and high voltage dissipation factor, tan δ, could be implemented as a condition monitoring tool for harvested MV cable insulation in submerged environments.

24 POWER TRANSMISSION AND DISTRIBUTION↗

Time Temperature-Precipitation Behavior in An Al-Cu-Li Alloy 2195

Al-Cu-Li alloy 2195, with its combination of good cryogenic properties, low density, and high modulus, has been selected by NASA to be the main structural alloy of the Super Light Weight Tank (SLWT) for the Space Shuttle. Alloy 2195 is strengthened by an aging treatment that precipitates a particular precipitate, labeled as T1(Al2CuLi). Other phases, such as GP zone, (theta)', (theta)", theta, (delta)', S' are also present in this alloy when artificially aged. Cryogenic strength and fracture toughness are critical to the -SLWT application, since the SLWT will house liquid oxygen and hydrogen. Motivation for the Time-Temperature-Precipitation (TTP) study at lower temperature (lower than 350 F) comes in part from a recent study by Chen, The study found that the cryogenic fracture toughness of alloy 2195 is greatly influenced by the phases present in the matrix and subgrain boundaries. Therefore, the understanding of TTP behavior can help develop a guideline to select appropriate heat treatment conditions for the desirable applications. The study of TTP behavior at higher temperature (400 to 1000 F) was prompted by the fact that the SLWT requires a welded construction. Heat conduction from the weld pool affects the microstructure in the heat-affected zone (HAZ), which leads to changes in the mechanical properties. Furthermore, the SLWT may need repair welding for more than one time and any additional thermal cycles will increase precipitate instability and promote phase transformation. As a result considerable changes in HAZ microstructure and mechanical properties are expected during the construction of the SLWT. Therefore, the TTP diagrams can serve to understand the thermal history of the alloy by analyzing the welded microstructure. In the case welding, the effects of thermal cycles on the microstructure and mechanical properties can be predicted with the aid of the TTP diagrams. The 2195 alloy (nominally Al + 4 pct Cu + 1 pct Li + 0.3 pct Ag + 0.3 pct Mg + 0.1 pct Zr) used in this study was received in the form of 1.7 inch thick rolled plates. In brief goal of this study is to develop TTR diagram for the solutiontreated and stretched alloy 2195 from which the precipitation sequence at any service or aging conditions can be preducted.A subgrain boundary TTR diagram is also presented since precipitations at subgrain boundary can control and/or modify a wide veriety of material properties, such as cryogenic fracture toughness.

Chen, P. S.↗

A simplified model for glass formation

A simplified model of glass formation based on the formal theory of transformation kinetics is presented, which describes the critical cooling rates implied by the occurrence of glassy or partly crystalline bodies. In addition, an approach based on the nose of the time-temperature-transformation (TTT) curve as an extremum in temperature and time has provided a relatively simple relation between the activation energy for viscous flow in the undercooled region and the temperature of the nose of the TTT curve. Using this relation together with the simplified model, it now seems possible to predict cooling rates using only the liquidus temperature, glass transition temperature, and heat of fusion.

Uhlmann, D. R.↗

Direct Conversion of Biomass Carbohydrates to Platform Chemicals: 5-Hydroxymethylfurfural (HMF) and Furfural

5-hydroxymethylfurfural (HMF) and furfural are promising platform molecules which can be converted to fuel intermediates and hydrocarbon fuels. Herein, one-step, direct conversion of the carbohydrates in never treated biomass to HMF and furfural in a microwave reactor was investigated. The influence of reaction temperature, time, feedstock, addition of Lewis and Bronsted acids, solvent and solvent to aqueous ratio were studied to find the optimum process conditions to maximize the yields of furfurals. The reaction conditions of 200 degrees C for 5 min with 33 mM HCl and 8 mM AlCl 3 using a dioxane/water (4:1) miscible solvent system were found to be the most conducive for direct dehydration of the glucan and hemicelluloses present in untreated poplar wood to furfural and HMF in yields of 91 and 69%, respectively. Furfural could be easily produced in yields greater than 80%, and once formed, it was found to be stable under the various process conditions explored. In contrast, HMF yields varied with both reaction time and temperature, as it readily underwent rehydration to levulinic acid in yields approaching 25-30% at increased reaction severity. The additions of both Bronsted (HCl) and Lewis (AlCl 3 ) acids in catalytic amounts, i.e., 33 and 8 mM, respectively, were required to maximize the yield of furfurals. Reactions were also performed on other feedstocks (corn stover, switchgrass, loblolly pine, and pure cellulose) to investigate the effect of feedstock type on furfurals yields. Results showed that HMF and furfural yields were primarily dependent on hexosan and pentosan loading regardless of the type of feedstock. In addition, biomass physical features, such as crystallinity or the presence of other biomass constituents, such as lignin, had little influence on furfurals yields.

09 BIOMASS FUELS↗

Thermal Aging Effects on the Yield and Tensile Strength of 9Cr-1Mo-V (Grade 91)

The long-term exposure of 9Cr-1Mo-V (Grade 91) steel to elevated temperature can have a significant effect on reducing its yield and tensile strength. The yield and tensile strength changes, in turn, have potential implications to the assurance of the integrity of components constructed with this material over their design or intended lifetime. The ASME Boiler & Pressure Vessel Code (BPVC), Section III, Division 5 (III-5, high temperature reactors) provides tabulated reduction factors for Grade 91 yield and tensile strength as a function of exposure temperature and time up to 300,000 h. ASME BPVC III-5 s intent to extend these factors to an exposure duration of 500,000 h, the lack of available historic information to support the existing factors, and the recent development of a physics-based prediction model for ASME BPVC application are prime motivation for this study. This work describes results of the conventional time-temperature Hollomon–Jaffe parameter, strength reduction ratio prediction method using an updated, extensive Grade 91 unaged and related aged material strength database. The method, previously used by Oak Ridge National Laboratory in its evaluation of Grade 91 and likely used in development of the existing BPVC III-5 reduction factors, provides strength reduction ratio predictions useful for general component fitness-for-service assessments and for computing BPVC III-5 reduction factors as defined. Specific reduction factors to 500,000 h at 650 °C applicable to ASME BPVC III-5 are computed from the strength reduction ratios.

36 MATERIALS SCIENCE↗

Role of Hf and Zr in the hydrogen embrittlement of Ta and Cb alloys

The hydrogen embrittlement of aged T-111 and similar Ta and Cb alloys is characterized and the mechanisms believed responsible for the increased sensitivity of T-111 to low temperature hydrogen embrittlement after aging for 1000 hours or longer near 1040 C are described. A total of eight Ta base alloys and two Cb base alloys were investigated. The effects of pre-age annealing temperature, aging time, temperature and environment, and alloy composition on the susceptibility to hydrogen embrittlement were investigated. The primary method of determining the effects of these variables on the ductility of T-111 was by bend testing at 25 and -196 C. Fractured specimens were examined by the scanning electron microscope, electron microprobe, metallography and X-ray diffration.

Stephens, J. R.↗

Role of HF and Zr in the hydrogen embrittlement of Ta and Cb alloys

An attempt is made to characterize the hydrogen embrittlement of aged T-111 and similar Ta and Cb alloys and to describe the mechanisms believed responsible for the increased sensitivity of T-111 to low temperature hydrogen embrittlement after aging for 1000 hr or longer near 1040 C. A total of eight Ta-base alloys and two Cb-base alloys were investigated. The effects of pre-age annealing temperature, aging time, temperature and environment, and alloy composition on the susceptibility to hydrogen embrittlement were investigated. The primary method of determining the effects of these variables on the ductility of T-111 was by bend testing at 25 and -196 C. Fractured specimens were examined by the scanning electron microscope, electron microprobe, metallography, and X-ray diffraction.

Stephens, J. R.↗

Crystallization kinetics, viscous flow, and thermal history of lunar breccia 67975

The maximum crystal growth rate for the 67975 matrix composition, about 0.00073 cm/min, was found to occur at about 990 C (undercooling 220 C). The Shaw (1972) model and, to a slightly lesser extent, the Bottinga and Weill (1972) model indicate the variation of viscosity with temperature. Time-temperature-transformation and continuous cooling curves were constructed from the measured crystal growth rates and viscosities and used to estimate the cooling rate required to form bodies with the degree of crystallinity observed in the matrix of the breccia. It is estimated on the basis of kinetic analysis that the 67975 breccia cooled at a rate of about 0.06 C/min over the temperature range below the liquidus. Heat flow analyses indicate that the 67975 breccia did not cool in the size of the lunar sample but as part of a much larger body. Viscous singering as well as cooling of a melt-clast mixture are investigated.

Uhlmann, D. R.↗