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NASA NTRS1986

Beta Silicon Nitride Whiskers

Process for growing fibrous beta silicon nitride helps meet potentially great demand for silicon nitride ceramics. Ceramics have high tensile strength and resistance to thermal shock, which make them attractive choice for high-temperature engine parts. Process forms whiskers of strong, stable, heatresistant material. Whiskers expected to find application as reinforcement in composite silicon nitride ceramic parts. Corklike material useful in present form for thermal barrier tiles. Process forms whiskers of strong, stable, heat-resistant material.

Holliday, R. J.↗

NASA NTRSDate not supplied

NASA's Composite Overwrap Lessons Learned on 40k Thrust Chamber Assemblies

Filament wound carbon fiber/polymer composite overwraps combined with additively manufactured (AM) copper alloy combustion chambers are a critical part of NASA’s Rapid Analysis and Manufacturing Propulsion Technology (RAMPT) project. The composite overwrap is a high strength-to-weight material and allows for significant weight reduction of the high-pressure thrust chamber assembly, reduction of overall cost, and reduced fabrication time while offering structural robustness. Integrated AM/composite overwrap chamber assemblies using 2,000 lbf (2k) and 7,000 lbf (7k) thrust were successfully hot fire tested at NASA Marshall Space Flight Center (MSFC). These assemblies allowed the team to learn lessons related to the design, analysis, and manufacturing of these integrated assemblies. A final goal of the RAMPT project is to design and test a 40,000 lbf (40k) thrust chamber assembly. The40k chamber presented the team several new challenges including an integral inlet port in the main body of the composite overwrap. Through multiple iterations of manufacturing techniques, varied materials, and Non-Destructive Evaluations (NDE), many lessons were learned to obtain a final design solution that would not only allow for the interrupted port inlet but also allow for sufficient material margins for the most critically stressed part of the chamber. This paper will cover the manufacturing techniques exploring fabric designs to help subsidize the coverage in the areas left bare by the inlet port during the filament winding process and custom tooling needed for the final full chamber processing. The original material choice of bismaleimide (BMI) 5250-4 from the 7k chamber performed well for the extreme environment of hot fire testing but proved to be difficult with the increased scale and interrupted port design of the 40kchamber. Discussion in this paper will cover these changes, including evaluation of the design, comparison to the prior 2k and 7k designs, and show the final hardware that will be tested. One primary goal of this work and RAMPT project is to provide this development process and data to industry for infusion into future engine designs.

Filament Wound↗

NASA NTRS1995

Probabilistic material strength degradation model for Inconel 718 components subjected to high temperature, high-cycle and low-cycle mechanical fatigue, creep and thermal fatigue effects

This report presents the results of both the fifth and sixth year effort of a research program conducted for NASA-LeRC by The University of Texas at San Antonio (UTSA). The research included on-going development of methodology for a probabilistic material strength degradation model. The probabilistic model, in the form of a postulated randomized multifactor equation, provides for quantification of uncertainty in the lifetime material strength of aerospace propulsion system components subjected to a number of diverse random effects. This model is embodied in the computer program entitled PROMISS, which can include up to eighteen different effects. Presently, the model includes five effects that typically reduce lifetime strength: high temperature, high-cycle mechanical fatigue, low-cycle mechanical fatigue, creep and thermal fatigue. Statistical analysis was conducted on experimental Inconel 718 data obtained from the open literature. This analysis provided regression parameters for use as the model's empirical material constants, thus calibrating the model specifically for Inconel 718. Model calibration was carried out for five variables, namely, high temperature, high-cycle and low-cycle mechanical fatigue, creep and thermal fatigue. Methodology to estimate standard deviations of these material constants for input into the probabilistic material strength model was developed. Using an updated version of PROMISS, entitled PROMISS93, a sensitivity study for the combined effects of high-cycle mechanical fatigue, creep and thermal fatigue was performed. Then using the current version of PROMISS, entitled PROMISS94, a second sensitivity study including the effect of low-cycle mechanical fatigue, as well as, the three previous effects was performed. Results, in the form of cumulative distribution functions, illustrated the sensitivity of lifetime strength to any current value of an effect. In addition, verification studies comparing a combination of high-cycle mechanical fatigue and high temperature effects by model to the combination by experiment were conducted. Thus, for Inconel 718, the basic model assumption of independence between effects was evaluated. Results from this limited verification study strongly supported this assumption.

Bast, Callie C.↗

NASA NTRS1986

Determination of band oscillator strengths of atmospheric molecules from high resolution vacuum ultraviolet cross section measurements

An account is given of progress in work on (1) the determination of band oscillator strengths of the Schumann-Runge absorption bands of (16)O2 and (18)O2 from cross section measurements conducted at 79 K; (2) the determination of the absolute absorption cross section of the Schumann-Runge bands of (16)O(18)O from optical depth measurements performed on mixtures of (16)O2, (18)O2 and (16)O(18)O at 79K; and (3) the influence of Schumann-Runge linewing contributions on the determination of the Herzberg continuum absorption cross section of (16)O2 in the wavelength region 194 to 204 nm. The experimental investigations are effected at high resolution with a 6.65 m scanning spectrometer which is, by virtue of its small instrumental width (EWHM = 0.0013 nm), uniquely suitable for cross section measurements of molecular bands with discrete rotational structure. Absolute cross sections, which are independent of the instrumental function and from which band oscillator strengths are directly determined, are measured for the absorption bands that are most predissociated. Such measurements are needed for (1) accurate calculations of the stratospheric production of atomic oxygen and heavy ozone formed following the photopredissociation of (18)O(16)O by solar radiation penetrating between the absorption lines of (16)O2; (2) elucidation of the mechanism of predissociation of the upper state of the Schumann-Runge bands; and (3) determination of the true shape of the Herzberg continuum cross section.

Parkinson, W. H.↗

DOE OSTI2020

Unraveling the dislocation–precipitate interactions in high-entropy alloys

The precipitates play a significant role in not only enhancing the strength, but also maintaining the high toughness in alloys. However, the interactions of the nanoscale precipitates with dislocations in the high entropy alloys (HEAs) are difficult to observe directly by in-situ TEM experiments due to the limits of the resolution and time. Here, using atomic simulations we report the synergistic strengthening of the coherent precipitate and atomic-scale lattice distortion in the HEAs at cryogenic/elevated temperatures. The effects of temperature, chemical disorder, precipitate spacing, precipitate size, elemental segregation, and dislocation-cutting number on the critical stress for the dislocation to overcome a row of precipitates are studied. A random stacking fault energy landscape along the slip plane, the lattice distortion at different temperatures, and the interface/surface energy at various crystallographic orientations are obtained. Compared with the traditional metals and alloys, HEAs have the severe atomic-scale lattice distortions to generate the local high tensile/compressive stress fields. This complex stress causes the dislocation line to bend, and thus improves the dislocation slip resistance, resulting in the strong solid-solution strengthening. The stacking fault strengthening induced by the obvious difference of the stacking fault energies between the HEA matrix and precipitate (within the inner of the HEA matrix), and the formation of the antiphase domain boundary contribute to the high strength. The precipitate embedded by the solute atoms produces the strong lattice distortion to enhance the dislocation slip resistance at high temperatures. Hence, the current results provide the mechanistic insight into the phenomenon that the coherent precipitate combined with the severe atomic-scale lattice distortion can enhance the strength at cryogenic/elevated temperatures to further broaden the scope of applications of advanced HEAs.

36 MATERIALS SCIENCE↗

DOE OSTI2022

Dielectric strength of noble and quenched gases for high pressure time projection chambers

Abstract Dielectric breakdown strength is one of the critical performance metrics for pure gases and gas mixtures used in large, high pressure gas time projection chambers. In this paper we experimentally study dielectric breakdown strengths of several important time projection chamber working gases and gas-phase insulators over the pressure range 100 mbar to 10 bar, and gap sizes ranging from 0.1 to 10 mm. Gases characterized include argon, xenon, CO $$_2$$ 2 , CF $$_4$$ 4 , and mixtures 90-10 argon-CH $$_4$$ 4 , 90-10 argon-CO $$_2$$ 2 and 99-1 argon-CF $$_4$$ 4 . We develop a theoretical model for high voltage breakdown based on microphysical simulations that use electron swarm Monte Carlo results as input to Townsend- and Meek-like discharge criteria. This model is shown to be highly predictive at high pressure, out-performing traditional Paschen–Townsend and Meek–Raether models significantly. At lower pressure-times-distance, the Townsend-like model is an excellent description for noble gases whereas the Meek-like model provides a highly accurate prediction for insulating gases.

73 NUCLEAR PHYSICS AND RADIATION PHYSICS↗

NASA NTRS1990

Reinforcements: The key to high performance composite materials

Better high temperature fibers are the key to high performance, light weight composite materials. However, current U.S. and Japanese fibers still have inadequate high temperature strength, creep resistance, oxidation resistance, modulus, stability, and thermal expansion match with some of the high temperature matrices being considered for future aerospace applications. In response to this clear deficiency, both countries have research and development activities underway. Once successful fibers are identified, their production will need to be taken from laboratory scale to pilot plant scale. In such efforts it can be anticipated that the Japanese decisions will be based on longer term criteria than those applied in the U.S. Since the initial markets will be small, short term financial criteria may adversely minimize the number and strength of U.S. aerospace materials suppliers to well into the 21st century. This situation can only be compounded by the Japanese interests in learning to make commercial products with existing materials so that when the required advanced fibers eventually do arrive, their manufacturing skills will be developed.

Grisaffe, Salvatore J.↗

DOE OSTI2025

Investigation of MgO additives on microstructure and properties of thin LLZO electrolytes for all-solid-state batteries

To realize high-energy density lithium lanthanum zirconate (LLZO)-based solid-state batteries (SSB), LLZO electrolytes should be fabricated with low thickness and high mechanical strength. An effective strategy for strengthening ceramic materials is to use additives. Here, we employed MgO nanopowders and fibers as additives for the thin LLZO electrolyte in order to improve the mechanical strength. The microstructure, mechanical properties, and electrochemical properties are characterized to investigate the effects of adding MgO and sintering time. The MgO remains at grain boundaries after sintering, making the microstructure of LLZO fine and uniform. The mechanical strength of the MgO-added LLZO was enhanced by more than 60% while maintaining high ionic conductivity (1 × 10 -4 S cm -1 ) at room temperature. Li symmetric cells using the MgO fiber–LLZO and MgO powder–LLZO exhibit 2 and 3 times higher critical current density (CCD) than those of pure LLZO, and a solid-state full cell exhibits stable cycling performance. Further, these results demonstrate that the use of MgO nanopowder or fiber as an additive for thin LLZO is beneficial for high-current density cycling, by improving mechanical properties and microstructure.

25 ENERGY STORAGE↗

DOE OSTI2021

Mechanical, corrosion, and wear properties of biomedical Ti–Zr–Nb–Ta–Mo high entropy alloys

The microstructures, mechanical, corrosion, and wear behaviors of the Ti x ZrNbTaMo (x = 0.5, 1, 1.5, and 2, molar ratio) high entropy alloys (HEAs) were studied in this work. It was found that the Ti–Zr–Nb–Ta–Mo HEAs showed a dendrite structure with two body-centered-cubic (BCC) solid solution phases. The Ti 0.5 ZrNbTaMo HEA exhibited a high hardness of about 500 HV, high compressive strength approaching 2,600 MPa, and large plastic strain of over 30%. Furthermore, the highly-protective oxide films formed on the surface of Ti–Zr–Nb–Ta–Mo HEAs in the phosphate buffer saline (PBS) solution, which resulted in the high corrosion resistance of the HEAs. The Ti–Zr–Nb–Ta–Mo HEAs exhibited the greater dry- and wet-wear resistance than that of the traditional biomedical Ti6Al4V alloy. The results also indicated that with the decrease in the Ti content, the wear resistance of the Ti–Zr–Nb–Ta–Mo HEAs in the PBS solution improved. Finally, the Ti 0.5 ZrNbTaMo alloy presented the highest corrosive wear resistance among the four HEAs owing to its combination of good mechanical properties and high chemical stability.

36 MATERIALS SCIENCE↗

NASA NTRS1988

Slurry-pressing consolidation of silicon nitride

A baseline slurry-pressing method for a silicon nitride material is developed. The Si3N4 composition contained 5.8 wt percent SiO2 and 6.4 wt percent Y2O3. Slurry-pressing variables included volume percent solids, application of ultrasonic energy, and pH. Twenty vol percent slurry-pressed material was approximately 11 percent stronger than both 30 vol percent slurry-pressed and dry-pressed materials. The Student's t-test showed the difference to be significant at the 99 percent confidence level. Twenty volume percent (300 h) slurry-pressed test bars exhibited strengths as high as 980 MPa. Large, columnar beta-Si3N4 grains caused failure in the highest strength specimens. The improved strength correlated with better structural uniformity as determined by radiography, optical microscopy, and image analysis.

Sanders, William A.↗

NASA NTRS1989

Slurry-pressing consolidation of silicon nitride

Sanders, William A.↗

NASA NTRS1992

Aluminum 2219-T87 and 5456-H116 - A comparative study of spacecraft wall materials in dual-wall structures under hypervelocity impact

All earth-orbiting spacecraft are susceptible to high-speed impacts by pieces of orbital debris. To prevent mission failure and possibly loss of life, protection against perforation by high-speed orbital debris particles must be included in the spacecraft design. Although any number of materials can be used to manufacture perforation-resistant structures, aluminum is often used in such systems because of its relatively high strength-to-weight ratio. This paper presents the results of a study in which the high speed impact response characteristics of dual-wall structures made from two different aluminum alloys were analyzed to determine which alloy would be more suitable for use in a perforation-resistant dual-wall structural system that is to be exposed to the orbital debris environment. Impact response characteristics were obtained numerically and experimentally. At impact speeds below 7 km/s, it was found that the two aluminum alloys considered contributed similar levels of perforation resistance; at speeds in excess of 7 km/s, aluminum 2219-T87 was superior to aluminum 5546-H116 in preventing perforation of dual-wall structural systems.

Schonberg, William P.↗

DOE OSTI2020

Determining Compression Characteristics of Honeycomb Material - 19674

The objective is to determine compression test characteristics of stainless steel honeycomb material to be able to represent honeycomb structures accurately in analytical models used to simulate hypothetical accident scenarios of shipping packages. Honeycomb is a material used primary in the aerospace industry due to its high strength-to-weight ratio. Because it doesn't have a shelf life and can withstand high heats, it is an excellent candidate for a structural material in package designs. Honeycomb has orthotropic material properties. The honeycomb currently being evaluated is made of metal ribbons spot welded together to form hexagon pattern between metal plates. The hexagon ribbons are brazed to the metal plates. The complexity of the honeycomb significantly lengthens the simulation time, which is further complicated when the brazing, welding, and imperfections of the material is considered. This means to affectively represent the honeycomb in simulation programs, such as Abaqus, the material needs to be approximated as a uniform orthotropic material. This requires material properties in each of the three directions, T, W, and L. The T direction is defined as the 'strong' direction, perpendicular to the honeycomb sheet. The L direction is parallel the ribbon and the W direction is perpendicular to the ribbon. Honeycomb has 3 different compression stages. Stage 1 is the initial compression where the honeycomb maintains its structural integrity and does not permanently deform from loads from normal operations. Stage 2 is when the initial buckling causes irreversible damage to the honeycomb. Stage 2 is the one we are most interested in because it absorbs the most energy from a hypothetical accident scenario. During Stage 2, the honeycomb fails layer-by-layer, indicating that the more layers, the longer material crushing is sustained, and thus the more energy that is absorbed. Stage 3 is final compression, similar to compressing solid metal. During stage 3 the stress increases with a diminishing rate of elongation and the honeycomb is completely failed where the plates between the honeycomb core sandwich the crushed honeycomb ribbon. The stress-strain graph bellow shows compression test of 3 different samples in the T direction. The red lines divide the three stages. The far left is Stage 1, the middle stage 2, and the right stage 3. The data collected is displayed in the table below. The expressions in the table represent the regression formula that represents each stage of the compression on a stress-strain graph. Stage 1 is assumed to intersect with the origin; data for stage 3 for the crush in W and L directions where unable to be gathered due to the nature of failure for those directions. Stage 1 and 2 are linear regressions while stage 3 is a degree 2, to best match the curve. Linear regression is used on stage 2 because ultimately that represents the energy absorbed. With more data, a degree n x 2 regression would be a more appropriate regression for stage 2, where n is the number of layers. The table below is the approximation of each scenario and stage. Each stage starts and ends at the intersection of the next stage. There where two main objectives for these tests: firstly to understand how honeycomb performs under extreme compression, and secondly to be able to numerically represent the honeycomb structure. Both of these where completed to varying degrees. It is important understood how the honeycomb fails. If it is crushed in the T direction it retains its integrity even after being crushed, however when crushed in the L and W crush direction, if it fails, it disintegrates, and loses all integrity. Also, the more layers the more time the material spends in stage 2. Failure is started by buckling, thus if there is any imperfection, the stress will not spike but transition straight into stage 2. The data collected and aggregated can be used for initial simulation of honeycomb used in packages. The initial testing has set the ground work for more data to be collected in order to verify results and to allow more confidence in the simulation results. This is only the initial data collected. The next steps is to continue to collect more data to verify results and to test more variants of honeycomb, with different brazing, layers, and shape.

36 MATERIALS SCIENCE↗

DOE OSTI2024

NSUF BOILER Pre-Irradiation Characterization and High Flux Isotope Reactor Experiment Design

Alumina-forming austenitic (AFA) stainless steels have emerged as a candidate alloy because of their high-temperature strength, formability, cost, and compatibility with primary coolants for lead-cooled fast reactors (LFRs). This class of steels has exceptional high-temperature oxidation performance; however, a high concentration of Ni is required to stabilize the austenite phase and to provide sufficient creep strength. AFA stainless steels are also susceptible to liquid metal embrittlement (LME). Additionally, under neutron irradiation, Ni will enrich at grain boundaries due to radiation-induced segregation (RIS). Nickel RIS can increase the LME under these coupled effects. Oak Ridge National Laboratory (ORNL) and the NSUF program have leveraged its High Flux Isotope Reactor (HFIR) and experience with complex irradiation experiments to design experiment capsules that test the aforementioned coupled effects. These capsules are designed for insertion in the central flux trap, the highest flux region, of HFIR. The experiment capsules will be filled with Pb, designed to passively melt from the gamma heating in HFIR. The specimens were fabricated into miniature tensile specimens from two different alloys, GA05-25Ni and GA05-20Ni, varying Ni concentrations. The experiment capsules are designed to achieve target temperatures of 400 °C and 650 °C with accumulated dosage of 3 dpa. This report documents the specimen alloy characterization, experimental design, and expected performance of the capsules.

21 SPECIFIC NUCLEAR REACTORS AND ASSOCIATED PLANTS↗

DOE OSTI2023

Bona fide upcycling strategy of anhydride cured epoxy and reutilization of decomposed dual monomers into multipurpose applications

Waste epoxy materials become an enormous problem to society and the environment. The advantages of epoxy resins derive from their rigid and chemically stable networks, but these qualities also make them difficult to dispose of or recycle. In this work, we demonstrated an efficient degradation of anhydride cured epoxy resin by aminolysis in aminoethanol without using any catalysts. The epoxy resin was fully decomposed at 160 °C in 4 h, resulting in two distinct high purity monomers (HHPA-OH and BPA-OH). To fully realize this upcycling approach, The BPA-OH was used to synthesize a polyurethane coating with an excellent glass transition temperature (88.9 °C), scratch hardness (8H), gouge hardness (6H), adhesive strength (5B), and strong solvent resistance. The HHPA-OH with two hydroxyl groups was reacted with methacrylic anhydride to form a dimethacrylate monomer which was then used as a viable crosslinker for photo-curable 3D printing thermosetting polymer with tensile strength as high as 64 MPa and impact strength of 4.86 kJ/m 2 . This work demonstrates a feasible pathway to convert anhydride cured epoxy waste to new monomeric recyclates for superior polymer products.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

NASA NTRS1997

Atomic Physics with the Goddard High Resolution Spectrograph on the Hubble Space Telescope: Oscillator Strengths for Neutral Carbon - III

High quality spectra of interstellar absorption from C I toward beta(sup 1) S(sub co), rho O(sub ph) A, and chi O(sub ph) were obtained with the Goddard High Resolution Spectrograph on HST. Many weak lines were detected within the observed wavelength intervals: 1150-1200 A for beta(sup 1) S(sub co) and 1250-1290 A for rho O(sub ph) A and chi O(sub ph). Curve-of-growth analyses were performed in order to extract accurate column densities and Doppler parameters from lines with precise laboratory-based f-values. These column densities and b-values were used to obtain a self-consistent set of f-values for all the observed C I lines. A particularly important constraint was the need to reproduce data for more than one line of sight. For about 50% of the lines, the derived f-values differ appreciably from the values quoted by Morton.

Zsargo, J.↗

DOE OSTI2023

Novel effects of grain size and ion implantation on grain boundary segregation in ion irradiated austenitic steel

Nuclear reactor environments are extreme in nature due to the combination of exposure to corrosive coolant, mechanical stresses, and neutron irradiation damage. This combination of environments can lead to irradiation induced/assisted precipitation, segregation, and embrittlement coupled with enhanced creep and stress corrosion cracking. While nanostructured materials are of interest in a variety of applications due to their unique properties including high mechanical strength, for nuclear applications nanostructured materials have the added benefit of irradiation resistance due to the high volume density of sinks for irradiation-induced defects. In this study, we show unique radiation-induced segregation (RIS) behavior in nanocrystalline 304 stainless steel (SS304). Typical RIS in austenitic steels includes Ni enrichment and Cr depletion within the grain boundaries. In nanostructured SS304 this RIS is reduced. Furthermore, interestingly, some grain boundaries in the nanocrystalline SS304 in this study were found to be enriched in Cr after Fe 2+ ion irradiation at 500 °C up to 50 displacements per atom (dpa). To understand this unique observation, lattice-based atomic kinetic Monte Carlo simulations were performed to investigate the effects of grain size, thermal segregation, as well as injected interstitials (introduced as Fe self-ions). The results indicate that the Cr enrichment at grain boundaries may be caused by combined effects of grain size, self-ion injection and preferential Cr diffusion via the interstitial mechanism. In conclusion, the findings also suggest a possible difference in RIS between ion and neutron irradiations.

36 MATERIALS SCIENCE↗

DOE OSTI2022

Design of an Additively Manufactured Recuperator With 800 °C Inlet Temperature for sCO2 Power Cycle Application

Abstract Recuperators with design temperatures at and above 800 °C can further increase the thermal efficiency of supercritical CO2 power cycles by enabling higher turbine exhaust temperatures. Mar-M247 is a well-suited nickel-based superalloy for high temperature service due to its high creep strength that prevents excessive material thickness being required for pressure containment. Additive manufacturing using a high-speed laser-directed energy deposition (L-DED) process presents a promising solution, with build trials demonstrating the ability to produce nonconventional flow channels for enhanced heat transfer. A design process is presented that includes aerothermal and mechanical evaluation to maximize performance within the constraints of the manufacturing process. A 2-D heat transfer network and pressure drop code allows prediction of flow distribution and its effect on overall thermal performance. Established literature correlations, along with CFD simulation, inform the prediction of heat transfer coefficients and friction factors for the flowpaths and enhancement features in the heat exchanger core. Mechanical evaluation using finite element analysis (FEA) modeling with the intent of the ASME Boiler & Pressure Vessel Code (BPVC) Section VIII, Div. 2 assesses the operational safety of the design. The detailed design features annular finned passages that take advantage of helical flow paths to distribute the flow from separated headers to shared heat transfer surfaces. Performance predictions for the recuperator at a 50 kW scale provide insights into the feasibility of the additively manufactured (AM) process to produce recuperators on a commercial scale that extend existing operating envelopes.

Engineering↗