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Thermal-Structures and Materials Testing Laboratory

Since its inception and successful implementation in 1997 at James Madison University, the Thermal Structures and Materials Testing Laboratory (T-SaMTL) funded by the NASA Langley Research Center is evolving into one of the University's premier and exemplary efforts to increase minority representation in the sciences and mathematics. Serving ten (10) students and faculty directly and almost fifty (50) students indirectly, T-SAMTL, through its recruitment efforts, workshops, mentoring program, tutorial services and its research and computational laboratories has marked the completion of the first year with support from NASA totaling $ 100,000. Beginning as an innovative academic research and mentoring program for underrepresented minority science and mathematics students, the program now boasts a constituency which consists of 50% graduating seniors in the spring of 1998 with 50% planning to go to graduate school. The program's intent is to increase the number of underrepresented minorities who receive doctoral degrees in the sciences by initiating an academically enriched research program aimed at strengthening the academic and self actualization skills of undergraduate students with the potential to pursue doctoral study in the sciences. The program provides financial assistance, academic enrichment, and professional and personal development support for minority students who demonstrate the potential and strong desire to pursue careers in the sciences and mathematics. James Madison University was awarded the first $100,000, in April 1997, by The NASA Langley Research Center for establishment and support of its Thermal Structures and Materials Testing

Teate, Anthony A.

Materials testing of the IUS techroll seal material

As a part of the investigation of the control system failure Inertial Upper Stage on IUS-1 flight to position a Tracking and Data Relay Satellite (TDRS) in geosynchronous orbit, the materials utilized in the techroll seal are evaluated for possible failure models. Studies undertaken included effect of temperature on the strength of the system, effect of fatigue on the strength of the system, thermogravimetric analysis, thermomechanical analysis, differential scanning calorimeter analysis, dynamic mechanical analysis, and peel test. The most likely failure mode is excessive temperature in the seal. In addition, the seal material is susceptible to fatigue damage which could be a contributing factor.

Nichols, R. L.

Development and characterization of an aerosol-generated multi-method analytical particle test material

Ceria (CeO 2 ) particles with low to ultra-low loading of nickel dopant were produced using an aerosol-based, droplet-to-particle synthesis via an in-line calcination technique. This aerosol-based synthesis method enables the production of particles with a monodisperse size distribution. These produced and well-characterized, multi-element, ceria-based particles demonstrate a material exemplar for multi-method analytical testing. They were prepared from a cerium nitrate feedstock where low loading nickel dopant was added at target Ni/(Ni + Ce) atomic percents of 1 %, 0.1 %, and 0.01 %, using a nickel nitrate spike. This methodology proved to produce ceria particles doped with a dynamic range of low to ultra-low loadings of nickel over a 24-h period, with consistent size distribution, morphology, and composition. The successful incorporation of nickel was demonstrated with bulk and single particle inductively coupled plasma mass spectroscopy and revealed notable particle-to-particle elemental homogeneity. X-ray photoelectron spectroscopy demonstrated the presence of a high concentration of nickel dopant incorporated preferentially toward the surface of the particles, and that this dopant aided oxidation of surface Ce(III) atoms to Ce(IV). These particle test materials were then validated through X-ray absorption near edge spectroscopy, comparing the ultra-low 0.01 % Ni and low 1 % Ni-doped ceria samples. This revealed a more-reduced oxidation state of the nickel with an increase in dopant concentration. Finally, this work demonstrates a synthesis and systematic characterization scheme to produce multi-method analytical test particulates.

36 MATERIALS SCIENCE

International Low-Earth-Orbit Spacecraft Materials Test Program Initiated for Better Prediction of Durability and Performance

Spacecraft in low Earth orbit (LEO) are subjected to many components of the environment, which can cause them to degrade much more rapidly than intended and greatly shorten their functional life. The atomic oxygen, ultraviolet radiation, and cross contamination present in LEO can affect sensitive surfaces such as thermal control paints, multilayer insulation, solar array surfaces, and optical surfaces. The LEO Spacecraft Materials Test (LEO-SMT) program is being conducted to assess the effects of simulated LEO exposure on current spacecraft materials to increase understanding of LEO degradation processes as well as to enable the prediction of in-space performance and durability. Using ground-based simulation facilities to test the durability of materials currently flying in LEO will allow researchers to compare the degradation evidenced in the ground-based facilities with that evidenced on orbit. This will allow refinement of ground laboratory test systems and the development of algorithms to predict the durability and performance of new materials in LEO from ground test results. Accurate predictions based on ground tests could reduce development costs and increase reliability. The wide variety of national and international materials being tested represent materials being functionally used on spacecraft in LEO. The more varied the types of materials tested, the greater the probability that researchers will develop and validate predictive models for spacecraft long-term performance and durability. Organizations that are currently participating in the program are ITT Research Institute (USA), Lockheed Martin (USA), MAP (France), SOREQ Nuclear Research Center (Israel), TNO Institute of Applied Physics (The Netherlands), and UBE Industries, Ltd. (Japan). These represent some of the major suppliers of thermal control and sensor materials currently flying in LEO. The participants provide materials that are exposed to selected levels of atomic oxygen, vacuum ultraviolet radiation, contamination, or synergistic combined environments at the NASA Lewis Research Center. Changes in characteristics that could affect mission performance or lifetime are then measured. These characteristics include changes in mass, solar absorptance, and thermal emittance. The durability of spacecraft materials from U.S. suppliers is then compared with those of materials from other participating countries. Lewis will develop and validate performance and durability prediction models using this ground data and available space data. NASA welcomes the opportunity to consider additional international participants in this program, which should greatly aid future spacecraft designers as they select materials for LEO missions.

Rutledge, Sharon K.

Instrumented Materials Testing

This presentation starts with an introduction to the need for materials testing. Classic failures (such as brittle ship hull fractures) are discussed before fundamental discoveries in fracture analysis (Griffith, Westergaard, and Irwin). Next standard tests are identified, followed by a look at brittle versus ductile failure. Griffith's result (the composite paradigm) that smaller composite specimens are stronger because they have smaller flaws, is covered. This leads into composite tests. And finally, stress waves are shown as an example that will initiate damage.

Mackin, Thomas J.

Europa Propulsion Valve Seat Material Testing

The Europa mission and spacecraft design presented unique challenges for selection of valve seat materials that met the fluid compatibility requirements, and combined fluid compatibility and high radiation exposure level requirements. The Europa spacecraft pressurization system valves will be exposed to fully saturated propellant vapor for the duration of the mission. The effects of Nitrogen Tetroxide (NTO) and Monomethylhydrazine (MMH) propellant vapors on heritage valve seat materials, such as Vespel SP-1 and Polychlorotrifluoroethylene (PCTFE), were evaluated to determine if an alternate material is required. In liquid system applications, Teflon is the only available compatible valve seat material. Radiation exposure data for Teflon in an air or vacuum environment has been previously documented. Radiation exposure data for Teflon in an oxidizer environment such as NTO, was not available, and it was unknown whether the effects would be similar to those on air-exposed samples. Material testing was conducted by Marshall Space Flight Center (MSFC) and White Sands Test Facility (WSTF) to determine the effects of propellant vapor on heritage seat materials for pressurization valve applications, and the effects of combined radiation and NTO propellant exposure on Teflon. The results indicated that changes in heritage pressurization valve seat materials' properties rendered them unsuitable for the Europa application. The combined radiation and NTO exposure testing of Teflon produced results equivalent to combined radiation and air exposure results.

Addona, Brad M.

Structure–Property Relationships of Recycled Lithium-Ion Battery Cathodes: Microstructure Optimization Using Virtual Materials Testing

The increasing demand for sustainable battery technologies requires effective recycling strategies for end-of-life lithium-ion battery cathodes. In this study, virtual materials testing, a well-established framework for modeling conventionally manufactured NMC-based cathodes, is applied to partially recycled cathodes. To this end, virtual cathodes consisting of mixtures of pristine and recycled NMC particles are utilized to systematically analyze structure–property relationships depending on mixing ratios and different spatial arrangement strategies. For this purpose, a stochastic 3D model is developed that is capable of generating virtual cathodes with arbitrary volume fractions of active materials and mixing ratios of pristine and recycled NMC particles. Particularly, the stochastic 3D model can mimic the different size distributions of pristine and recycled particles that are observed in image data. Additionally, the model allows the structuring of pristine and recycled NMC either uniformly mixed or layer-wise arranged, mimicking single- and dual-layer cathodes. Subsequently, a systematic computational analysis is conducted to assess the influence of increasing active material ratios of recycled particles, ranging from 0 % to 100 %, while maintaining a constant overall active material volume fraction. The impact of particle mixing on cathode performance is evaluated by examining transport-relevant geometrical descriptors and effective properties, such as geodesic tortuosity, specific surface area, and tortuosity factor.

25 ENERGY STORAGE

Materials Testing on the DC-X and DC-XA

Flight testing of thermal protection materials has been carried out over a two year period on the base heat shield of the Delta Clipper (DC-X and DC-XA), as well on a body flap. The purpose was to use the vehicle as a test bed for materials and more efficient repair or maintenance processes which would be potentially useful for application on new entry vehicles (i.e., X-33, RLV, planetary probes), as well as on the existing space shuttle orbiters. Panels containing Thermal Protection Systems (TPS) and/or structural materials were constructed either at NASA Ames Research Center or at McDonnell Douglas Aerospace (MDA) and attached between two of the four thrusters in the base heat shield of the DC-X or DC-XA. Three different panels were flown on DC-X flights 6, 7, and 8. A total of 7 panels were flown on DC-XA flights 1, 2, and 3. The panels constructed at Ames contained a variety of ceramic TPS including flexible blankets, tiles with high emissivity coatings, lightweight ceramic ablators and other ceramic composites. The MDS test panels consisted primarily of a variety of metallic composites. This report focuses on the ceramic TPS test results.

Smith, Dane

Mars Space Suit Materials Testing Using SHERLOC Calibration Target Data: The Max-CF Project

The Mars 2020/“Perseverance” rover carries a suite of space suit materials as part of the SHERLOC* calibration target [1]. The materials are periodically analyzed by SHERLOC as part of a regular calibration routine and are generating a rich data set regarding their degradation in the martian surface environment. The Maximization of Calibration Fabrics (Max-CF) project will effectively turn SHERLOC data into a measure of space suit material service lifetimes by exposing a second set of materials in a Mars chamber, replicating SHERLOC measurements using the analogous ACRONM** instrument at JSC, and then performing materials testing to include tensile testing. These data can be used to inform space suit design and/or materials development, improving crew safety for future Mars missions. This will partially address NASA’s Strategic Knowledge Gap 8 (Mars Surface Technology) which identifies a need to develop technologies to “sustain humans on the surface of Mars [and] enable human mobility and exploration” [2]. This abstract describes the overall Max-CF project and progress on the laboratory-based study to date.

M Fries

Methods and instruments for materials testing

Methods and instruments for characterizing a material, such as the properties of bone in a living human subject, using a test probe constructed for insertion into the material and a reference probe aligned with the test probe in a housing. The housing is hand held or placed so that the reference probe contacts the surface of the material under pressure applied either by hand or by the weight of the housing. The test probe is inserted into the material to indent the material while maintaining the reference probe substantially under the hand pressure or weight of the housing allowing evaluation of a property of the material related to indentation of the material by the probe. Force can be generated by a voice coil in a magnet structure to the end of which the test probe is connected and supported in the magnet structure by a flexure, opposing flexures, a linear translation stage, or a linear bearing. Optionally, a measurement unit containing the test probe and reference probe is connected to a base unit with a wireless connection, allowing in the field material testing.

Hansma, Paul

Overview of advanced plasma-facing materials testing for Fusion Pilot Plants at DIII-D

Characterization and testing of advanced plasma-facing materials (PFMs) for Fusion Pilot Plants (FPP) is being conducted at the DIII-D National Fusion Facility through the ongoing two-year FPP Candidate Materials Thrust. Year one tested 17 novel materials utilizing the Divertor Materials Evaluation System (DiMES), with samples analyzed pre- and post-experiment via SEM, EDS, and confocal microscopy. Repeatable reference discharges were developed to ensure uniformity between experiments, including a new strike-point rastering scenario to provide more uniform heat/particle flux across DiMES during ELMing H-mode discharges. Various sample geometries and temperatures were used to achieve FPP-relevant conditions, including samples angled 10° towards the incident plasma flux and pre-heating up to 500 °C. The first exposure of liquid lithium (Li) capillary porous structures in a tokamak demonstrated uniform emission of Li vapor and suppression of Li droplets in H-mode when preheated to 350 °C. Dispersoid-strengthened W with 1 wt% TaC, TiC, and ZrC exposed to H-mode showed cracking and dispersoid ejection for all varieties except TiC, providing a clear down-selection. Ultra-high temperature ceramic materials TiB 2 and ZrB 2 showed minimal degradation under L-mode exposure. Silicon carbide (SiC) fiber composites showed arcing along edges, while CVD SiC remained pristine. Atmospheric plasma-sprayed W and SiC coatings endured H-mode exposure without macroscopic delamination; SiC exhibited granular ejection, while W showed increased outgassing. Additional W-based alloys were stress tested in H-mode, including Ni-based W heavy alloys, W f SiC f /W composites, W multi-principle element alloys, and functionally-graded W/SiC, to varying degrees of success.

DIII-D

Thermocouple Calibration and Accuracy in a Materials Testing Laboratory

A consolidation of information has been provided that can be used to define procedures for enhancing and maintaining accuracy in temperature measurements in materials testing laboratories. These studies were restricted to type R and K thermocouples (TCs) tested in air. Thermocouple accuracies, as influenced by calibration methods, thermocouple stability, and manufacturer's tolerances were all quantified in terms of statistical confidence intervals. By calibrating specific TCs the benefits in accuracy can be as great as 6 C or 5X better compared to relying on manufacturer's tolerances. The results emphasize strict reliance on the defined testing protocol and on the need to establish recalibration frequencies in order to maintain these levels of accuracy.

Lerch, B. A.

Automation software for a materials testing laboratory

The software environment in use at the NASA-Lewis Research Center's High Temperature Fatigue and Structures Laboratory is reviewed. This software environment is aimed at supporting the tasks involved in performing materials behavior research. The features and capabilities of the approach to specifying a materials test include static and dynamic control mode switching, enabling multimode test control; dynamic alteration of the control waveform based upon events occurring in the response variables; precise control over the nature of both command waveform generation and data acquisition; and the nesting of waveform/data acquisition strategies so that material history dependencies may be explored. To eliminate repetitive tasks in the coventional research process, a communications network software system is established which provides file interchange and remote console capabilities.

Mcgaw, Michael A.

Guidelines for Assessing the Toxic Hazard of Spacecraft Chemicals and Test Materials

This document describes the criteria and procedural guidelines used by the NASA/JSC Toxicology Office (JSCSTO), to perform toxicological evaluations. The JSCSTO is responsible for conducting toxicological assessments and assigning toxic hazard levels (THLs) for essentially all chemicals and test materials to be used in or transported to the habitable areas of U.S. spacecraft, non‐U.S. spacecraft inhabitaed by U.S. crew members or habitable areas of off‐Earth habitats where U.S. crew members would be present, including chemicals carried by visiting spacecraft(visiting vehicles) to and from the International Space Station (ISS). Biohazard assessments for biological materials used in payload experiments are performed by the NASA Biosafety Review Board. Radioactive materials are assessed by the Space Radiation Analysis Group for radiation hazards; the flammability rating on flammable materials is assessed by the JSC Materials and Processes Branch, ES4. This document will focus on the assessment of chemically‐induced toxicity hazards. The toxicological assessments, together with assessments on radioactive, biological, physical, and flammability hazards, are incorporated into a mission‐specific Hazardous Materials Summary Table (HMST).

Valerie Elizabeth Ryder