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DOE OSTI2023

An autonomous laboratory for the accelerated synthesis of novel materials

To close the gap between the rates of computational screening and experimental realization of novel materials, we introduce the A-Lab, an autonomous laboratory for the solid-state synthesis of inorganic powders. This platform uses computations, historical data from the literature, machine learning (ML) and active learning to plan and interpret the outcomes of experiments performed using robotics. Over 17 days of continuous operation, the A-Lab realized 41 novel compounds from a set of 58 targets including a variety of oxides and phosphates that were identified using large-scale ab initio phase-stability data from the Materials Project and Google DeepMind. Synthesis recipes were proposed by natural-language models trained on the literature and optimized using an active-learning approach grounded in thermodynamics. Analysis of the failed syntheses provides direct and actionable suggestions to improve current techniques for materials screening and synthesis design. The high success rate demonstrates the effectiveness of artificial-intelligence-driven platforms for autonomous materials discovery and motivates further integration of computations, historical knowledge and robotics.

36 MATERIALS SCIENCE↗

NASA NTRS2001

Modeling the Gas Dynamics Environment in a Subscale Solid Rocket Test Motor

Subscale test motors are often used for the evaluation of solid rocket motor component materials such as internal insulation. These motors are useful for characterizing insulation performance behavior, screening insulation material candidates and obtaining material thermal and ablative property design data. One of the primary challenges associated with using subscale motors however, is the uncertainty involved when extrapolating the results to full-scale motor conditions. These uncertainties are related to differences in such phenomena as turbulent flow behavior and boundary layer development, propellant particle interactions with the wall, insulation off-gas mixing and thermochemical reactions with the bulk flow, radiation levels, material response to the local environment, and other anomalous flow conditions. In addition to the need for better understanding of physical mechanisms, there is also a need to better understand how to best simulate these phenomena using numerical modeling approaches such as computational fluid dynamics (CFD). To better understand and model interactions between major phenomena in a subscale test motor, a numerical study of the internal flow environment of a representative motor was performed. Simulation of the environment included not only gas dynamics, but two-phase flow modeling of entrained alumina particles like those found in an aluminized propellant, and offgassing from wall surfaces similar to an ablating insulation material. This work represents a starting point for establishing the internal environment of a subscale test motor using comprehensive modeling techniques, and lays the groundwork for improving the understanding of the applicability of subscale test data to full-scale motors. It was found that grid resolution, and inclusion of phenomena in addition to gas dynamics, such as two-phase and multi-component gas composition are all important factors that can effect the overall flow field predictions.

Eaton, Andrew M.↗

NASA NTRS1988

Ignition of nonmetallic materials by impact of high-pressure gaseous oxygen

The sources of variability in the pneumatic impact test commonly used to screen nonmetallic materials for oxygen service and to rank batches or lots of particular materials were investigated together with the mechanism of ignition. Tests were conducted at the NASA/White Sands Test Facility in which the standard test chamber was replaced by an instrumented chamber to obtain information on the rates of pressurization, specimen heating, and time to ignition. Results showed that much of the variability in test data could be traced to the variability in system cleanliness and in the opening time of the high-speed valve. The prinicipal mechanism of ignition in the test is considered to be the heating of the gas initially in the test chamber by adiabatic compression; the presence of voids in the test materials may also be important.

Moffett, Gary E.↗

DOE OSTI2022

Roadmap to Iodine and Mercury Abatement Materials Selection in Nuclear Waste Processing Off-Gas Streams

This work provides a guide for candidate mercury (Hg) and iodine-129 (129I) abatement material identification, screening, evaluation, technical gap identification, and bench-scale testing prioritization while also conceptualizing a materials deployment roadmap for implementation of new materials in the Hanford Waste Treatment and Immobilization Plant (WTP) Low-Activity Waste (LAW) Facility at Hanford in Richland, Washington, and elsewhere in the U.S. Department of Energy (DOE) complex for similar applications. The study was prompted by the need to replace the Kombisorb BAT-37 due to uncertainties in Hg and 129I capture performance and future availability for use in the WTP LAW Facility secondary off-gas system, specifically the Carbon Adsorber units. However, replacement of this material could also mitigate two other issues with Kombisorb BAT-37 (and its successor BAT II 37): (1) fire safety risk due to exothermic heat generated by adsorption reactions between the carbon material and Hg and (2) the risk of low retention of 129I in glass and subsequent downstream impacts on secondary liquid waste treatment at the Effluent Treatment Facility.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

NASA NTRS1983

Design, fabrication and testing of porous tungsten vaporizers for mercury ion thrusters

The dispersions in the characteristics, performance and reliability of vaporizers for early model 30-cm thrusters were investigated. The purpose of the paper is to explore the findings and to discuss the approaches that were taken to reduce the observed dispersion and present the results of a program which validated those approaches. The information that is presented includes porous tungsten materials specifications, a discussion of assembly procedures, and a description of a test program which screens both material and fabrication processes. There are five appendices providing additional detail in the areas of vaporizer contamination, nitrogen flow testing, bubble testing, porosimeter testing, and mercury purity. Four neutralizers, seven cathodes and five main vaporizers were successfully fabricated, tested, and operated on thrusters. Performance data from those devices is presented and indicates extremely repeatable results from using the design and fabrication procedures.

Zavesky, R.↗

NASA NTRS1998

Effects of regenerator geometry on pulse tube refrigerator performance

This paper gives results of the cooling performance of a double-inlet pulse tube refrigerator using various regenerators. The same pulse tube was used for all the experiments and measured 4.76 mm in diameter and 46.2 mm in length. A commercial linear compressor with a swept volume of 4 cm3 was used in these experiments. The operating conditions were held constant at a mean pressure of 2.0 MPa and a frequency of 54 Hz. Using finite difference software called REGEN3.1, developed at NIST, and recent experiment results, we optimized a series of regenerators based on dimensions, materials and screen packing. The values used for calculating the thermal conduction through stacked screens by REGEN3.1 were based on recent experimental results from NIST. The regenerator tubes were designed using 316 stainless steel and titanium materials. The regenerator matrices investigated were 400-mesh and 500-mesh stainless steel screen. The valve settings for both orifices were adjusted to minimize the no-load temperature for all regenerators. A cooling capacity curve from 0 to 3 W was also determined. The performance of the pulse tube refrigerator using the different regenerators is discussed. The experimental results from the various regenerators are evaluated and compared with their corresponding numerically calculated coefficient of performance (COP) and regenerator design as determined by REGEN3.1.

NASA Discipline Life Sciences Technologies↗

NASA NTRSDate not supplied

Extending mARC II Arc-Jet Test Duration via Design and Implementation of Model System Cooling Sleeve

The mARC II is a 30 kW arc-jet facility at NASA Ames Research Center used to generate high-enthalpy flows for low-cost thermal protection system (TPS) technology development. Sustained operation of downstream instrumentation and material samples is constrained by thermal loading transmitted through the arc-jet test environment, limiting achievable run times and experimental throughput. This work presents the design, integration, and validation of a cooling sleeve implemented on the sweep arm drive motor feedthrough to mitigate thermal accumulation during testing. The addition of the cooling sleeve is a simple, robust upgrade that translates directly into enhanced facility capability by supporting longer run durations, reduced turnaround time, and higher throughput.

numerical simulations↗

NASA NTRS1994

Milestone 4: Thrust structure concepts and IHM screening Graphite Composite Primary Structure (GCPS)

The first part of the task was to select up to three promising thrust structure constructions and to select materials for screening tests. Part of the nondestructive evaluation and inspection (NDE/I) and integrated health management (IHM) task is to acquire and develop NDE/I sensor technologies and to integrate those sensors into the full scale test articles which will be produced under the TA2 program. Review of the anticipated fault modes and the available sensor technology data indicates that three sensor technologies should be assessed for the in-situ monitoring of the composite primary structure elements. These are: ultrasonics (dry contact), acoustic emissions, and fiber optics (embedded or attached). In fact, a combination of sensor technologies will be needed to detect and evaluate the fault modes; not only do sensor technology have specific capabilities and applicability, but the three Gr/Ep primary structures being demonstrated under the TA2 effort have differing requirements based on their respective failure modes and designs.

Greenberg, H. S.↗

NASA NTRS2001

Delta L: An Apparatus for Measuring Macromolecule Crystal Growth Rates in Microgravity

Strongly diffracting high quality macromolecule crystals of suitable volume are keenly sought for X-ray diffraction analysis so that high-resolution molecular structure data can be obtained. Such data is of tremendous value to medical research, agriculture and commercial biotechnology. In previous studies by many investigators microgravity has been reported in some instances to improve biological macromolecule X-ray crystal quality while little or no improvement was observed in other cases. A better understanding of processes effecting crystal quality improvement in microgravity will therefore be of great benefit in optimizing crystallization success in microgravity. In ground based research with the protein lysozyme we have previously shown that a population of crystals grown under the same solution conditions, exhibit a variation in X-ray diffraction properties (Judge et al., 1999). We have also observed that under the same solution conditions, individual crystals will grow at slightly different growth rates. This phenomenon is called growth rate dispersion. For small molecule materials growth rate dispersion has been directly related to crystal quality (Cunningham et al., 1991; Ristic et al., 1991). We therefore postulate that microgravity may act to improve crystal quality by reducing growth rate dispersion. If this is the case then as different, Materials exhibit different degrees of growth rate dispersion on the ground then growth rate dispersion could be used to screen which materials may benefit the most from microgravity crystallization. In order to assess this theory the Delta L hardware is being developed so that macromolecule crystal growth rates can be measured in microgravity. Crystal growth rate is defined as the change or delta in crystal size (defined as a characteristic length, L) over time; hence the name of the hardware. Delta L will consist of an optics, a fluids, and a data acquisition sub-assemblies. The optics assembly will consist of a video microscope camera mounted on three axis computer controlled translation stages. The fluids assembly consists of macromolecule and precipitant reservoirs, a temperature controlled growth cell and waste container, The data acquisition is achieved by using a frame-gabber, with images being stored on a hard drive. In operation, macromolecule and precipitant solution will be injected into the temperature controlled growth cell. As macromolecule crystals grow, the video microscope camera controlled by the translation stages, will be used to locate and record images of individual crystals, returning to the same crystals at specific time intervals. The images will be stored on the hard drive and used to calculate the crystal growth rate. To prevent vibrations interfering in the crystal growth rate measurements (Snell et al., 1997) Delta L will be used in connection with the Glovebox Integrated Microgravity Isolation Technology (g-LIMIT) inside the Microgravity Science Glovebox (MSG), onboard the International Space Station (ISS).

Judge, Russell A.↗

DOE OSTI2024

Data-driven search for promising intercalating ions and layered materials for metal-ion batteries

The rise in demand for lithium-ion batteries has led to a large-scale search for electrode materials and intercalating ion species to meet the demands of next-generation energy technologies. Recent efforts largely focus on searching for cathodes that can accommodate large amounts of intercalating ions, but similar work on anodes is relatively limited. This study utilizes machine learning methods to find alternative two-dimensional (2D) materials and intercalating ions beyond Li for metal-ion batteries with high-power efficiencies. The approach first uses density functional theory (DFT) calculations to estimate the theoretical capacities and voltages of various metal ions on 2D materials. The DFT-generated data also provide insights into the local structural accommodation upon ion intercalation on various 2D materials. Significant changes to the lattice can result in irreversible changes to the bonding environments in the anode material, resulting in poor cycling stability. Next, this study develops a binding energy and structural accommodation-based classification model to screen anode materials for next-generation batteries. The classification model selects intercalating ions and 2D material pairs suitable for batteries based on the calculated voltage and volumetric changes in the 2D material upon intercalation. Finally, this study builds a regression model to accurately predict the binding energies of the various intercalating ions on 2D materials. The approach highlights the importance of different elemental and structural features for classification and regression tasks. In conclusion, the insights gained from this study on the role of involved features, such as electronegativities of the constituent ions and the presence of unfilled electronic levels, will help to streamline further studies towards the search for future layered battery materials.

36 MATERIALS SCIENCE↗

NASA NTRS1976

Testing of molded high temperature plastic actuator road seals for use in advanced aircraft hydraulic systems

Molded high temperature plastic first and second stage rod seal elements were evaluated in seal assemblies to determine performance characteristics. These characteristics were compared with the performance of machined seal elements. The 6.35 cm second stage Chevron seal assembly was tested using molded Chevrons fabricated from five molding materials. Impulse screening tests conducted over a range of 311 K to 478 K revealed thermal setting deficiencies in the aromatic polyimide molding materials. Seal elements fabricated from aromatic copolyester materials structurally failed during impulse cycle calibration. Endurance testing of 3.85 million cycles at 450 K using MIL-H-83283 fluid showed poorer seal performance with the unfilled aromatic polyimide material than had been attained with seals machined from Vespel SP-21 material. The 6.35 cm first stage step-cut compression loaded seal ring fabricated from copolyester injection molding material failed structurally during impulse cycle calibration. Molding of complex shape rod seals was shown to be a potentially controllable technique, but additional molding material property testing is recommended.

Waterman, A. W.↗

NASA NTRS1994

BSM Delta qualification 2, volume 1

This report, presented in three volumes, provides the results of a two-motor Delta Qualification 2 program conducted in 1993 to certify the following enhancements for incorporation into Booster Separation Motor (BSM) flight hardware: (1) vulcanized-in-place nozzle aft closure insulation; (2) new isostatic ATJ bulk graphite throat insert material; (3) adhesive EA 9394 for bonding the nozzle throat, igniter grain rod/centering insert/igniter case; (4) deletion of the igniter adapter insulator ring; (5) deletion of igniter adapter/igniter case interface RTV; and (6) deletion of Loctite from igniter retainer plate threads. The enhancements above directly resulted from (1) the BSM Total Quality Management (TQM) Team initiatives to enhance the BSM producibility, and (2) the necessity to qualify new throat insert and adhesive systems to replace existing materials that will not be available. Testing was completed at both the component and motor levels. Component testing was accomplished to screen candidate materials (e.g., throat materials, adhesive systems) and to optimize processes (e.g., aft closure insulator vulcanization approach) prior to their incorporation into the test motors. Motor testing - consisting of two motors, randomly selected by USBI's onsite quality personnel from production lot AAY, which were modified to accept the enhancements - were completed to provide the final qualification of the enhancements for incorporation into flight hardware. It is concluded that all of the enhancements herein tested are qualified to be incorporated into flight hardware for the BSM.

Source record↗

NASA NTRS1994

BSM Delta Qualification 2, volume 2

This report, presented in three volumes, provides the results of a two-motor Delta Qualification 2 program conducted in 1993 to certify the following enhancements for incorporation into booster separation motor (BSM) flight hardware: vulcanized-in-place nozzle aft closure insulation; new iso-static ATJ bulk graphite throat insert material; adhesive EA 9394 for bonding the nozzle throat, igniter grain rod/centering insert/igniter case; deletion of the igniter adapter insulator ring; deletion of the igniter adapter/igniter case interface RTV; and deletion of loctite from igniter retainer plate threads. The enhancements above directly resulted from (1) the BSM total quality management (TQM) team initiatives to enhance the BSM producibility, and (2) the necessity to qualify new throat insert and adhesive systems to replace existing materials that will not be available. Testing was completed at both the component and motor levels. Component testing was accomplished to screen candidate materials (e.g., throat materials, adhesive systems) and to optimize processes (e.g., aft closure insulator vulcanization approach) prior to their incorporation into the test motors. Motor tests -- consisting of two motors, randomly selected by USBI's on-site quality personnel from production lot AAY, which were modified to accept the enhancements -- were completed to provide the final qualification of the enhancements for incorporation into flight hardware. Volume 2 details the environmental testing (vibration and shock) conducted at Marshall Space Flight Center (MSFC) to which the motors were subjected prior to static tests.

Source record↗

NASA NTRS1994

BSA Delta Qualification 2, volume 3, book 1

This report, presented in three volumes, provides the results of a two-motor Delta Qualification 2 program conducted in 1993 to certify the following enhancements for incorporation into booster separation motor (BSM) flight hardware: vulcanized-in-place nozzle aft closure insulation; new iso-static ATJ bulk graphite throat insert material; adhesive EA 9394 for bonding the nozzle throat, igniter grain rod/centering insert/igniter case; deletion of the igniter adapter insulator ring; deletion of the igniter adapter/igniter case interface RTV; and deletion of Loctite from igniter retainer plate threads. The enhancements above directly resulted from (1) the BSM total quality management (TQM) team initiatives to enhance the BSM producibility, and (2) the necessity to qualify new throat insert and adhesive systems to replace existing materials that will not be available. Testing was completed at both the component and motor levels. Component testing was accomplished to screen candidate materials (e.g., throat materials, adhesive systems) and to optimize processes (e.g., aft closure insulator vulcanization approach) prior to their incorporation into the test motors. Motor tests -- consisting of two motors, randomly selected by USBI's on-site quality personnel from production lot AAY, which were modified to accept the enhancements -- were completed to provide the final qualification of the enhancements for incorporation into flight hardware. Volume 3 book 1 provides supporting documentation to the analyses and plans of testing the two Delta Qualification units including thermal cycling planning/data acceptance records, environmental test procedures and pretest temperature conditioning history, Delta Qualification test plan, and specification SE0837 -- mix acceptance test specification.

Source record↗

NASA NTRS1994

BSM Delta Qualification 2, volume 3, book 2

This report, presented in three volumes, provides the results of a two-motor Delta Qualification 2 program conducted in 1993 to certify the following enhancements for incorporation into booster separation motor (BSM0 flight hardware: vulcanized-in-place nozzle aft closure insulation; new iso-static ATJ bulk graphite throat insert material, adhesive EA9394 for bonding the nozzle throat, igniter grain rod/centering insert/igniter case; deletion of the igniter adapter insulator ring; deletion of the igniter adapter/igniter case interface RTV; and deletion of loctite from igniter retainer plate threads. The enhancements above directly resulted from (1) the BSM total quality management (TQM) team initiatives to enhance the BSM producibility, and (2) the necessity to qualify new throat insert and adhesive systems to replace existing materials that will not be available. Testing was completed at both the component and motor levels. Component testing was accomplished to screen candidate materials (e.g., throat materials, adhesive systems) and to optimize processes (e.g., aft closure insulator vulcanization approach) prior to their incorporation into the test motors. Motor testing--consisting of two motors, randomly selected by USBI's on-site quality personnel from production lot AAY, which were modified to accept the enhancements -- was completed to provide the final qualification of the enhancements for incorporation into flight hardware. Volume 3, Book 2 provides various supporting documentation to the previous volumes with regards to the testing of the two Delta qualification units: data acceptance records, thermal conditioning analysis, igniter adapter thermal flake analysis, laboratory adhesive (EA-9394) qualification report, throat insert thermal/structural analysis, Delta Qualification Nonconformance Reports (NCR's), O-ring seating tests, and interim test report for vulcanization process qualification.

Source record↗

DOE OSTI2021

Developing Ideal Metalorganic Hydrides for Hydrogen Storage: from Theoretical Prediction to Rational Fabrication

Materials for hydrogen storage have been extensively explored for a few decades. Thousands of materials have been synthesized and tested, however, sparse systems could meet the practical requirements. Metalorganic hydrides discovered recently offer new opportunities. It is, however, extremely time-consuming and inefficient to experimentally screen potential materials from a large variety of metal cations and organic anions. In the present study, we performed wideranging theoretical predictions and screened more than 90 metalorganic hydrides, 20 of them were identified with both high hydrogen capacities (=5 wt%) and suitable thermodynamics (heat of H2 desorption: 25 ~ 35 kJ/mol-H2) that allows hydrogen uptake and release near ambient condition.

Jing, Zijun↗

NASA NTRS1997

Space Environmental Effects on the Optical Properties of Selected Transparent Polymers

Transparent polymer films are currently considered for use as solar concentrating lenses for spacecraft power and propulsion systems. These polymer films concentrate solar energy onto energy conversion devices such as solar cells and thermal energy systems. Conversion efficiency is directly related to the polymer transmission. Space environmental effects will decrease the transmission and thus reduce the conversion efficiency. This investigation focuses on the effects of ultraviolet and charged particle radiation on the transmission of selected transparent polymers. Multiple candidate polymer samples were exposed to near ultraviolet (NUV) radiation to screen the materials and select optimum materials for further study. All materials experienced transmission degradation of varying degree. A method was developed to normalize the transmission loss and thus rank the materials according to their tolerance of NUV. Teflon(Tm) FEP and Teflon(Tm) PFA were selected for further study. These materials were subjected to a combined charged particle dose equivalent to 5 years in a typical geosynchronous Earth orbit (GEO). Results from these NUV screening tests and the 5 year GEO equivalent dose are presented.

Edwards, David L.↗

NASA NTRS2003

On the Use of Accelerated Test Methods for Characterization of Advanced Composite Materials

A rational approach to the problem of accelerated testing for material characterization of advanced polymer matrix composites is discussed. The experimental and analytical methods provided should be viewed as a set of tools useful in the screening of material systems for long-term engineering properties in aerospace applications. Consideration is given to long-term exposure in extreme environments that include elevated temperature, reduced temperature, moisture, oxygen, and mechanical load. Analytical formulations useful for predictive models that are based on the principles of time-based superposition are presented. The need for reproducible mechanisms, indicator properties, and real-time data are outlined as well as the methodologies for determining specific aging mechanisms.

Gates, Thomas S.↗