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At least 523 records · Page 29

All sources NASA NTRS DOE OSTI

DOE OSTI2023

Scalable in situ non-destructive evaluation of additively manufactured components using process monitoring, sensor fusion, and machine learning

Laser Powder Bed Fusion (L-PBF) Additive Manufacturing (AM) is among the metal 3D printing technologies most broadly adopted by the manufacturing industry. However, the current industry qualification paradigm for critical-application L-PBF parts relies heavily on expensive non-destructive inspection techniques, which significantly limits the use-cases of L-PBF. In situ monitoring of the process promises a less expensive alternative to ex situ testing, but existing sensor technologies and data analysis techniques struggle to detect sub-surface flaws (e.g., porosity and cracking) on production-scale L-PBF printers. In this work, an in situ NDE (INDE) system was engineered to detect subsurface flaws detected in X-Ray Computed Tomography (XCT) directly from process monitoring data. A multilayer, multimodal data input allowed the INDE system to detect numerous subsurface flaws in the size range of 200–1000µm using a novel human-in-the-loop annotation procedure. Furthermore, a framework was established for generating probability-of-detection (POD) and probability-of-false-alarm (PFA) curves compliant with NDE standards by systematically comparing instances of detected subsurface flaws to post-build XCT data. Here, we also introduce for the first time in the AM in situ sensing literature the a 90/95 – the flaw size corresponding to a 90% detection rate on the lower 95% confidence interval of the POD curve. The INDE system successfully demonstrated POD capabilities commensurate with traditional NDE methods. Traditional ML performance metrics were also shown to be inadequate for assessing the ability of the INDE system’s flaw detection performance. It is the hope of the authors that future studies will adopt the POD and PFA approach outlined here to provide better insight into the utility of process monitoring for AM.

36 MATERIALS SCIENCE↗

DOE OSTI2016

In-situ TEM on the coalescence of birnessite manganese dioxides nanosheets during lithiation process

Highlights: • Evolution of MnO{sub 2} nanosheets during lithiation was in situ observed. • MnO{sub 2} was reacted with Li to form Mn and LiO{sub 2}. • Nanosheets expanded and aggregated due to lithiation. - Abstract: Nanostructure is believed to produce great benefits for anode materials in lithium ion batteries (LIBs) by enhancing lithium ion transfer, accommodating large volume change and increasing surface area. Whether the nanostructure (especially the porous nanostructure) could be well held during charging/discharging process is one of the most commonly concerned issues in LIBs research. The dynamic evolution of birnessite manganese dioxides nanosheets during lithiation process is investigated by in-situ transmission electron microscopy (TEM) for the first time. The TiO{sub 2}@MnO{sub 2} core-shell nanowires are used as the anode and Li metal as the counter electrode inside the TEM. Interestingly, the lithiation process is confirmed as MnO{sub 2} and Li converting to Li{sub 2}O and Mn. The original porous structure of the nanosheets is hard to preserve during lithiation process due to lithiation-induced contact flattening.

36 MATERIALS SCIENCE↗

DOE OSTI2014

In situ examination of oxygen non-stoichiometry in La{sub 0.80}Sr{sub 0.20}CoO{sub 3−δ} thin films at intermediate and low temperatures by x-ray diffraction

Structural evolution of epitaxial La{sub 0.80}Sr{sub 0.20}CoO{sub 3−δ} thin films under chemical and voltage stimuli was examined in situ using X-ray diffraction. The changes in lattice parameter (chemical expansivity) were used to quantify oxygen reduction reaction processes and vacancy concentration changes in lanthanum strontium cobaltite. At 550 °C, the observed lattice parameter reduction at an applied bias of −0.6 V was equivalent to that from the reducing condition of a 2% carbon monoxide atmosphere with an oxygen non-stoichiometry δ of 0.24. At lower temperatures (200 °C), the application of bias reduced the sample much more effectively than a carbon monoxide atmosphere and induced an oxygen non-stoichiometry δ of 0.47. Despite these large changes in oxygen concentration, the epitaxial thin film was completely re-oxidized and no signs of crystallinity loss or film amorphization were observed. This work demonstrates that the effects of oxygen evolution and reduction can be examined with applied bias at low temperatures, extending the ability to probe these processes with in-situ analytical techniques.

36 MATERIALS SCIENCE↗

DOE OSTI2014

Attenuation of wall disturbances in an electron cyclotron resonance oxygen–argon plasma using real time control

Present practice in plasma-assisted semiconductor manufacturing specifies recipes in terms of inputs such as gas flow rates, power and pressure. However, ostensibly identical chambers running identical recipes may produce very different results. Extensive chamber matching, i.e., initial iterative, empirical tuning of the process recipe, which entails time-consuming, ex situ statistical analysis of process metrics such as etch depth, uniformity, anisotropy and selectivity, is required to ensure acceptable results. Once matched, chambers are run open loop and are thus sensitive to disturbances such as actuator drift, wall seasoning and substrate loading, which may impact negatively on process reproducibility. An alternative approach, which may obviate the need for chamber matching and reduce the sensitivity of process metrics to exogenous disturbances, would be to specify a recipe in terms of quantities such as active species densities, and to regulate these in real time by adjusting the inputs with a suitable control algorithm. In this work, real time control of an electron cyclotron resonance O{sub 2}/Ar plasma used for photoresist ashing has been implemented. The design of elementary, model-based algorithms for the control of the argon 750 and oxygen 844 line intensities measured by optical emission spectroscopy is described. Fluorination of the chamber walls by means of an SF{sub 6} plasma prior to ashing inhibits wall recombination of oxygen radicals resulting in an approximately 20% increase in ash rate in the open loop case. However, closed loop control almost completely attenuates the effect of fluorination, thus demonstrating the efficacy of the control algorithms in ensuring a reproducible ash rate in the face of a wall disturbance.

42 ENGINEERING↗

DOE OSTI2017

In situ neutron diffraction analyses of temperature and stresses during friction stir processing of Mg-3Al-1Zn magnesium alloy

In this paper, the evolution of temperature and thermal stresses were examined during friction stir processing of a magnesium alloy using in situ neutron diffraction. Measured total lattice strains were de-convoluted into the thermal and stress components. Finally, it shows the maximum temperature of 464 °C and compressive stress distributions up to -52 MPa underneath the tool via the thermo-mechanical deformation in terms of the Zener-Hollomon parameter of 4.51 × 10 10 s -1 .

36 MATERIALS SCIENCE↗

DOE OSTI2022

Combining Spatial and Temporal Resolution in Cryo-TEM of Device Materials: Preprint

Cryogenic transmission electron microscopy (cryo-TEM) has been instrumental to reducing the effects of electron-beam sample interactions and enabling higher spatial resolution studies of beam sensitive materials. However, the process of thinning and freezing samples for cryo-TEM characterization is often complex and frequently involves removing materials from their environment or stimuli of interest for extended times. This can allow for structural relaxation, diffusion, and other dynamic processes to occur prior to characterization; for energy materials like battery electrodes, this makes it difficult to precisely correlate the imaged structure with native structures that evolve in-situ during device processing, operation, or aging. Here, we present methods to prepare cryo-TEM samples from energy materials during these critical processes in the relevant device lifetimes. This offers insights into improving the temporal resolution of cryo-TEM, while still exploiting its ability to achieve high spatial resolutions in characterizing beam sensitive materials.

BASIC BIOLOGICAL SCIENCES,MATERIALS SCIENCE↗

DOE OSTI2017

Formation of sodium bismuth titanate-barium titanate during solid-state synthesis

Phase formation of sodium bismuth titanate (Na 0.5 Bi 0.5 TiO 3 or NBT) and its solid solution with barium titanate (BaTiO 3 or BT) during the calcination process is studied using in situ high-temperature diffraction. The reactant powders were mixed and heated to 1000°C, while X-ray diffraction patterns were recorded continuously. Phase evolutions from starting materials to final perovskite products are observed, and different transient phases are identified. The formation mechanism of NBT and NBT–xBT perovskite structures is discussed, and a reaction sequence is suggested based on the observations. The in situ study leads to a new processing approach, which is the use of nano-TiO 2 , and gives insights to the particle size effect for solid-state synthesis products. Lastly, it was found that the use of nano-TiO 2 as reactant powder accelerates the synthesis process, decreases the formation of transient phases, and helps to obtain phase-pure products using a lower thermal budget.

36 MATERIALS SCIENCE↗

DOE OSTI2017

A Data Analysis Framework for Earth System Simulation within an In-Situ Infrastructure

This paper presents a generic procedure to implement a scalable and high performance data analysis framework for large-scale scientific simulation within an in-situ infrastructure. It demonstrates a unique capability for global Earth system simulations using advanced computing technologies (i.e ., automated code analysis and instrumentation), in-situ infrastructure (i.e ., ADIOS) and big data analysis engines (i.e ., SciKit-learn). This paper also includes a useful case that analyzes a globe Earth System simulations with the integration of scalable in-situ infrastructure and advanced data processing package. Finally, the in-situ data analysis framework can provides new insights on scientific discoveries in multiscale modeling paradigms.

97 MATHEMATICS AND COMPUTING↗

NASA NTRS1999

Development Unit Configuration and Current Status of the MIP/MTERC Experiment

The Mars In-Situ Propellant Production (ISPP) Precursor (MIP) experiment package is planned for inclusion on the Mars 2001 Lander. This experiment package consists of five experiments whose purpose is to demonstrate the performance of various ISPP processes in-situ on Mars. The demonstrated ability to produce propellant for Mars Return Vehicles (MRV) is considered to be a necessary precursor to any future manned mission to Mars. The Mars Thermal Environment/Radiator Characterization (MTERC) experiment is part of the MIP package and is intended to determine the Mars night sky temperature as well as to characterize the performance degradation of radiators caused by environmental exposure on Mars over time. Radiators are needed as part of the ISPP process to remove heat from the Mars Atmosphere Acquisition and Compression (MAAC) CO2 sorption compressor. MTERC will provide the data needed to optimize the design of radiators for ISPP and other processes. A MTERC Development Unit (DU) has been fabricated and tested at JPL. The MTERC DU consists of 1) a radiator subassembly, 2) a motor/cover subassembly, 3) a differential temperature control circuit and motor control electronics circuit board, and 4) a command and data handling electronics circuit board. This paper will describe the operational theory and the configuration of the MTERC DU and will discuss the current status of the MTERC experiment development including some selected results of performance testing that has been completed prior to the ISRU III meeting.

Juanero, K. J.↗

NASA NTRS1999

Development Unit Configuration and Current Status of the MIP/MTERC Experiment

The Mars In-Situ Propellant Production (ISPP) Precursor (MIP) experiment package is planned for inclusion on the Mars 2001 Lander. This experiment package consists of five experiments whose purpose is to demonstrate the performance of various ISPP processes in-situ on Mars. The demonstrated ability to produce propellant for Mars Return Vehicles (MRV) is considered to be a necessary precursor to any future manned mission to Mars. The Mars Thermal Environment/Radiator Characterization (MTERC) experiment is part of the MIP package and is intended to determine the Mars night sky temperature as well as to characterize the performance degradation of radiators caused by environmental exposure on Mars over time. Radiators are needed as part of the ISPP process to remove heat from the Mars Atmosphere Acquisition and Compression (MAAC) C02 sorption compressor. MTERC will provide the data needed to optimize the design of radiators for ISPP and other processes. A MTERC Development Unit (DU) has been fabricated and tested at JPL. The MTERC DU consists of: (1) a radiator subassembly, (2) a motor/cover subassembly, (3) a differential temperature control circuit and motor control electronics circuit board, and (4) a command and data handling electronics circuit board. This paper will describe the operational theory and the configuration of the MTERC DU and will discuss the current status of the MTERC experiment development including some selected results of performance testing that has been completed prior to the ISRU III meeting.

Juanero, K. J.↗

DOE OSTI2023

Denitrification and the challenge of scaling microsite knowledge to the globe

Here, our knowledge of microbial processes—who is responsible for what, the rates at which they occur, and the substrates consumed and products produced—is imperfect for many if not most taxa, but even less is known about how microsite processes scale to the ecosystem and thence the globe. In both natural and managed environments, scaling links fundamental knowledge to application and also allows for global assessments of the importance of microbial processes. But rarely is scaling straightforward: More often than not, process rates in situ are distributed in a highly skewed fashion, under the influence of multiple interacting controls, and thus often difficult to sample, quantify, and predict. To date, quantitative models of many important processes fail to capture daily, seasonal, and annual fluxes with the precision needed to effect meaningful management outcomes. Nitrogen cycle processes are a case in point, and denitrification is a prime example. Statistical models based on machine learning can improve predictability and identify the best environmental predictors but are—by themselves—insufficient for revealing process-level knowledge gaps or predicting outcomes under novel environmental conditions. Hybrid models that incorporate well-calibrated process models as predictors for machine learning algorithms can provide both improved understanding and more reliable forecasts under environmental conditions not yet experienced. Incorporating trait-based models into such efforts promises to improve predictions and understanding still further, but much more development is needed.

59 BASIC BIOLOGICAL SCIENCES↗

DOE OSTI2015

Additive manufacturing of materials: Opportunities and challenges

Additive manufacturing (also known as 3D printing) is considered a disruptive technology for producing components with topologically optimized complex geometries as well as functionalities that are not achievable by traditional methods. The realization of the full potential of 3D printing is stifled by a lack of computational design tools, generic material feedstocks, techniques for monitoring thermomechanical processes under in situ conditions, and especially methods for minimizing anisotropic static and dynamic properties brought about by microstructural heterogeneity. In this paper, we discuss the role of interdisciplinary research involving robotics and automation, process control, multiscale characterization of microstructure and properties, and high-performance computational tools to address each of these challenges. In addition, emerging pathways to scale up additive manufacturing of structural materials to large sizes (>1 m) and higher productivities (5–20 kg/h) while maintaining mechanical performance and geometrical flexibility are also discussed.

36 MATERIALS SCIENCE↗

DOE OSTI2019

Impact of Catalyst Ink Dispersing Methodology on Fuel Cell Performance Using in-Situ X-ray Scattering

This work presents a study of the effects of ultrasonic dispersing methodology and time on catalyst agglomerate size in polymer electrolyte membrane fuel cell catalyst ink dispersions. Cathode catalyst inks were prepared and characterized to elucidate the influences of ultrasonic dispersing method and time on catalyst ink particle size and CCL electrochemical properties. In situ ultra-small-, small-, and wide-angle X-ray scattering analyses were used to study the impact of ultrasonication time and methodology on changes in the agglomerate, aggregate, and particle size and distribution during the dispersing process. Ex-situ transmission electron microscopy was also used to investigate the particle size of these inks. Fuel cell membrane electrode assemblies (MEAs) were prepared and tested to determine the influence of ink properties on CCL electrochemical properties, including the electrochemical active surface area, mass activity, H2/air polarization curves, and oxygen mass-transport resistances. It was found that a combination of brief tip sonication followed by bath sonication was most effective at breaking up agglomerates, leading to maximum catalyst activity and MEA performance. Extended tip sonication was found to be too aggressive and resulted in detachment of the platinum nanoparticles from the carbon black support, which decreased electrochemical surface area and MEA performance. Quantification of oxygen mass transport resistance showed that electrodes with large catalyst agglomerates due to insufficient sonication had a higher non-Fickian (pressure independent) than properly dispersed catalyst. Through correlation of the performance with catalyst particle size, the desired CCL structure was proposed, which will provide insight into dispersion strategies for lab-scale spray coating and other processing techniques, as well as for large-scale manufacturing.

30 DIRECT ENERGY CONVERSION↗

DOE OSTI2018

Shrink or Substitute: Handling Process Failures in HPC Systems Using In-Situ Recovery

Efficient utilization of today's high-performance computing (HPC) systems with complex software and hardware components requires that the HPC applications are designed to tolerate process failures at runtime. With low mean-time-to-failure (MTTF) of current and future HPC systems, long running simulations on these systems requires capabilities for gracefully handling process failures by the applications themselves. In this paper, we explore the use of fault tolerance extensions to Message Passing Interface (MPI) called user-level failure mitigation (ULFM) for handling process failures without the need to discard the progress made by the application. We explore two alternative recovery strategies, which use ULFM along with application-driven in-memory checkpointing. In the first case, the application is recovered with only the surviving processes, and in the second case, spares are used to replace the failed processes, such that the original configuration of the application is restored. Our experimental results demonstrate that graceful degradation is a viable alternative for recovery in environments where spares may not be available.

Ashraf, Rizwan↗

NASA NTRS2015

In-Situ Resource Utilization for Space Exploration: Resource Processing, Mission-Enabling Technologies, and Lessons for Sustainability on Earth and Beyond

As humanity begins to reach out into the solar system, it has become apparent that supporting a human or robotic presence in transit andor on station requires significant expendable resources including consumables (to support people), fuel, and convenient reliable power. Transporting all necessary expendables is inefficient, inconvenient, costly, and, in the final analysis, a complicating factor for mission planners and a significant source of potential failure modes. Over the past twenty-five years, beginning with the Space Exploration Initiative, researchers at the NASA Glenn Research Center (GRC), academic collaborators, and industrial partners have analyzed, researched, and developed successful solutions for the challenges posed by surviving and even thriving in the resource limited environment(s) presented by near-Earth space and non-terrestrial surface operations. In this retrospective paper, we highlight the efforts of the co-authors in resource simulation and utilization, materials processing and consumable(s) production, power systems and analysis, fuel storage and handling, propulsion systems, and mission operations. As we move forward in our quest to explore space using a resource-optimized approach, it is worthwhile to consider lessons learned relative to efficient utilization of the (comparatively) abundant natural resources and improving the sustainability (and environment) for life on Earth. We reconsider Lunar (and briefly Martian) resource utilization for potential colonization, and discuss next steps moving away from Earth.

Specific impulse↗

DOE OSTI2021

In situ monitoring of microstructure evolution during thermal processing of uranium-zirconium alloys using laser-generated ultrasound

In this study, laser-generated ultrasound was used to monitor microstructure evolution during thermal processing of as-cast, polycrystalline binary uranium-zirconium metallic fuel alloys with compositions of U-20wt.%Zr (U-20Zr), U-50wt.%Zr (U-50Zr) and U-80wt.%Zr (U-80Zr). Ultrasonic waveforms were recorded during heating and cooling the samples from room temperature to >973 K and back. A phase transition temperature for all three compositions was estimated from the temperature at which an abrupt and rapid reduction in ultrasonic velocities was observed. Microstructural features on the length scale of tens of micrometers were inferred from the observation of scattering of ultrasonic waves by elastic heterogeneities above ~823 K in U-20Zr, while a hysteresis in the ultrasonic velocities of U-80Zr upon cooling was attributed to a partial retention of the high temperature phase following thermal annealing. The U-50Zr alloy exhibited a reversible viscoelastic response above 933 K, as evidenced by the observation of high frequency attenuation of the shear component of the waveforms at high temperature. Ultrasonic measurements were supplemented by in situ transmission electron microscopy (TEM). The TEM images revealed that the δ-U-Zr matrix in the three compositions underwent a spinodal decomposition above ~823 K into nanoscale regions. The ultrasonic measurements revealed larger, micron-scale structure evolution in the U-20Zr alloy at the same temperature. This large-scale structure is associated with heterogeneous regions having different Zr content. Our findings show the potential heating rate dependence of microstructural evolution in U-Zr alloys and highlight differences in the thermomechanical response and associated length scales during thermal annealing between single- and dual-phase compositions. These results demonstrate the utility of laser ultrasonics to rapidly and efficiently scan phase boundaries and monitor micrometer-scale structure evolution in metallic fuel alloys.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

DOE OSTI2020

In situ investigation of phosphonate retarder interaction in oil well cements at elevated temperature and pressure conditions

In this paper, the effect of a high-performance retarding additive in oil well cements was investigated under elevated temperature (165°C) and pressure (1000 psi) conditions via in situ synchrotron-based X-ray diffraction (XRD) and quasielastic neutron scattering (QENS) techniques. Under these temperature and pressure conditions, crystalline calcium silicate hydrates (C–S–H) are formed through the cement hydration process. From in situ XRD experiments, the retardation effect was observed by a change in the rate of the appearance of 11 Å tobermorites as well as a change in the rate of the α-C 2 SH generation and depletion. QENS analysis revealed that the retardation effect was related to the non-conversion of free water to chemical and constrained water components. A high presence of free water components was attributed to a decrease in 11Å tobermorites along with slower consumption of the quartz and portlandite phases. Furthermore, QENS results infer that the water molecules experienced confinement in the restricted pore spaces. The retarder inhibited this initial water confinement by slowing the bulk diffusion of free water in the confined region.

36 MATERIALS SCIENCE↗

NASA NTRS1999

Development Unit Configuration and Current Status of the MIP/MAAC Experiment

The Mars In-Situ Propellant Production (ISPP) Precursor (MIP) experiment package is planned for inclusion on the Mars 2001 Lander. This experiment package consists of five experiments whose purpose is to demonstrate the performance of various ISPP processes in-situ on Mars. The demonstrated ability to produce propellant for Mars Return Vehicles (MRV) is considered to be a necessary precursor to any future manned mission to Mars. The Mars Atmosphere Acquisition and Compression (MAAC) experiment is part of the MIP package and is intended to demonstrate that, by using a sorption compressor, CO2 can be preferentially adsorbed at about 6 torr from the Mars atmosphere during the night when the bed is cold then subsequently compressed to about 800 torr by heating the bed and desorbing CO2 during the day. The compressed CO2 produced by MAAC is to be fed to the Oxygen Generator Subsystem (OGS) where pure oxygen is to be produced. Pure oxygen is considered to be one of the primary constituents of a future manned MRV propellant system. A MAAC Development Unit (DU) has been fabricated and tested at JPL. The MAAC DU consists of 1) a sorption bed filled with a CO2 selective sorbent material, 2) a purge system to be used to periodically backflush non-CO2 gases from the sorbent bed during adsorption, 3) a JPL-developed gas-gap heat switch that allows heat transfer to a radiator for heat removal from the bed during the night time adsorption period and that impedes heat transfer during the day time desorption period, 4) a radiator to radiate heat to the night sky during the adsorption period, 5) a set of three isolation valves and connecting tubing. 6) two pressure transducers and several thermocouples for monitoring the MAAC operating conditions, and command and data handling electronics. This paper will describe the operational theory and the configuration of the MAAC DU and will discuss the current status of the MAAC experiment development including some selected results of performance testing that has been completed prior to the ISRU III meeting.

Karlmann, P. B.↗