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Comments on the analysis of returned comet samples

It is argued that returned comet samples should be distributed to individual laboratories for analysis much in the same way that lunar samples are. In the context of emerging technologies, certain developments in other fields which may prove beneficial to the study of comets are reviewed, including cryogenic and tomographic techniques. It is noted that the lack of expertise in the area of cryogenic examination of comet samples is a current weakness in the ability of the extraterrestrial material community to handle comet samples and thus requires further training and preparations. Computer tomography scan images of a 'dirty snowball' are presented to illustrate the importance of developing new methods for comet sample analysis. It is suggested that microanalytic measurements of extraterrestrial samples at the atom-counting limit appear promising for the future.

Walker, Robert M.↗

Pre-Mission Input Requirements to Enable Successful Sample Collection by a Remote Field/EVA Team

This paper is intended to evaluate the sample collection process with respect to sample characterization and decision making. In some cases, it may be sufficient to know whether a given outcrop or hand sample is the same as or different from previous sampling localities or samples. In other cases, it may be important to have more in-depth characterization of the sample, such as basic composition, mineralogy, and petrology, in order to effectively identify the best sample. Contextual field observations, in situ/handheld analysis, and backroom evaluation may all play a role in understanding field lithologies and their importance for return. For example, whether a rock is a breccia or a clast-laden impact melt may be difficult based on a single sample, but becomes clear as exploration of a field site puts it into context. The FINESSE (Field Investigations to Enable Solar System Science and Exploration) team is a new activity focused on a science and exploration field based research program aimed at generating strategic knowledge in preparation for the human and robotic exploration of the Moon, near-Earth asteroids (NEAs) and Phobos and Deimos. We used the FINESSE field excursion to the West Clearwater Lake Impact structure (WCIS) as an opportunity to test factors related to sampling decisions. In contract to other technology-driven NASA analog studies, The FINESSE WCIS activity is science-focused, and moreover, is sampling-focused, with the explicit intent to return the best samples for geochronology studies in the laboratory. This specific objective effectively reduces the number of variables in the goals of the field test and enables a more controlled investigation of the role of the crewmember in selecting samples. We formulated one hypothesis to test: that providing details regarding the analytical fate of the samples (e.g. geochronology, XRF/XRD, etc.) to the crew prior to their traverse will result in samples that are more likely to meet specific analytical objectives than samples collected in the absence of this premission information. We conducted three tests of this hypothesis. Our investigation was designed to document processes, tools and procedures for crew sampling of planetary targets. This is not meant to be a blind, controlled test of crew efficacy, but rather an effort to recognize the relevant variables that enter into sampling protocol and to develop recommendations for crew and backroom training in future endeavors. Methods: One of the primary FINESSE field deployment objectives was to collect impact melt rocks and impact melt-bearing breccias from a number of locations around the WCIS structure to enable high precision geochronology of the crater to be performed [1]. We conducted three tests at WCIS after two full days of team participation in field site activities, including using remote sensing data and geologic maps, hiking overland to become familiar with the terrain, and examining previously-collected samples from other islands. In addition, the team members shared their projects and techniques with the entire team. We chose our "crew members" as volunteers from the team, all of whom had had moderate training in geologic fieldwork and became familiar with the general field setting. The first two tests were short, focused tests of our hypothesis. Test A was to obtain hydrothermal vugs; Test B was to obtain impact melt and intrusive rock as well as the contact between the two to check for contact metamorphism and age differences. In both cases, the test director had prior knowledge of the site geology and had developed a study-specific objective for sampling prior to deployment. Prior to the field deployment, the crewmember was briefed on the sampling objective and the laboratory techniques that would be used on the samples. At the field sites (Fig. 2), the crewmember was given 30 minutes to survey a small section of outcrop (10-15 m) and acquire a suite of three samples. The crewmember talked through his process and the test director kept track of the timeline in verbal cues to the crewmember. At the conclusion, the team member conducting the scientific study appraised the samples and train of thought. Test C was a 90-minute EVA simulation using two crewmembers working out of line-of-sight in communication with a science backroom. The science objectives were determined by the science backroom team in advance using a Gigapan image of the outcrop (Fig. 1). The science team formulated hypotheses for the outcrop units and created sampling objectives for impact-melt lithologies; the science team turned these into a science plan, which they communicated to the crew in camp prior to crew deployment. As part of the science plan, the science team also discussed their sample needs in depth with the crewmembers, including laboratory methods, objectives, and samples sizes needed. During the deployment, the two crewmembers relayed real-time information to the science backroom by radio with no time delay. Both the crew and science team re-evaluated their hypotheses and science plans in real-time. Discussion: Upon evaluation, we found that the focused tests (Tests A and B) were successful in meeting their scientific objectives. The crewmember used their knowledge of how the samples were to be used in further study (technique, sample size, and scientific need) to focus on the sampling task. The crewmember was comfortable spending minimal time describing and mapping the outcrop. The crewmember used all available time to get a good sample. The larger test was unsuccessful in meeting the sampling objectives. When the crewmembers began describing the lithologies, it was quickly apparent that the lithologies were not as the backroom expected and had communicated to the crew. When the outcrop wasn't as expected, the crew members instinctively switched to field characterization mode, taking significant time to characterize and map the outcrop. One crew member admitted that he "kind of lost track" of the sampling strategy as he focused on the basic outcrop characterization. This is the logical first step in a field geology campaign, that a significant amount of time must be spent by the crew and backroom to understand the outcrop and its significance. Basic field characterization of an outcrop is a focused activity that takes significant time and training [2, 3]. Sampling of representational lithologies can be added to this activity for little cost [4]. However, we have shown that identification of unusual or specific samples for laboratory study also takes significant time and knowledge. We suggest that sampling of this type be considered a separate activity from field characterization, and that crewmembers be trained in sampling needs for different kinds of studies (representative lithologies vs. specialized samples) to acquire a mindset for sampling similar to field mapping. Sampling activities should be given a significant amount of specifically allocated time in scheduling EVA activities; and in the better case, that sampling be done as a second activity to a previously studied outcrop where both crew and backroom are comfortable with its context and characteristics. Our hypothesis posited that crewmember knowledge of how the samples would be used upon return would aid them in choosing relevant samples. Our testing bore this hypothesis out to some extent. We therefore recommend that crewmember training should include exposure to the laboratory techniques and analyses that will be used on the samples to foster this knowledge. There is also the potential for increasing crewmember contextual knowledge real-time in the field through the introduction of in situ geochemical technologies such as field portable XRF. The presence of field portable geochemical technology could enable the astronauts to interrogate the samples for K abundance real-time, ensuring they could collect valuable and dateable samples [5]. Though simulations such as these can teach us a fair bit about decision making processes and timeline building, one EVA participant noted that when he wasn't collecting "real" samples, he wasn't at his best. This effect suggests that higher-fidelity studies involving truly remote participants conducting actual scientific studies merit further attention to capture lessons for application to future crew situations.

sample collection↗

Preparation, analysis and release of simulated interplanetary grains into low Earth orbit

Astronomical observations which reflect the optical and dynamical properties of interstellar and interplanetary grains are the primary means of identifying the shape, size, and the chemistry of extraterrestrial grain materials. Except for recent samplings of extraterrestrial particles in near-Earth orbit and in the stratosphere observations were the only method of deducing the properties of extraterrestrial particles. In order to elucidate the detailed characteristics of observed dust, the observations must be compared with theoretical studies, some of which are discussed in this volume, or compared with terrestrial laboratory experiments. The formation and optical characterization of simulated interstellar and interplanetary dust with particular emphasis on studying the properties on irregularly shaped particles were discussed. Efforts to develop the techniques to allow dust experiments to be carried out in low-Earth orbit were discussed, thus extending the conditions under which dust experiments may be performed.

Stephens, J. R.↗

Ionic Liquids in Analytical Chemistry: Fundamentals, Technological Advances, and Future Outlook

The development of new analytical methods most often focus on novel materials used to impart selectivity or sensitivity to the protocol. Ionic liquids (ILs) are a class of solvents that have been extensively explored as promising materials for various applications and continue to be explored due to their tunable physicochemical properties. These materials possess melting temperatures below 100 °C and can interact with analytes through a multitude of interactions afforded by their readily tunable chemical structure. These interactions include electrostatic, dispersive, hydrogen bonding, π–π, and dipolar interactions and can be modulated or strengthened based on the functional groups present within the chemical structure. ILs consist predominately of organic cations and either inorganic or organic anions, both of which can be functionalized with desired moieties. Common cation and anions found in IL chemical structures are presented in Figure 1. The unique polarity afforded by the ionic structure has also led to their increasing use in areas including sample preparation, chemical separations, electrochemistry, mass spectrometry, and spectroscopy.

Zeger, Victoria R. [Iowa State Univ., Ames, IA (Un↗

Novel High Barrier Films for Packaging Food and Medicine

Long manned missions require food packaging to maintain food safety, nutrition, and acceptability for the length of 3-5 years1,2 while the shelf life assigned by NASA for current provisions is 18-24 months1. The focus of this design project was to make a polymer film specifically to function as a high oxygen barrier to later be included in an improved multi-layer packaging system of other specialized polymers with capabilities to allow for a 5-year shelf-life. To qualify as a high oxygen barrier film and to be a successful design for the future packaging, the resulting film is required to have an oxygen transmission rate (OTR) less than 0.06 cc/ m2/24 hr/atm, the standard for the current packaging3. This new film was designed to have a decreased permeability by increasing the “tortuous path” a gas molecule travels to permeate through a film. The increase in the “tortuous path” of a gas molecule is accomplished by introducing a 2D material additive. The additive chosen for this project was hexagonal boron nitride (h-BN) which exfoliates into boron nitride nanosheets (BNNs). Nylon 6 was chosen as the candidate for the matrix. This project is required to determine the best methods to synthesize the sample film and then to test the OTR of the film to determine if this design was successful. This project examined methods for pulverizing polymer resin pellets, h-BN exfoliation, and film fabrication using a hot press. This report includes the exfoliation and analysis of h-BN, procedural preparations for films, and a modeling study of estimated OTR of the h-BN/Nylon. The work in this report did not yield a high barrier composite film because of the laboratory closure in response to COVID -19 guidance but provides a concise method of the additive preparation and film synthesis. This gives a good starting point for future research in high barrier films by 2D additive composites.

Polymer, Nylon, PET, boron nitride, nanocomposite↗

Microstructural evaluation of thin-wall sections of 316L stainless steel produced by laser powder-bed fusion processing

The synthesis of thin wall sections that are only 0.4 mm thick is achieved with LPBF AM. Sample preparation is optimized using metallographic polishing to produce samples with only 0.3 um rms roughness for scanning electron microanalysis with EBSD and EDS. A fully austenitic 316L phase is found without evidence of secondary phases. Unlike some AM products that can readily evidence composition segregation due to solute rejection as attributable to temperature gradients within the solidification

Jankowski, Alan F. [Sandia National Laboratories (↗

Argonne National Laboratory Site Environmental Report for Calendar Year 2024

This report discusses the status and accomplishments of the environmental protection program at Argonne National Laboratory for calendar year 2024. The status of Argonne environmental protection activities with respect to compliance with the various laws and regulations is discussed, along with environmental management, efficiency efforts, environmental corrective actions, and habitat restoration. To evaluate the effects of Argonne operations on the environment, samples of environmental media collected on the site, at the site boundary, and off the Argonne site were analyzed and compared with applicable guidelines and standards. A variety of radionuclides were measured in air, surface water, groundwater, and bottom sediment samples. In addition, chemical constituents in surface water, groundwater, and wastewater were analyzed. External penetrating radiation doses were measured, and the potential for radiation exposure to off-site population groups and on-site members of the public was estimated. Results are interpreted with respect to the origin of radioactive and chemical substances (i.e., natural, Argonne, and other) and are compared with applicable standards intended to protect human health and the environment. A U.S. Department of Energy (DOE) dose calculation methodology, based on International Commission on Radiological Protection (ICRP) recommendations and the U.S. Environmental Protection Agency’s (EPA) CAP 88 computer code, was used in preparing this report.

54 ENVIRONMENTAL SCIENCES↗

High-resolution analysis of clay minerals and amorphous materials in martian analog environments

Mudrocks and mud-sized sediments (i.e., silt to clay) dominate the surface of Earth and Mars. These fine-grained sediments preserve a rich history of sedimentary processes from source to sink and shed light on ancient climates. However, both the physical and chemical nature of these materials make them difficult to fully characterize with traditional laboratory techniques. Here, we explore a cross-disciplinary and high-resolution approach using synchrotron radiation for X-ray diffraction, pair distribution function analysis, and submicrometer-scale X-ray fluorescence, combined with transmission electron microscopy, to better understand the nanostructure and composition of mud-sized sediments from a glacio-fluvial watershed in southwest Iceland. Our results demonstrate that sediments in the cold and wet climate of Iceland are more altered than previously thought, as evidenced by the identification of kaolinite and mixed-layer kaolinite-smectite. Additionally, sediments are enriched in amorphous materials and nanocrystalline phases, as determined from grain morphologies and compositions consistent with allophane, hisingerite, ferrihydrite, and halloysite. These alteration products are present as intimate mixtures that vary across depositional sites, demonstrating the dynamic nature of the secondary assemblage from source to sink. This work has implications for Mars, where, for example, basalt-sourced sedimentary rocks from Gale crater are abundant in clay minerals and amorphous materials. Finally, this work underpins the importance of using high-resolution techniques, a coordinated methodology, and developing innovative approaches for future planetary sample return missions (e.g., Mars sample return).

36 MATERIALS SCIENCE↗

Phase stability and microstructure of neutron-irradiated substoichiometric yttrium dihydrides

The impact of the neutron-displacement damage on phase stability and microstructure of substoichiometric yttrium dihydrides (YH x , x <2) were investigated to assess their use as solid moderator in high-temperature nuclear reactors. YH x specimens were, thus, subjected to neutron irradiations in the range of 0.1–2 displacements per yttrium atom (dpa-Y) in the temperature range of 536–878°C at the Oak Ridge National Laboratory's (ORNL's) High Flux Isotope Reactor (HFIR). YH x specimens were initially prepared at stoichiometry (H/Y) ratios of 1.69 and 1.83. HFIR-irradiated specimens were characterized by variety of techniques to investigate H retention characteristics including dimensional analysis, optical microscopy, scanning electron microscopy electron back scatter diffraction (EBSD), transmission electron microscopy, thermal desorption spectroscopy (TDS), and high-energy x-ray diffraction (HE-XRD) characterizations. Overall, YH x exhibited notable structural and phase stability under short-term neutron-irradiation, except for the samples with significant silicon carbide (SiC) interaction at high doses and temperatures. Basic dimensional and mass measurements were misleading for accurate assessment of H retention, as confirmed by EBSD phase maps, XRD line profiles, and TDS signals. Thus, it was discussed that a robust H retention metric is needed to assess irradiated hydrides. Further, nanoscale cavities were observed as a result of the neutron irradiation in all samples. Although no clear impact of dose and irradiation temperature was determined, the initial H/Y ratio had an impact on the cavity number density where low H/Y specimens had high-resistance to cavity formation. The Y-vacancy cluster formation at the collision stage of the displacement cascade and their stabilization by H were considered to be the likely underlying mechanisms for the observed cavity microstructure.

22 GENERAL STUDIES OF NUCLEAR REACTORS↗

Engineering diamond interfaces free of dark spins

Nitrogen-vacancy (NV) centers in diamond are utilized extensively as quantum sensors for imaging fields at the nanoscale. The ultrahigh sensitivity of NV magnetometers has enabled the detection and spectroscopy of individual electron spins, with potentially far-reaching applications in condensed matter physics, spintronics, and molecular biology. However, the surfaces of these diamond sensors naturally contain electron spins, which create a background signal that can be hard to differentiate from the signal of the target spins. In this study, we develop a surface modification approach that eliminates the unwanted signal of these so-called dark electron spins. Our surface passivation technique, based on coating diamond surfaces with a thin titanium oxide (Ti⁢O 2 ) layer, reduces the dark spin density. The observed reduction in dark spin density aligns with our findings on the electronic structure of the diamond-Ti⁢O 2 interface. The reduction, from a typical value of 2000 μm −2 to a value below that set by the detection limit of our NV sensors (200 μm −2 ), results in a twofold increase in Hahn-echo coherence time of near surface NV centers. Furthermore, we derive a comprehensive spin model that connects dark spin relaxation with NV coherence, providing additional insights into the mechanisms behind the observed spin dynamics. Our findings are directly transferable to other quantum platforms, including nanoscale solid-state qubits and superconducting qubits.

74 ATOMIC AND MOLECULAR PHYSICS↗

Plutonium-238 Loadout Calorimeter Return To Service

The calorimeter in the transfer area in Building 7920 at the US Department of Energy’s Oak Ridge National Laboratory is used to measure the amount of 238 Pu in the Plutonium Heat Source Oxide. The calorimetry measurement is taken after the oxide is packaged in an ORISC (Oak Ridge Inner Shipping Capsule)/FSO (Fuel Storage Outer) assembly before loading into the Containment Vessel and shipping container. The equipment is used in three specific configurations: zero measurement (nothing in the sample cup), FSO measurement (actual measurement of 238 Pu), and reference calibration measurement (using the reference FSO as a known heat source). System checks were performed in July 2023 in preparation for scheduled material loadout. During these checks, personnel discovered that the reference FSO had experienced an electrical short in the heater cable and was no longer functional. The calorimeter was in the reference calibration measurement configuration at this time. Facility management was notified when the damage was discovered. The data from the Yokogawa recorder were pulled and analyzed for a span of time between September 2022 and July 2023. An unusual spike was found in the sample cup temperature data that started on October 19, 2022, and ended on October 20, 2022. The sample cup reached a temperature of 191.1°C. The maximum allowable temperature for the calorimeter thermopile to reach is 220°C based on the manufacturer statement provided in Appendix B of this report [1]. The calorimeter thermopile and the sample cup thermocouple are physically close to each other; therefore, the data suggest that the calorimeter itself never saw a temperature in excess of 191.1°C. Physical damage present on the cable, tape, and insulation suggests that the temperature reached a higher value in some locations within the sample cup than the data shows. Because of this discrepancy, testing of the calorimeter was required to confirm that the calorimeter is functioning the same as it was before the electrical short. The intent of this report is to assess the functionality of the calorimeter and determine if it is acceptable to use for 238 Pu loadout material measurement. Testing showed that the calorimeter is functionally equivalent to the initial calibration that was performed in the summer of 2021, and thus, the calorimeter was cleared to be used for its intended purposes.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗

Variable Pressure - Scanning Electron Microscopy (VP-SEM)

Variable Pressure (or Environmental) Scanning Electron Microscopy (VP-SEM) combined with Energy Dispersive X-ray Spectroscopy (EDS) is one of the most powerful methods for characterizing the sub-micron topography and chemical composition of uncoated samples. Terrestrially, VP-SEM is extensively used to non-destructively study geologic and manufactured materials with high spatial resolution (tens of nanometers) and large depth-of-field. An SEM offers a geologist a first survey of microscopic mineral phases via secondary electron imaging (SEI), which provides a topographic look at a sample, as well as backscattered electron (BEI) imaging, which contrasts the phases present based on their geochemistry (atomic number). A VP-SEM utilizes a gas in the sample chamber as a charge dissipation and signal amplification method, allowing analysis of a sample without preparation in the form of a conductive coating. A miniaturized VP-SEM operating in-situ on a lander or rover would be able to use the CO2-rich Martian atmosphere (e.g., Nier et al., 1976; Williams 2016) as an imaging medium for this purpose. Adaptation of a VP-SEM for in-situ Mars surface studies will provide a new imaging capability (via SEI) that is at least an order of magnitude higher resolution than the Mars Hand Lens Imager (MAHLI) on the Mars Science Laboratory (Williams et al., 2015), and equal to or better than the achieved resolution of the Atomic Force Microscope on the Phoenix Mars lander (Pike et al., 2011). In addition, the MVP-SEM is capable of BSI and simultaneous chemical analysis of the imaged region. In this sense, the MVP-SEM can be regarded as an instrument suite that will provide a new set of information not achievable by any other instrument. The Miniaturized Variable Pressure Scanning Electron Microscope (MVP-SEM) was designed, built, and benchtop tested by a team at NASA’s Marshall Space Flight Center and Jet Propulsion Laboratory (JPL), Jacobs Space Exploration Group, Applied Physics Technologies, Inc. (AP-Tech), and Creare LLC, working with a team of technical and science collaborators. Benchtop testing was successful, proving concept feasibility. To date, the MVP-SEM has achieved an imaging resolution of <100 nm in the lab, and with continued optimization, even better performance (~50 nm resolution) is possible. Use in-situ on the lunar or other planetary surfaces would require some redesign to optimize instrument performance, but such an instrument would be equally useful.

Variable Pressure Scanning Electron Microscopy↗

Miniature Variable Pressure - Scanning Electron Microscopy (MVP-SEM)

Variable Pressure (or Environmental) Scanning Electron Microscopy (VP-SEM) combined with Energy Dispersive X-ray Spectroscopy (EDS) is one of the most powerful methods for characterizing the sub-micron topography and chemical composition of uncoated samples. Terrestrially, VP-SEM is extensively used to non-destructively study geologic and manufactured materials with high spatial resolution (tens of nanometers) and large depth-of-field. An SEM offers a geologist a first survey of microscopic mineral phases via secondary electron imaging (SEI), which provides a topographic look at a sample, as well as backscattered electron (BEI) imaging, which contrasts the phases present based on their geochemistry (atomic number). A VP-SEM utilizes a gas in the sample chamber as a charge dissipation and signal amplification method, allowing analysis of a sample without preparation in the form of a conductive coating. A miniaturized VP-SEM operating in-situ on a lander or rover would be able to use the CO2-rich Martian atmosphere (e.g., Nier et al., 1976; Williams 2016) as an imaging medium for this purpose. Adaptation of a VP-SEM for in-situ Mars surface studies will provide a new imaging capability (via SEI) that is at least an order of magnitude higher resolution than the Mars Hand Lens Imager (MAHLI) on the Mars Science Laboratory (Williams et al., 2015), and equal to or better than the achieved resolution of the Atomic Force Microscope on the Phoenix Mars lander (Pike et al., 2011). In addition, the MVP-SEM is capable of BSI and simultaneous chemical analysis of the imaged region. In this sense, the MVP-SEM can be regarded as an instrument suite that will provide a new set of information not achievable by any other instrument. The Miniaturized Variable Pressure Scanning Electron Microscope (MVP-SEM) was designed, built, and benchtop tested by a team at NASA’s Marshall Space Flight Center and Jet Propulsion Laboratory (JPL), Jacobs Space Exploration Group, Applied Physics Technologies, Inc. (AP-Tech), and Creare LLC, working with a team of technical and science collaborators. Benchtop testing was successful, proving concept feasibility. To date, the MVP-SEM has achieved an imaging resolution of <100 nm in the lab, and with continued optimization, even better performance (~50 nm resolution) is possible. Use in-situ on the lunar or other planetary surfaces would require some redesign to optimize instrument performance, but such an instrument would be equally useful.

Variable Pressure Scanning Electron Microscopy↗

Laboratory studies of the diffuse reflectance spectra of frosts and minerals occurring on astronomical objects

A vacuum monochromator was integrated into the system and optics chosen to increase data collection in the infrared spectral region. Using a InSb detector, good reflectance data was obtained to 5.5 micron from a variety of samples including magnesium oxide, barium sulfate, water frost and Bloedite. Magnesium oxide was found to be a poorer reflector than the barium sulfate throughout the visible and near infrared region. The barium sulfate material was shown to be a Lambert reflector in the visible region and over an angular range of 60 deg. Several samples of water frost were prepared and in reflectance measured from 0.3 micron to 5.5 microm. The fine grained frosts were better reflectors than the coarse grained frosts, usually by 20 percent or more, over the entire spectral range. The minerals Bloedite and sulfur were also investigated further.

Glaser, F. M.↗

Materials Characterization, Prediction, and Control Project: Summary Report on Material Characterization, Part 1

The Pacific Northwest National Laboratory (PNNL) undertook the Materials Characterization, Prediction, and Control (MCPC) Laboratory Directed Research and Development Project to advance understanding of nuclear material processing and enable multifold acceleration in the development and qualification of new material systems in national security and advanced energy applications (Smith 2021). The MCPC Project executed research across three scientific vertices—material characterization, predictive modeling, and data analytics—with extensive support by a data curation and management team. The central technical objective in the MCPC Project was to improve the prediction and characterization of the process-structure-property relationships within the microstructurally refined region of stainless-steel samples prepared utilizing friction stir processing (FSP). Application of the FSP technique is well established at PNNL within the Solid Phase Processing capability through many years of investment across a range of materials and applications (PNNL 2024). Three distinct rounds of FSP experiments were performed by the experimental team, producing replicate samples utilizing across different nominal processing conditions (Condition IDs) listed in Table 1. The starting material on which FSP was applied was commercially available unprocessed stainless-steel type 316L material. Chosen processing conditions were very diverse, and some were intentionally chosen to produce defects. Several samples experienced tool breakage during experimentation, so a full set of three replicates was not produced for every nominal processing condition.

36 MATERIALS SCIENCE↗

Materials Characterization, Prediction, and Control Project: Summary Report on Material Characterization, Part 2

The Pacific Northwest National Laboratory (PNNL) undertook the Materials Characterization, Prediction, and Control (MCPC) Laboratory Directed Research and Development Project to advance understanding of nuclear material processing and enable multifold acceleration in the development and qualification of new material systems in national security and advanced energy applications (Smith 2021). The MCPC Project executed research across three scientific vertices—material characterization, predictive modeling, and data analytics—with extensive support by a data curation and management team. The central technical objective in the MCPC Project was to improve the prediction and characterization of the process-structure-property relationships within the microstructurally refined region of stainless-steel samples prepared utilizing friction stir processing (FSP). Application of the FSP technique is well established at PNNL within the Solid Phase Processing capability through many years of investment across a range of materials and applications (PNNL 2024).

36 MATERIALS SCIENCE↗

Materials Characterization, Prediction, and Control Project: Summary Report on Material Characterization, Part 3

The Pacific Northwest National Laboratory (PNNL) undertook the Materials Characterization, Prediction, and Control (MCPC) Laboratory Directed Research and Development Project to advance understanding of nuclear material processing and enable multifold acceleration in the development and qualification of new material systems in national security and advanced energy applications (Smith 2021). The MCPC Project executed research across three scientific vertices—material characterization, predictive modeling, and data analytics—with extensive support by a data curation and management team. The central technical objective in the MCPC Project was to improve the prediction and characterization of the process-structure-property relationships within the microstructurally refined region of stainless-steel samples prepared utilizing friction stir processing (FSP). Application of the FSP technique is well established at PNNL within the Solid Phase Processing capability through many years of investment across a range of materials and applications (PNNL 2024).

36 MATERIALS SCIENCE↗

Materials Characterization, Prediction, and Control Project: Summary Report on Material Characterization, Part 4

The Pacific Northwest National Laboratory (PNNL) undertook the Materials Characterization, Prediction, and Control (MCPC) Laboratory Directed Research and Development Project to advance understanding of nuclear material processing and enable multifold acceleration in the development and qualification of new material systems in national security and advanced energy applications (Smith 2021). The MCPC Project executed research across three scientific vertices—material characterization, predictive modeling, and data analytics—with extensive support by a data curation and management team. The central technical objective in the MCPC Project was to improve the prediction and characterization of the process-structure-property relationships within the microstructurally refined region of stainless-steel samples prepared utilizing friction stir processing (FSP). Application of the FSP technique is well established at PNNL within the Solid Phase Processing capability through many years of investment across a range of materials and applications (PNNL 2024).

36 MATERIALS SCIENCE↗