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All sourcesNASA NTRSDOE OSTI
NASA NTRS2005

In Situ Resource Utilization (ISRU) Experiments for Mars Exploration

In situ resource utilization can best be described as living off the land. In our case the land is the planet Mars. ISRU is based on the idea that some fraction of the consumables, life support and propellant materials do not have to be flown from earth. Rather, they can be manufactured or extracted from resources already present on Mars. The primary resources on Mars are the atmosphere, polar caps and regolith. The atmosphere of Mars is mostly carbon dioxide as shown in the table below. The proportion of oxygen on the other hand is quite small. Still, there is quite a bit of oxygen in the Martian atmosphere, but it is unfortunately tied up with carbon. Thus, one of the goals of ISRU is the separation of breathable oxygen from the carbon dioxide. Several means of separation have been proposed. We have begun experiments on another approach for production of oxygen with carbon monoxide as a useful by product. Our work on a CO2 separator is described later in this report. Regolith melting is another means of obtaining materials. Two materials of interest are iron and silicon. Iron oxide is plentiful on Mars and is of obvious importance for structural components. Silicon is the foundation of solid state devices. Power generation on Mars may be accomplished using silicon solar cells. There is discussion of the feasibility of in situ production of solar cells. This would require a means of extracting silicon from the regolith. We have conducted several experiments concerning melting and glassification of the Mars soil simulant. Other summer faculty fellows have tried various means of processing the stimulant material. These include furnace melting, microwave melting and laser ablation. We have conducted several furnace melting experiments in both air and carbon dioxide environments. We have also carried out experiments to test spark melting in a carbon dioxide atmosphere. These experiments suggest the possibility of using arc melting in a reducing atmosphere. It is important to keep in mind that we are working with a soil stimulant. Any simulant, no matter how chemically similar it is to Martian regolith, may differ in mineralogy. The underlying assumption in this work is that once a glass is formed, any differences between simulant and regolith are unimportant. The exact means of forming the glass do, however, depend on the mineralogy of the regolith. A sample return mission is required to help answer these questions.

Marone, Matt↗
DOE OSTI2025

Investigating the Effect of Water on the Mechanical Properties of Cellulose from Multiscale Molecular Dynamics Simulations

Classical molecular dynamics (MD) simulations provide insight into the structure and physicochemical properties of materials with atomic resolution. However, the length and time scales accessible to atomistic MD are orders of magnitude smaller than many relevant processes such as the response of a bulk material to experimentally accessible strain rates, which presents challenges when comparing models to experimental measurements. Bottom-up coarse-graining provides a means for systematically mapping atomistic information to lower resolution models to increase the length and time scales achievable by simulation. Cellulose is an abundant carbohydrate biopolymer with applications to many fields of research, such as materials science and renewable energy, due to its desirable mechanical properties and viability for conversion into biofuel. The effect of moisture content on the Young's modulus of cellulose is of special interest due to its native environment often being in the hydrated secondary plant cell wall and the grinding energy requirements for biomass feedstock preprocessing. The current work investigates the effects of water solvent on the Young's modulus of cellulose calculated from coarse-grained MD mechanical stress simulations. The coarse-grained model was parametrized from atomistic MD calculations of cellulose-cellulose potentials of mean force using umbrella sampling techniques under vacuum and solvated conditions. The Young's moduli of the coarse-grained cellulose assemblies parametrized from cellulose in vacuum or solvated in water were computed via mechanical stress simulations to highlight the importance of capturing solvent interactions for modeling the mechanical behavior of cellulose.

BASIC BIOLOGICAL SCIENCES,RADIATION PROTECTION AND↗
NASA NTRS2005

Overview of Biomineralization and Nanobacteria

Biomineralization is a frequently used term in nanotechnology, astrobiology, geology, and medicine. In the process of biomineralization, a living organism provides a chemical environment that controls the nucleation and growth of unique mineral phases. Often these materials exhibit hierarchical structural order, leading to superior physical properties, not found either in their inorganic counterparts or in synthetic materials. Biomineralization is widespread in the biosphere and hundreds of different minerals are produced or assisted by a variety of organisms from bacteria to humans. Teeth, bones, kidney stones, and skeletons of algae, mussels, and magnetotactic bacteria are all examples of biomineralization. We do not fully understand the control mechanism of biomineralization either in primitive or in developed organisms. The presence of organic molecules, among other characteristics, can influence the coherence length for X-ray scattering in biogenic crystals. Control over biomineral properties can be accomplished at a myriad of levels, including the regulation of particle size, shape, crystal orientation, polymorphic structure, defect texture, and particle assembly. In the latter case, cellular processes enable control in both the spatial and temporal domain in such a way that hierarchical composite structures can be built which increase the toughness and durability of the material, which is invaluable for load-bearing materials such as bones, teeth, mollusk shells, etc. Durability of biominerals produces remarkably preserved bacterial and cyanobacterial microfossils from billions of years-old samples. The differentiation between microfossils and nonbiogenic artifacts has been a lively discussion subject in astrobiology especially in the last decade. Clearly, more detailed information on the mechanism of biomineralization, and the effect of organic matter on crystal formation/fossilization would help focus such discussions.

Ciftcioglu, N.↗
NASA NTRS2013

NASA Tech Briefs, Februrary 2013

Topics covered include: Measurements of Ultra-Stable Oscillator (USO) Allan Deviations in Space; Gaseous Nitrogen Orifice Mass Flow Calculator; Validation of Proposed Metrics for Two-Body Abrasion Scratch Test Analysis Standards; Rover Low Gain Antenna Qualification for Deep Space Thermal Environments; Automated, Ultra-Sterile Solid Sample Handling and Analysis on a Chip; Measuring and Estimating Normalized Contrast in Infrared Flash Thermography; Spectrally and Radiometrically Stable, Wideband, Onboard Calibration Source; High-Reliability Waveguide Vacuum/Pressure Window; Methods of Fabricating Scintillators With Radioisotopes for Beta Battery Applications; Magnetic Shield for Adiabatic Demagnetization Refrigerators (ADR); CMOS-Compatible SOI MESFETS for Radiation-Hardened DC-to-DC Converters; Silicon Heat Pipe Array; Adaptive Phase Delay Generator; High-Temperature, Lightweight, Self-Healing Ceramic Composites for Aircraft Engine Applications; Treatment to Control Adhesion of Silicone-Based Elastomers; High-Temperature Adhesives for Thermally Stable Aero-Assist Technologies; Rockballer Sample Acquisition Tool; Rock Gripper for Sampling, Mobility, Anchoring, and Manipulation; Advanced Magnetic Materials Methods and Numerical Models for Fluidization in Microgravity and Hypogravity; Data Transfer for Multiple Sensor Networks Over a Broad Temperature Range; Using Combustion Synthesis to Reinforce Berms and Other Regolith Structures; Visible-Infrared Hyperspectral Image Projector; Three-Axis Attitude Estimation With a High-Bandwidth Angular Rate Sensor Change_Detection.m; AGATE: Adversarial Game Analysis for Tactical Evaluation; Ionospheric Simulation System for Satellite Observations and Global Assimilative; Modeling Experiments (ISOGAME); An Extensible, User- Modifiable Framework for Planning Activities; Mission Operations Center (MOC) - Precipitation Processing System (PPS) Interface Software System (MPISS); Automated 3D Damaged Cavity Model Builder for Lower Surface Acreage Tile on Orbiter; Mixed Linear/Square-Root Encoded Single-Slope Ramp Provides Low-Noise ADC with High Linearity for Focal Plane Arrays; RUSHMAPS: Real-Time Uploadable Spherical Harmonic Moment Analysis for Particle Spectrometers; Powered Descent Guidance with General Thrust-Pointing Constraints; X-Ray Detection and Processing Models for Spacecraft Navigation and Timing; and Extreme Ionizing-Radiation-Resistant Bacterium

Source record↗
NASA NTRSDate not supplied

A New Coordinated NanoSIMS, Transmission Electron Microscopy and Atom Probe Tomography Approach For the Characterization of Primitive Astromaterials

Presolar grains are remnants of evolved stellar systems preserved within primitive extraterrestrial materials. They are important for studying physical and chemical processing, and formation mechanisms occurring within the interstellar medium, Solar Nebula and their parent stellar environments [1]. Our recent work has shown coordinated nano-scale Secondary Ion Mass Spectrometry (NanoSIMS) and Atom Probe Tomography (APT) can show isotopic and chemical signatures at major to trace levels, morphological signatures, and regional contextual relationships [2,3]. Previous studies have shown Transmission Electron Microscopy (TEM) of Focus Ion Beam (FIB) TEM lamella, can provide localized contextual relationships, crystallographic information and chemical information [1]. Coordinating NanoSIMS, TEM, and APT could gain access to almost all contextual, structural and geochemical signatures within each presolar grain. However, this has proved challenging owing to the preparation requirements for TEM and APT. For example, studying specimen prepared as APT needles in TEM removes the local context, the higher degree of surface exposure can alter the chemistry of beam sensitive materials, and the shank angle of the needle can impact the quality of TEM diffraction images. We designed a new FIB method which takes a 100 nm thick FIB-TEM lamella and sandwiches it between two indium slices (5 μm x ~300 nm x 3 μm). The indium is melted onto the lamella surface using the electron beam (Fig 1). This process adds bulk to the lamella, making it more amenable to APT needle formation (Fig 2). Consequently, samples can be prepared per the optimal requirements for each technique improving data quality, acquisition stability, and access to the signatures and relationships summarised earlier. This technique can be used for measuring multiple phases across a TEM lamella and targeting an individual phase. For example, a presolar grain identified in NanoSIMS could be targeted, studied in TEM and then indium sandwiched with its precise location in the TEM lamella marked using a Pt button for preparation of an APT needle and atomic scale acquisition. [1] A. M. Davis (2014) Meteorites and cosmochemical processes, 1. [2] Nevill N. et al. (2023) LPSC, 54, #1707. [3] Nevill N. et al. (2023) LPSC, 54, #1714.

NanoSIMS↗
DOE OSTI2025

Single Crystalline Na 0.67 Ni 0.33 Mn 0.67 O 2 Positive Electrode Material via Molten Salt Synthesis for Sodium Ion Batteries

P2-layered Na 0.67 Ni 0.33 Mn 0.67 O 2 (NNMO) has emerged as a promising positive electrode material for sodium ion batteries due to its appealing electrochemical properties. Synthesis of polycrystalline NNMO (PC-NNMO) materials through conventional calcination of solid precursors remains the prevailing method, where heating occurs in a dry environment with air or O 2 . On the other hand, the molten salt method, where precursors are submerged in molten salt medium during calcination, emerged in recent years to be a scalable technique for more controlled crystal growth and uniform morphology in a variety of materials. Here, we utilize the molten salt method to synthesize single crystalline NNMO (SC-NNMO) materials with enhanced electrochemical properties. The SC-NNMO material exhibits an initial specific discharge capacity of 95 mAh g –1 at a 0.1C rate, retaining approximately 88.5% of its capacity after 100 cycles over a wide voltage range of 2.0–4.2 V. Furthermore, SC-NNMO maintains a capacity retention of 83.9% after 300 cycles at a 1C rate compared to 66.6% for PC-NNMO, indicating excellent long-term cycling stability. This stability is further confirmed by the performance of an SC-NNMO//hard carbon full cell, which retains 90.3% of its capacity after 200 cycles at 1C within a voltage window of 1.9–4.1 V. The enhancement in stability of the SC-NNMO sample is attributed to the single crystalline structure suppressing the undesired P2–O2 phase transition at high voltage. This study also presents an easy, efficient, and straightforward molten salt process for SC-NNMO material synthesis, offering valuable insights into the potential application of such methodology for the large-scale, cost-effective production of various sodium-layered transition metal oxide positive electrode materials for SIBs.

72 PHYSICS OF ELEMENTARY PARTICLES AND FIELDS↗
NASA NTRSDate not supplied

Chemical Reactivity of In-Situ Lunar Dust for Biotoxicity Assessment

Introduction: How does the chemical reactivity of in-situ lunar dust compare to Apollo samples currently stored in curation facilities here on Earth? Essential investigations of this question will help us to further mitigate exploration risks for future human explorers on the Moon and will also provide critical information for astrobiologists and space biologists using the Moon for scientific inquiry. Discussion: Apollo 14 dust biotoxicity studies, carried out by the NASA Lunar Airborne Dust Toxici-ty Assessment Group (LADTAG), included numerous physiochemical studies[1] and cellular and animal ex-periments. Intratracheal instillation [2] and inhalation studies [3] in rats both showed Apollo 14 dust to be intermediate in toxicity compared to low-tox titanium dusts and high-tox quartz dusts of similar particle siz-es. The collective results were used in models [4] to establish a safe exposure limit for astronauts [5]. Alt-hough LADTAG took extensive steps to preserve what chemical reactivity may still have existed in the sam-ples, it is simply unknown if they possessed true in-situ chemical reactivity or if that reactivity has de-cayed. Initial gas loss on collection and other altera-tions, and even intermittent exposure to Earth-normal conditions during subsequent decades of handling, obscure a forensic reconstruction of the initial state. Because a mineral dust’s chemical reactivity influ-ences its biotoxicity [6], researchers have developed methods to “activate” lunar dust and simulants [7][8]. Past studies that modeled impact processes and radia-tion [9] in the lunar environment suggest that in-situ lunar dust is likely to be more chemically reactive than Earth-exposed samples. Because of these results, in-situ measurements are warranted [10]. Other studies have examined the hydroxyl generating capability of iron bearing mineral phases [11][12] and further em-phasize the role iron plays in chemical reactivity of lunar material, as well as decay of chemical reactivity in mineral dusts [12]. Recent observations of the lunar surface reveal the presence of hematite [13], a finding that further supports the hypothesis that in-situ lunar dust is reactive. Since the lunar surface is heterogene-ous, dust biotoxicity is expected to vary from site to site [14] due to particle size, mineralogy, physical characteristics, degree of space weathering, and chemi-cal reactivity (Figure 1). This circumstance dictates dust assessments at a suite of lunar sites enabled by upcoming NASA and commercial lunar payload ser-vices (CLPS) opportunities. Dose, location, and dura-tion of particle exposure will also affect biological responses. In-situ chemical reactivity measurements can inform cross-cutting collaborative research cam-paigns such as astrobiology studies examining regolith interactions with organisms and its ability to preserve chemical and structural biomarkers, as well as space biology investigations that examine regolith-microbe interactions relating to life support systems, plant growth, biomining, and development of regolith bio-composites. Figure 1: Environment conditions on the lunar surface that may alter regolith reactivity. Summary A series of in-situ measurements of lu-nar dust free radical chemistry at future Artemis and CLPS landing sites, combined with LADTAG-like studies of freshly collected lunar dust specimens, will reveal the true chemical reactivity of in-situ lunar dust and generate scientific data that can be compared to the chemical reactivity and biotoxicity of samples from Apollo landing sites. Furthermore, results from in situ measurements and biotoxicity studies of freshly col-lected specimens can also be used to validate, or re-quire revision of, the current astronaut permissible exposure limit [15]. References: [1] McKay D et al (2015), Acta As-tronaut 107:163–176. [2] Rask J et al (2013), LPSC, p 3062. [3] Lam CW et al (2013), Inhal Toxicol 25:661–678. [4] James JT, et. al. (2013) , Inhal Toxicol 25:243–256. [5] Scully RR, et.al. (2013), Inhal Toxi-col 25:785–793. [6] Porter, D. W., et.al., (2002), Tox-icology 175, 63–71. [7] Wallace WT, et.al., (2009), Meteorit Planet Sci 44:961–970. [8] Wallace WT, et.al., (2010), Earth Planet Sci Lett 295:571–577. [9] Loftus D, Rask J, et.al., (2010), Earth Moon Planet 107:95–105. [10] Rask J, et.al., (2009) LEAG p 57. [11] Turci F, et.a., (2015), Astrobiology. 2015;15(5):371-380. [12] Hendrix DA, et.al., (2019), Geohealth. 2019;3(1):28-42. [13] Li, S., et.al., (2020), Science advances, 6(36), p.eaba1940. [14] Rask J. (2018), In: Cudnik B. (eds) Encyclopedia of Lunar Science. Springer, Cham. [15] Rask, J, (2020), LPI, Artemis III Sci. def. paper 2120.

chemical reactivity↗
DOE OSTI2024

Experimental Examination of Additively Manufactured Patterns on Structural Nuclear Materials for Digital Image Correlation Strain Measurements

Abstract Background There are a limited number of commercially available sensors for monitoring the deformation of materials in-situ during harsh environment applications, such as those found in the nuclear and aerospace industries. Such sensing devices, including weldable strain gauges, extensometers, and linear variable differential transformers, can be destructive to material surfaces being investigated and typically require relatively large surface areas to attach (> 10 mm in length). Digital image correlation (DIC) is a viable, non-contact alternative to in-situ strain deformation. However, it often requires implementing artificial patterns using splattering techniques, which are difficult to reproduce. Objective Additive manufacturing capabilities offer consistent patterns using programmable fabrication methods. Methods In this work, a variety of small-scale periodic patterns with different geometries were printed directly on structural nuclear materials (i.e., stainless steel and aluminum tensile specimens) using an aerosol jet printer (AJP). Unlike other additive manufacturing techniques, AJP offers the advantage of materials selection. DIC was used to track and correlate strain to alternative measurement methods during cyclic loading, and tensile tests (up to 1100 µɛ) at room temperature. Results The results confirmed AJP has better control of pattern parameters for small fields of view and facilitate the ability of DIC algorithms to adequately process patterns with periodicity. More specifically, the printed 100 μm spaced dot and 150 μm spaced line patterns provided accurate measurements with a maximum error of less than 2% and 4% on aluminum samples when compared to an extensometer and commercially available strain gauges. Conclusion Our results highlight a new pattern fabrication technique that is form factor friendly for digital image correlation in nuclear applications.

Novich, K. A. (ORCID:0000000204466022)↗
NASA NTRS2018

Electrodynamic Dust Shield (EDS) Preparation for MISSE-11 Launch

The dusty surfaces of the Moon, Mars, and various asteroids present a significant challenge to NASA’s manned and unmanned space exploration efforts. The fine, electrostatically charged dust is difficult to remove and has resulted in vision obscuration, false instrument readings, contamination, elevated temperatures, performance reduction, and equipment failure. To alleviate these problems, NASA KSC’s Electrostatics and Surface Physics Laboratory (ESPL) is developing active dust mitigation systems for solar system exploration and in situ resource utilization (ISRU). Part of KSC’s Swamp Works system, the lab emphasizes fast-paced, hands-on, cost-effective, and collaborative innovation. The Electrodynamic Dust Shield (EDS) is an ESPL technology being developed to prevent dust accumulation on space components. It consists of a dielectric substrate embedded with parallel electrodes which, when applied with high voltage out-of-phase waveforms, produce a traveling electric field wave that scatters dust particles from its surface via dielectrophoretic and electrostatic forces. The EDS is currently fully functional and has been tested for scalability and endurance in reduced gravity/pressure flight. Next, it will be part of the May 2019 Materials International Space Station Experiment-11 (MISSE-11) payload, which will test small shield samples for performance durability with exposure to the harsh space environment. The summer objective was to test EDS functionality before active and passive dust shield samples launch on MISSE-11, in order to screen for good flight/control samples as well as to compare pre-flight and post-flight clearing efficiencies. I imaged glass and Kapton shields of 2-phase and 3-phase electrode configurations with the Keyence VHX-5000 digital microscope to check for damage before and after all testing for a qualitative pre-flight baseline; helped with vacuum testing of high-voltage shield breakdown; assembled shields and wires using Electrobond 004 silver epoxy; and helped with vacuum and cryogenic dust clearance testing of assembled EDS systems. I learned CAD (computer-aided design) and 3D printing skills to create parts for a shaker table/motor assembly, which will allow for repeatable experiments by evening out EDS dust distribution in a consistent manner prior to dust scattering testing. I will also be improving the interfacing with Alpha Space’s prototype Data Communications Unit (DCU), a payload component to control power to the EDS and store data, by mapping the DCU structure upon power-up and writing shell scripts to improve various processes. Finally, I also CADed and 3D-printed plastic supports for three different geometries of the Electrostatic Precipitator (ESP), a project that aims to use high voltage electrodes to charge and filter out dust from the Martian atmosphere drawn for ISRU devices. This work on dust mitigation technologies will help to support future robotic and human space exploration missions, including NASA’s Journey to Mars; the EDS has especially significant applications to spacecraft solar panels, thermal radiators, viewports, and astronaut visors. This opportunity has also allowed me to become more familiar with various lab equipment and hardware testing, develop key modeling skills in SolidWorks, explore past and present components critical to America’s space program, work with inspiring peers and mentors, and ascertain my dream of working permanently for NASA.

space↗
NASA NTRSDate not supplied

Playing with DIRT: Building the Framework for a Comprehensive In-Situ Soil Materials Testing Database

Long-term, sustainable planetary exploration will require the ability to "live off the land," relying on In-Situ Resource Utilization (ISRU) and In-Situ Construction as core capabilities. Reduction of both risk and launch mass for lunar construction will require evaluating and comparing regolith materials for use as feedstocks suitable for in-situ beneficiation and fabrication of building components. These material assessment capabilities will inform lunar infrastructure design decisions, with co-benefits for terrestrial construction using in-situ materials. Current planetary construction technology development relies on lunar mapping and orbital data, Apollo-era sample analyses, current simulant inventories, and tests conducted using analog site soils. Requirements for lunar infrastructure design decisions and construction systems will be determined based on specific environmental conditions, mission architectures, and the materials available within traverse range of lunar feedstock processing depots. Critical for success is the capability to identify, evaluate and make effective use of a wide range of materials as they are found in-situ on the lunar surface. This paper discusses the development of a digital repository for data on soil and regolith properties, beginning with their structural performance in both cementitious and non-cementitious building material formulations. The Database for In-situ Resource Testing (DIRT) compiles a catalog of raw materials, additives, and formulations, with notations pertaining to material sources and preparation techniques entered via a web-based user interface. Design of consistent data schemas for site-sourced materials evaluation will facilitate linkage with relevant terrestrial and planetary materials databases while enabling guided data input via templates for participation by broader groups of collaborators. Results of these analyses are compiled in a centralized repository to generate insights applicable for regolith resources and landing sites yet to be precisely defined. Collection of thorough records of material characteristics, applications and performance will support innovative construction solutions not only for space infrastructure but for sustainable, resilient design in the terrestrial built environment.

Sarah Joey Seitz↗
DOE OSTI2025

Integrated process-structure–property–performance optimization of cold-sprayed zinc coatings on AZ91 magnesium alloy

High-pressure die cast (HPDC) AZ91 magnesium alloy is widely used in automotive components such as transmission housings and brackets for its excellent strength-to-weight ratio. Zinc-based cold spray coatings can be applied selectively to vulnerable areas to enhance corrosion resistance, minimize galvanic coupling with dissimilar metals, and eliminate the need for full-surface oxide coatings, making the process more efficient and targeted. A comprehensive evaluation of 16 combinations of nitrogen carrier gas temperatures and pressures led to the identification of an optimal range of process parameters, yielding Zn coatings with porosity <0.5 % by area, wear rates reduced by a factor of two compared to uncoated AZ91, and adhesion strengths up to 35 MPa. The enhanced mechanical performance of the coating is attributed to the low porosity and the formation of a metallurgical bond at the coating-substrate interface. Corrosion studies using macroscale potentiodynamic polarization (PDP) and electrochemical impedance spectroscopy (EIS) revealed a significant decrease in corrosion rate and a shift to more noble corrosion potentials (ZCP) for coated substrates. Furthermore, the Zn cold-sprayed samples exhibited significantly lower corrosion-induced evolved hydrogen content compared to the base AZ91 substrate and AZ91 coated with industrial coatings, demonstrating that the Zn layer effectively protects the substrate from the corrosive environment. Overall, cold spray Zn coatings significantly improve the mechanical and corrosion performance of AZ91 Mg alloys, addressing key material challenges and enabling their broader use in automotive applications.

Corrosion performance↗
DOE OSTI2024

Characterization of MoS 2 films via simultaneous grazing incidence X-ray diffraction and grazing incidence X-ray fluorescence (GIXRD/GIXRF)

Physical vapor deposited (PVD) molybdenum disulfide (nominal composition MoS 2 ) is employed as a thin film solid lubricant for extreme environments where liquid lubricants are not viable. The tribological properties of MoS 2 are highly dependent on morphological attributes such as film thickness, orientation, crystallinity, film density, and stoichiometry. These structural characteristics are controlled by tuning the PVD process parameters, yet undesirable alterations in the structure often occur due to process variations between deposition runs. Nondestructive film diagnostics can enable improved yield and serve as a means of tuning a deposition process, thus enabling quality control and materials exploration. Grazing incidence X-ray diffraction (GIXRD) for MoS 2 film characterization provides valuable information about film density and grain orientation (texture). However, the determination of film stoichiometry can only be indirectly inferred via GIXRD. The combination of density and microstructure via GIXRD with chemical composition via grazing incidence X-ray fluorescence (GIXRF) enables the isolation and decoupling of film density, composition, and microstructure and their ultimate impact on film layer thickness, thereby improving coating thickness predictions via X-ray fluorescence. We have augmented an existing GIXRD instrument with an additional X-ray detector for the simultaneous measurement of energy-dispersive X-ray fluorescence spectra during the GIXRD analysis. This combined GIXRD/GIXRF analysis has proven synergetic for correlating chemical composition to the structural aspects of MoS 2 films provided by GIXRD. We present the usefulness of the combined diagnostic technique via exemplar MoS 2 film samples and provide a discussion regarding data extraction techniques of grazing angle series measurements.

MoS2↗
DOE OSTI2026

Uncertainty-Aware Machine Learning for Small-Angle X-ray Scattering Analysis in Autonomous Experimentation

Small-angle X-ray scattering (SAXS) is a powerful high-throughput characterization tool for probing nanoscale structure in native sample environments, providing real-time morphological information such as nanoparticle size and shape during synthesis. However, automated SAXS data analysis for extracting meaningful structural parameters is non-trivial and remains a bottleneck in closed-loop experimentation towards autonomous materials discovery, which demands fast, reliable, and uncertainty-aware data analysis. Here, we develop a machine-learning approach for automated SAXS analysis tailored to closed-loop nanoparticle synthesis. A Random Forest (RF) regression model is trained on 100,000 synthetic SAXS curves generated from polydisperse spherical nanoparticles with realistic background contributions. Using normalized one-dimensional SAXS intensity profiles as input, the RF model directly predicts nanoparticle radius, size polydispersity, and background parameters, while the ensemble standard deviation across trees provides built-in uncertainty quantification (UQ). On synthetic data, we show that combining fit-quality metrics (R 2 , MAE) with thresholds on prediction uncertainty reliably identifies accurate parameter estimates without access to ground truth. We then apply the trained model to 365 experimental SAXS profiles of citrate-reduced gold nanoparticles synthesized using an automated droplet-flow microreactor with in situ SAXS at a synchrotron beamline, classifying the results into high- and low-confidence subsets based on UQ metrics. Finally, we integrate RF-based SAXS analysis into a simulated closed-loop optimization campaign using Gaussian process Bayesian optimization to minimize nanoparticle polydispersity, benchmarking against conventional automated Levenberg–Marquardt fitting. The RF-guided campaign exhibits substantially faster convergence and lower relative opportunity cost (∼0.07 vs ∼0.3), demonstrating that uncertainty-aware machine-learning SAXS analysis significantly enhances the efficiency and robustness of autonomous nanomaterials synthesis workflows.

Bayesian optimization↗
DOE OSTI2025

Chemical Imaging of Atmospheric Biomass Burning Particles from North American Wildfires

The effects of biomass burning aerosols (BBA) on radiative forcing and cloud formation depend on chemical composition and the internal structures of individual particles within smoke plumes. To improve our understanding of the chemical and physical properties of BBA emitted at different times of the day and their evolution during atmospheric aging, we conducted a study as a part of the Fire Influence on Regional to Global Environments and Air Quality field campaign. Particle samples were collected onboard a research aircraft from smoke plumes from a wildfire in eastern Oregon during late afternoon and nighttime flights on August 28, 2019. A time-resolved aerosol collector was used to collect samples on substrates for offline spectromicroscopic imaging to investigate the single-particle characteristics of BBA particles. Approximately 20,400 individual particles from 10 selected samples were analyzed using computer-controlled scanning electron microscopy coupled with energy-dispersive X-ray microanalysis, revealing their elemental composition, morphology, and viscosity. Elemental microanalysis indicated that aged potassium is likely found in the form of K 2 SO 4 , KNO 3 , and possible K-organic salts. Further chemical speciation and carbon bonding mapping within individual particles were conducted using synchrotron-based scanning transmission X-ray microscopy (STXM) coupled with near edge X-ray absorption fine structure (NEXAFS) spectroscopy. Real-time, water-soluble light absorption measurements were acquired using a particle-into-liquid sampler instrument coupled to a liquid waveguide capillary cell and total organic analyzer. In the late afternoon samples, 65% of the total particle number population consisted entirely of organic components, compared to 46% in the nighttime particles. These differences were attributed to discrepancies in composition at the time of emission and to the daytime condensation and accumulation of photochemically formed secondary organic material on existing BBA particles, a process that halts at night. Microscopy images indicated that particle viscosity was lower in the nighttime particles (<10 1 Pa·s), likely due to increased relative humidity and a higher contribution from hygroscopic inorganic components. The chemical heterogeneity of individual particles was quantified using STXM-derived mixing state parameters. The nature of carbon bonding within individual particles was inferred from the extent of carbon sp 2 hybridization derived from NEXAFS spectra. Average percentages of sp 2 hybridization range between 40% and 60%, with no noticeable differences between late afternoon and nighttime flights. These findings were compared with the online optical properties of both late afternoon and nighttime smoke plumes, providing valuable insights into the complex relationship between chemical composition and optical properties of BBA particles at different times of the day.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2025

In situ high-temperature Raman spectroscopy for online EAF slag analysis

Real-time monitoring of slag chemistry is critical for optimizing Electric Arc Furnace (EAF) steelmaking operations, where dynamic variations in slag composition directly influence slag foaming, refractory degradation, and thermal efficiency. Conventional techniques such as X-ray fluorescence (XRF), Fourier-transform infrared (FTIR), and scanning electron microscopy coupled with energy-dispersive X-ray spectroscopy (SEM-EDS) are commonly used to analyze slag composition, but their offline nature and equipment constraints limit their applicability for online monitoring in harsh industrial environments. To address this challenge, we present an in situ, high-temperature analytical approach that integrates Raman spectroscopy with a custom designed fiber-optic probe for real-time slag characterization at 1550 °C. The system enables non destructive spectral acquisition from molten slags, providing molecular-level insights into silicate polymerization and iron oxidation states. Eight synthetic slag samples were evaluated, and key Raman features—such as Q n silicate units and FeO₄/FeO₆ coordination environments—were identified and quantitatively correlated with slag basicity and Fe₂O₃ content. The results demonstrate agreement between Raman spectral ratios and bulk slag chemistry, validating the method’s capability to track compositional and structural changes under molten temperature. This work establishes the feasibility of deploying fiber-optic Raman probe for online EAF slag monitoring and highlights their potential to support closed-loop control strategies, thereby enhancing process stability, refractory protection, and steel quality in industrial steelmaking applications.

47 OTHER INSTRUMENTATION↗
DOE OSTI2024

Tailoring Carbide Dispersed Steels: A Path to Increased Strength and Hydrogen Tolerance

The use of transition metal carbides is reported for use as a hydrogen trapping mechanism for ferritic and austenitic steel materials. The program combined computational modeling and simulations to guide experiments towards candidate metal carbide traps, both for interfacial and interior trapping. It was found that interfacial trapping is less effective than interior trapping, with the group IVB transition metal carbides being the most effect internal traps with a loss of carbon. The sub-stoichiometric rocksalt structure accommodate the hydrogen atoms in its octahedral interstices. Using percolation theory, carbon loss of approximately 25% or more was sufficient to ensure an interconnected network of vacancies for such trapping from the surface to the internal sites within the carbide. Using this as a guide, the program developed a means to provide a uniform dispersion of ZrC nanoparticles with either Fe or 304L micron-scale powders which was then consolidated by direct current sintering. Electrolytic hydrogen diffusivity studies confirmed the reduction of hydrogen diffusion in the matrix with increasing ZrC content, which was a linear response over the sample range studied (0.01 to 1.0 wt.%). The consolidated material was micro-tensile tested in either a non-hydrogen or hydrogen charge condition and compared to a control with no carbides. Additions up to 0.05 wt.% ZrC increased the yield strength with no loss in ductility in either the non-hydrogen or hydrogen tested condition. ZrC concentrations above this amount further increased the yield strength at the expense of ductility. While these samples had a lower absolute ductility value prior to failure, the relative change in ductility between the non-hydrogen and hydrogen charge states was less for the carbides than that of the control. Metal-rich ZrC nanoparticles were fabricated through a conformal coating process yielding ZrC0.66 particles that were then incorporated into a metal matrix. Notch fatigue testing in a hydrogen environment was conducted where the number of cycles to failure was found to be less in the control than that of the carbide addition. However, the spread in experimental data and the number of samples tested limits a conclusive outcome based on defects noticed in the gauge section of all the powder processed samples. The collective outcomes of this report provide further insight into the mechanisms by which carbides act as hydrogen traps; a means to process such carbides through powder metallurgy; and their associated mechanical performance in either a non-hydrogen or hydrogen-charged condition.

08 HYDROGEN↗
NASA NTRS1993

Viscoelastic characterization of thin-film polymers exposed to low Earth orbit

The materials made available through the Long Duration Exposure Facility (LDEF) satellite provide a set of specimens that can be well characterized and have a known exposure history with reference to atomic oxygen and ultraviolet radiation exposure. Mechanical characteristics measured from control samples and exposed samples provide a data base for predicting the behavior of polymers in low earth orbit. Samples of 1.0 mil thick low density polyethylene were exposed to the low earth orbit environment for a period of six years. These materials were not directly exposed to ram atomic oxygen and offer a unique opportunity for measuring the effect of atomic oxygen and UV radiation on mechanical properties with little concern to the effect of erosion. The viscoelastic characteristics of these materials were measured and compared to the viscoelastic characteristics of control samples. To aid in differentiating the effects of changes in crystallinity resulting from thermal cycling, from the effects of changes in chemical structure resulting from atomic oxygen/UV attack to the polymer, a second set of control specimens, annealed to increase crystallinity, were measured as well. The resulting characterization of these materials will offer insight into the impact of atomic oxygen/UV on the mechanical properties of polymeric materials. The viscoelastic properties measured for the control, annealed, and exposed specimens were the storage and loss modulus as a function of frequency and temperature. From these datum is calculated the viscoelastic master curve derived using the principle of time/temperature superposition. Using the master curve, the relaxation modulus is calculated using the method of Ninomiya and Ferry. The viscoelastic master curve and the stress relaxation modulus provide a direct measure of the changes in the chemical or morphological structure. In addition, the effect of these changes on long-term and short-term mechanical properties is known directly. It should be noted that the dependence on directionality for the polymer films was considered since these films were manufactured by a blown-film process.

Letton, Alan↗
NASA NTRSDate not supplied

In-Situ Scanning Electron Microscope Experiments for Microscale Mechanical Testing and Validated Modeling of Fiber Reinforced Thermoplastics

A novel, in-situ, scanning electron microscope (SEM) mechanical testing capability for materials at the microscale which provides experimental validation to a machine learning (ML) toolset for full-field validation of physics-based micromechanics models is being developed by researchers at NASA Glenn Research Center. These are enabling technologies for the integration of multiscale digital twins for materials into system level models which will result in the improved performance, material discovery, reduced production cost and time, rapid characterization, and prognostic structural health monitoring (SHM) for materials and structures for extreme environments in support of NASA space exploration missions. In order to bridge the material structure-to-system gap for digital twins, physics-based models must be experimentally validated at multiple length scales. Seminal microscale experiments, conducted at the Air Force Research Laboratory (AFRL), were limited to transverse compression of single-layer, unidirectional thermoset polymer matrix composite (PMC) micropillar specimens [1]. The early phases of the current project followed those initial results and setup to reproduce the compression testing of PMC material on the custom-built piezoelectric actuated micromechanical testing rig built by MicroTesting Solutions LLC. In this work, samples of thermoplastic PMC material were first machined into 3 mm cubes, and then further machining and final milling was done using a Focused Ion Beam (FIB). The initial experiment was done on a pillar roughly 20 µm x 20 µm x 40 µm tall. Additional pillars were milled with final sizes ranging from 20 µm x 20 µm x 40 µm tall to 40 µm x 40 µm x 65 µm tall. A speckle pattern for in-situ full-field measurements using Digital Image Correlation (DIC) was applied with platinum, which was coated on the surface, and then the FIB was used to mill away some of the coating to produce an irregular pattern of Pt on the pillar surface. The samples were loaded into the custom testing rig and placed into the SEM and loaded under compression until failure. Images were collected in the SEM during testing. Post-processing of the images was conducted using DIC to obtain full-field displacement and strain measurements elucidating the role of the matrix as well as fiber-fiber interaction at the microscale within the composite subjected to compression loading well into the non-linear regime of the material. Moreover, the evolution of fiber-matrix debonding and matrix cracking is observed in-situ at the microscale. This data, along with images segmented with a newly developed ML toolset [2], was used to create and validate physics-based micromechanics models. An image of the failed micropillar is shown in Figure 1. The techniques developed in the initial compression experiment was tailored to the validation needs of the models and expanded to include different sized samples as well as possibly tension and fatigue.

Laura Wilson↗