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DOE OSTI2025

Tuning transition metal nanoparticles on a non-traditional support via experimental design

The ability to control metal nanoparticle size and morphology on supported catalysts is crucial for optimizing catalytic performance in targeted applications. Here, this work presents a systematic approach for tuning Ni particle and crystallite size on an unconventional, low-porosity silica fume support through select thermal treatments. The catalyst was synthesized via the deposition of nickelocene onto silica fume, resulting in well-dispersed Ni nanoparticles. A face-centered central composite design was employed to systematically assess the effects of time, temperature, and sintering gas environment on metal particle growth. The results demonstrate that the sintering gas environment is the primary factor governing particle and crystallite evolution, with temperature as the next most significant influence. Nickel nanoparticles sintered at temperatures of 650 °C and above under inert conditions exhibited substantial growth and polycrystalline structures, whereas samples treated in oxidative environments formed NiO, restricting particle mobility. Minimally oxidative (500 ppm O₂) environments facilitated rapid sintering while effectively removing residual ligands from the one-step nickelocene deposition process. Extensive structural characterization via a combination of scanning transmission electron microscopy, X-ray diffraction, hydrogen temperature programmed reduction, and small-angle X-ray scattering revealed that oxidative treatments enhanced metal-support interactions, as evidenced by increased reduction temperatures and narrower particle size distributions. These findings establish quantitative relationships between sintering parameters and Ni nanoparticle characteristics, providing a framework for rational catalyst design through controlled thermal treatments. This methodology is broadly applicable to other catalytic systems and provides a quantitative foundation for catalyst design.

CVD↗

NASA NTRS2009

Pre-Flight Characterization of Samples for the MISSE-7 Spacesuit Fabric Exposure Experiment

A series of six sample spacesuit pressure garment assembly (PGA) fabric samples were prepared for the Materials International Space Station Experiment 7 (MISSE-7) flight experiment to test the effects of damage by lunar dust on the susceptibility of the fabrics to radiation damage. These included pristine Apollo-era fluorinated ethylene-propylene (FEP) fabric, Apollo-era FEP fabric that had been abraded with JSC-1A lunar simulant, and a piece of Alan Bean s Apollo 12 PGA sectioned from near the left knee. Also included was a sample of pristine orthofabric, and orthofabric that had been abraded to two different levels with JSC-1A. The samples were characterized using optical microscopy, field emission scanning electron microscopy, and atomic force microscopy. Two sets of six samples were then loaded in space environment exposure hardware, one of which was stored as control samples. The other set was affixed to the MISSE-7 experiment package, and will be mounted on the International Space Station, and exposed to the wake-side low Earth orbit environment. It will be retrieved after an exposure of approximately 12 months, and returned for post flight analysis.

Gaier, James R.↗

DOE OSTI2025

Optical Fiber H2 Sensor Operating in Harsh Environments of Subsurface H2 Storage Reservoirs

Monitoring hydrogen concentration in the subsurface storage reservoirs is vital to ensure the integrity and safety of the storage facilities. An optical fiber hydrogen sensor consisting of a palladium-based sensing layer and a protective polymer layer was developed and evaluated in simulated subsurface hydrogen storage conditions. The developed optical fiber hydrogen sensor has demonstrated successful sensing performance at ~80 °C, ~1,000 psi, and ~100% RH. In addition, the sensor was exposed to real subsurface microbial samples in the harsh environments to monitor microbially induced changes in hydrogen concentration. The sensor has shown stable H2 sensing responses in the replicated underground hydrogen storage conditions without deterioration or loss of H2 sensitivity in the presence of biological samples.

filter layer↗

NASA NTRS2019

Demisability of GFRP and CFRP Components of Reentering Orbital Debris: Phase I Test Results

Observations of surviving reentry debris on the ground and research performed by Hyperschall Technologie Göttingen (HTG) [1] indicated that significantly more glass fiber-reinforced polymer (GFRP) and carbon fiber-reinforced polymer (CFRP) components survive reentry than current models predict. NASA’s Orbital Debris Program Office conducted a series of tests to evaluate the accuracy of material demise models for reentering orbital debris used in NASA’s Object Reentry Survival Analysis Tool (ORSAT) and Debris Assessment Software (DAS). Testing is planned in a multi-phase series to allow for quick quantification of results as well as refinement of methods resulting from lessons learned during early phases. The Phase 1 tests discussed here validated ORSAT models for homogeneous metals, provided an efficient quantification of composite material demisability properties like mass loss rate and overall time to demise, and identified potential failure modes, which are currently not well understood. Phase 2 tests will be used to further understand mass loss rates and modes of both thermal and mechanical failure in composite materials. The authors exposed 95 samples of aluminum, CFRP, Kevlar fiber-reinforced polymer, GFRP, and sheets of G10 fiberglass to conditions approximating the reentry environment using an inductively coupled plasma (ICP) torch facility. The cylindrical CFRP samples were exposed to the atmospheric pressure plasma, at both the end and the midpoint, to investigate the difference in demisability between parts with exposed edges, like panels, and parts with no edges, such as carbonoverwrapped pressure vessels (COPVs). In a non-oxidative environment, no composite materials demised within the 5-minute test time. In the oxidative, elevated heat flux environment, CFRP samples demised between 210 s and 270 s. For the first 100 s of insertion time, most of the mass loss was due to pyrolysis of resin, creating an approximately bi-linear mass-loss rate curve with time. In a non-oxidative environment, carbon filaments were observed to unravel from some of the CFRP end-burned samples; however, this effect did not seem to affect the overall time to demise for the samples significantly. These results indicate that both GFRP and CFRP components survive reentry with significantly more remaining mass than current models predict.

Greene, Benton R.↗

DOE OSTI2021

Genetic and behavioral adaptation of Candida parapsilosis to the microbiome of hospitalized infants revealed by in situ genomics, transcriptomics, and proteomics

Background Candida parapsilosis is a common cause of invasive candidiasis, especially in newborn infants, and infections have been increasing over the past two decades. C. parapsilosis has been primarily studied in pure culture, leaving gaps in understanding of its function in a microbiome context. Results. Here, we compare five unique C. parapsilosis genomes assembled from premature infant fecal samples, three of which are newly reconstructed, and analyze their genome structure, population diversity, and in situ activity relative to reference strains in pure culture. All five genomes contain hotspots of single nucleotide variants, some of which are shared by strains from multiple hospitals. A subset of environmental and hospital-derived genomes share variants within these hotspots suggesting derivation of that region from a common ancestor. Four of the newly reconstructed C. parapsilosis genomes have 4 to 16 copies of the gene RTA3, which encodes a lipid translocase and is implicated in antifungal resistance, potentially indicating adaptation to hospital antifungal use. Time course metatranscriptomics and metaproteomics on fecal samples from a premature infant with a C. parapsilosis blood infection revealed highly variable in situ expression patterns that are distinct from those of similar strains in pure cultures. For example, biofilm formation genes were relatively less expressed in situ, whereas genes linked to oxygen utilization were more highly expressed, indicative of growth in a relatively aerobic environment. In gut microbiome samples, C. parapsilosis co-existed with Enterococcus faecalis that shifted in relative abundance over time, accompanied by changes in bacterial and fungal gene expression and proteome composition. Conclusions The results reveal potentially medically relevant differences in Candida function in gut vs. laboratory environments, and constrain evolutionary processes that could contribute to hospital strain persistence and transfer into premature infant microbiomes.

59 BASIC BIOLOGICAL SCIENCES↗

NASA NTRS2014

Variations in Cathodoluminescent Intensity of Spacecraft Materials Exposed to Energetic Electron Bombardment

Many contemporary spacecraft materials exhibit cathodoluminescence when exposed to electron flux from the space plasma environment. A quantitative, physics-based model has been developed to predict the intensity of the glow as a function of incident electron current density and energy, temperature, and intrinsic material properties. We present a comparative study of the absolute spectral radiance for several types of dielectric and composite materials based on this model which spans three orders of magnitude. Variations in intensity are contrasted for different electron environments, different sizes of samples and sample sets, different testing and analysis methods, and data acquired at different test facilities. Together, these results allow us to estimate the accuracy and precision to which laboratory studies may be able to determine the response of spacecraft materials in the actual space environment. It also provides guidance as to the distribution of emissions that may be expected for sets of similar flight hardware under similar environmental conditions.

plasma environment↗

NASA NTRS2014

Variations in Cathodoluminescent Intensity of Spacecraft Materials Exposed to Energetic Electron Bombardment

orders of magnitude↗

NASA NTRS1978

Self-sterilizing canister

Canister, originally conceived for remote sterilization of spacecraft packages, could be used terrestrially to handle samples in biologically hazardous environments. Multiwalled canister includes inner layer of pyrotechnic powder. For sterilization, electrically activated squib ignites powder, raising temperature of outer surface of canister to 230 degrees centigrade for several minutes. Thermal-buffer inner layer prevents inside temperature for exceeding 100 degrees centigrade to protect contents from damage. Samples in field hospitals and other emergency situations could also be handled by equipment.

Yang, L. C.↗

NASA NTRS1992

Microgravity ignition experiment

The purpose of this project is to develop a flight-ready apparatus of the microgravity ignition experiment for the GASCAN 2 program. The microgravity ignition experiment is designed to study how a microgravity environment affects the time to ignition of a sample of alpha-cellulose paper. A microgravity environment will result in a decrease in the heat transferred from the sample due to a lack of convection currents, which would decrease time to ignition. A lack of convection current would also cause the oxygen supply at the sample not to be renewed, which could delay or even prevent ignition. When this experiment is conducted aboard GASCAN 2, the dominant result of the lack of ignition will be determined. The experiment consists of four canisters containing four thermocouples and a sensor to detect ignition of the paper sample. This year the interior of the canister was redesigned and a mathematical model of the heat transfer around the sample was developed. This heat transfer model predicts an ignition time of approximately 5.5 seconds if the decrease of heat loss from the sample is the dominant factor of the lack of convection currents.

Motevalli, Vahid↗

NASA NTRS1993

Contamination measurements on experiment M0003

The contamination monitors on the M0003 experiment consisted of passive sample collectors to measure molecular and particulate deposition. The collectors were placed in the leading and trailing edge trays of M0003. The objective was to quantify the contaminants and determine how contamination affected the other materials in the trays. Duplicate collectors were placed inside the vacuum canisters that provided protection from the launch, ascent, deployment, and recovery environments. Analyses of the samples show small quantities of molecular deposition on both the leading and trailing edge trays. Silicone deposits are negligible. The aluminized fused silica, second surface mirrors showed small changes in solar absorptances. This is consistent with the small quantities of molecular deposits deduced from the FTIR measurements. The results of particle deposition, light scatter, and a micrometeoroid (or debris) impact are presented.

Borson, Eugene N.↗

NASA NTRS1978

Optical effects module

The possible degradation of optical samples exposed to the effluent gases and particulate matter emanating from the payload of the space transportation system during orbital operations may be determined by measuring two optical parameters for five samples exposed to this environment, namely transmittance and diffuse reflectance. Any changes detected in these parameters as a function of time during the mission are then attributable to surface contamination or to increased material absorption. These basic functions are attained in the optical effects module by virtue of the following subsystems which are described: module enclosure; light source with collimator and modulator; sample wheel with holders and rotary drive; photomultipliers for radiation detection; processing and sequencing electronic circuitry; and power conditioning interfaces. The functions of these subsystems are reviewed and specified.

Source record↗

DOE OSTI2026

Direct and rapid uranium isotopic analysis of environmental sample swipes via microextraction – LS-APGD/Orbitrap mass spectrometry

Accurate and precise isotopic analysis of actinides collected on environmental sample swipes from within nuclear facilities is an important safeguarding measure for detecting undeclared materials and activities. Traditional isotope ratio (IR) analysis of actinides using a bulk digestion approach can be laborious and time-consuming. Recently, direct analysis of environmental swipe samples using a microextraction approach has been explored as an alternative to conventional bulk digestion methods. The present study further evaluates this approach for accurate and precise isotopic analysis of uranium (U) in cotton swipe samples using the liquid sampling-atmospheric pressure glow discharge (LS-APGD)/Orbitrap-FTMS Booster detection system. The instrumental parameters were optimized, and quantitative capabilities were demonstrated through excellent linearity (R2 = 0.99) across a deposited mass range of 1 to 500 ng, with a limit of detection of 90 pg (in a 2 × 4 mm region) for total U; well below typical U concentrations (ng–mg range) in environmental sample swipes. The 235U/238U ratio showed excellent accuracy (−0.3% relative difference from the certificate value), with ∼20× improvement over previous microextraction-Orbitrap methods. Precision (∼1% relative standard deviation) was also greatly enhanced by ∼5×. This study also demonstrates that figures of merit achieved with neat U solution were not highly degraded when various external interfering elements/matrices were introduced. Finally, the developed method was successfully applied to analyze practical swipe samples representative of laboratory and outdoor environments. The presented figures of merit and applicability to practical samples further validate the capability of the platform for rapid analysis (<7 minutes) of environmental swipe samples.

Shrestha, Suraj [Clemson University, SC]↗

NASA NTRS2010

Thermal Control Materials on MISSE-6 with Comparison to Earlier Flight Data

This slide presentation reviews the results of exposing thermal control materials as studied during Materials International Space Station Experiment-6 (MISSE-6). It discusses the location of the materials, and the type of environmental exposure. It then reviews the effect on the various types of coatings, showing the results with graphs and photos of the samples after the experimental exposure to the low earth orbital environment for comparison with the control sample and with earlier flights.

Finckenor, Miria M.↗

DOE OSTI2021

Exploring the Ion Solvation Environments in Solid-State Polymer Electrolytes through Free-Energy Sampling

The success of poly(ethylene oxide) (PEO) in solid-state polymer electrolytes for lithium-ion batteries is well established. Recently, in order to understand this success and to explore possible alternatives, we studied polyacetal electrolytes to deepen the understanding of the effect of the local chemical structure on ion transport. Advanced molecular dynamics techniques using newly developed, tailored interaction potentials have helped elucidate the various coordination environments of ions in these systems. In particular, the competition between cation-Anion pairing and coordination by the polymer has been explored using free-energy sampling (metadynamics). At equivalent reduced temperatures, with respect to the polymer-specific glass-Transition temperature, two-dimensional free-energy plots reveal the existence of multiple coordination environments for the lithium (Li) ions in these systems and their relative stabilities. Furthermore, we observe that the Li-ion movement in PEO follows a serial, stepwise pathway when moving from one coordination state to another, whereas this happens in a more continuous and concerted fashion in a polyacetal such as poly(1,3-dioxalane) [P(EO-MO)]. The implication is that interconversion between coordination states of the Li ions may be easier in P(EO-MO). However, the overarching observation from our free-energy analysis is that Li-ion coordination is dominated by the polymer (in either case) and contact-ion pairs are rare. We rationalize the observed higher increase in glass-Transition temperature (Tg) with salt loading in polyacetals as due to intermolecular Li-ion coordination involving multiple polymer chains, rather than just one chain for PEO-based electrolytes. This interchain coupling in the polyacetals, resulting in the higher Tg, works against any gains due to variations in Li-ion coordination that might enhance transport processes over PEO. Further research is required to overcome the interdependence between local coordination and macroscopic properties to compete with PEO electrolytes at the same absolute working temperature.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2024

The ancestral environment of teosinte populations shapes their root microbiome

Summary Background The composition of the root microbiome affects the host’s growth, with variation in the host genome associated with microbiome variation. However, it is not known whether this intra-specific variation of root microbiomes is a consequence of plants performing targeted manipulations of them to adapt to their local environment or varying passively with other traits. To explore the relationship between the genome, environment and microbiome, we sampled seeds from teosinte populations across its native range in Mexico. We then grew teosinte accessions alongside two modern maize lines in a common garden experiment. Metabarcoding was performed using universal bacterial and fungal primers to profile their root microbiomes. Results The root microbiome varied between the two modern maize lines and the teosinte accessions. We further found that variation of the teosinte genome, the ancestral environment (temperature/elevation) and root microbiome were all correlated. Multiple microbial groups significantly varied in relative abundance with temperature/elevation, with an increased abundance of bacteria associated with cold tolerance found in teosinte accessions taken from high elevations. Conclusions Our results suggest that variation in the root microbiome is pre-conditioned by the genome for the local environment (i.e. non-random). Ultimately, these claims would be strengthened by confirming that these differences in the root microbiome impact host phenotype, for example, by confirming that the root microbiomes of high-elevation teosinte populations enhance cold tolerance.

Genetics & Heredity↗

NASA NTRS2017

Ballooning for Biologists: Mission Essentials for Flying Experiments on Large NASA Balloons

Despite centuries of scientific balloon flights, only a handful of experiments have produced biologically-relevant results. Yet unlike orbital spaceflight, it is much faster and cheaper to conduct biology research with balloons, sending specimens to the near space environment of Earths stratosphere. Samples can be loaded the morning of a launch and sometimes returned to the laboratory within one day after flying. The National Aeronautics and Space Administration (NASA) flies large, unmanned scientific balloons from all over the globe, with missions ranging from hours to weeks in duration. A payload in the middle portion of the stratosphere (approx. 35 km above sea level) will be exposed to an environment similar to the surface of Mars: temperatures generally around -36 C, atmospheric pressure at a thin 1 kPa, relative humidity levels <1%, and a harsh illumination of ultraviolet (UV) and cosmic radiation levels (about 100 W/sq m and 0.1 mGy/d, respectively) that can be obtained nowhere else on the surface of the Earth, including environmental chambers and particle accelerator facilities attempting to simulate space radiation effects. Considering the operational advantages of ballooning and the fidelity of space-like stressors in the stratosphere, researchers in aerobiology, astrobiology, and space biology can benefit from balloon flight experiments as an intermediary step on the extraterrestrial continuum (ground, low Earth orbit, and deep space studies). Our presentation targets biologists with no background or experience in scientific ballooning. We will provide an overview of large balloon operations, biology topics that can be uniquely addressed in the stratosphere, and a roadmap for developing payloads to fly with NASA.

Smith, David J.↗

NASA NTRS1995

Effect of the space environment on materials flown on the EURECA/TICCE-HVI experiment

The primary benefit of accurately quantifying and characterizing the space environmental effects on materials is longer instrument and spacecraft life. Knowledge of the limits of materials allows the designer to optimize the spacecraft design so that the required life is achieved. Materials such as radiator coatings that have excellent durability result in the design of smaller radiators than a radiator coated with a lower durability coating. This may reduce the weight of the spacecraft due to a more optimum design. Another benefit of characterizing materials is the quantification of outgassing properties. Spacecraft which have ultraviolet or visible sensor payloads are susceptible to contamination by outgassed volatile materials. Materials with known outgassing characteristics can be restricted in these spacecraft. Finally, good data on material characteristics improves the ability of analytical models to predict material performance. A flight experiment was conducted on the European Space Agency's European Retrievable Carrier (EuReCa) as part of the Timeband Capture Cell Experiment (TICCE). Our main objective was to gather additional data on the dust and debris environments, with the focus on understanding growth as a function of size (mass) for hypervelocity particles 1E-06 cm and larger. In addition to enumerating particle impacts, hypervelocity particles were to be captured and returned intact. Measurements were performed post-flight to determine the flux density, diameters, and subsequent effects on various optical, thermal control and structural materials. In addition to these principal measurements, the experiment also provided a structure and sample holders for the exposure of passive material samples to the space environment, e.g., the effects of thermal cycling, atomic oxygen, etc. Preliminary results are presented, including the techniques used for intact capture of particles.

Maag, Carl R.↗

NASA NTRS2009

Visible and Near-IR Reflectance Spectra for Smectite, Sulfate And Perchlorate under Dry Conditions for Interpretation of Martian Surface Mineralogy

Visible and near-IR (VNIR) spectral data for the martian surface obtained from orbit by the MRO-CRISM and OMEGA instruments are interpreted as having spectral signatures of H2O/OH-bearing phases, including smectites and other phyllosilicates, sulfates, and high-SiO2 phases [e.g., 1-4]. Interpretations of martian spectral signatures are based on and constrained by spectra that are obtained in the laboratory on samples with known mineralogical compositions and other physicochemical characteristics under, as appropriate, Mars-like environmental conditions (e.g., temperature, pressure, and humidity). With respect to environmental conditions, differences in the absolute concentration of atmospheric H2O can effect the hydration state and therefore the spectra signatures of smectite phyllosilicates (solvation H2O) and certain sulfates (hydration H2O) [e.g., 5-7]. We report VNIR spectral data acquired under humid (laboratory air) and dry (dry N2 gas) environments for two natural smectites (nontronite API-33A and saponite SapCa-1) to characterize the effect of solvation H2O on spectral properties. We also report spectral data for the thermal dehydration products of (1) melanterite (FeSO4.7H2O) in both air and dry N2 gas and (2) Mg-perchlorate (Mg(ClO4)2.6H2O) in dry N2 environments. Spectral measurements for samples dehydrated in dry N2 were made without exposing them to humid laboratory air.

Morris, R.V.↗