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Search indexed NASA NTRS and DOE OSTI research on propulsion, heat transfer, battery materials and energy systems. Follow report and document links to the original sources.

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At least 253 records · Page 14
All sourcesNASA NTRSDOE OSTI
DOE OSTI2024

Light-enhanced oxygen degradation of MAPbBr 3 single crystal

Organometal halide perovskites are promising materials for optoelectronic applications, whose commercial realization depends critically on their stability under multiple environmental factors. In this study, a methylammonium lead bromide (MAPbBr 3 ) single crystal was cleaved and exposed to simultaneous oxygen and light illumination under ultrahigh vacuum (UHV). The exposure process was monitored using X-ray photoelectron spectroscopy (XPS) with precise control of the exposure time and oxygen pressure. It was found that the combination of oxygen and light accelerated the degradation of MAPbBr 3 , which could not be viewed as a simple addition of that by oxygen-only and light-only exposures. The XPS spectra showed significant loss of carbon, bromine, and nitrogen at an oxygen exposure of 10 10 Langmuir with light illumination, approximately 17 times of the additive effects of oxygen-only and light-only exposures. It was also found that the photoluminescence (PL) emission was much weakened by oxygen and light co-exposure, while previous reports had shown that PL was substantially enhanced by oxygen-only exposure. Measurements using a scanning electron microscope (SEM) and focused ion beam (FIB) demonstrated that the crystal surface was much roughened by the co-exposure. Furthermore, Density functional theory (DFT) calculations revealed the formation of superoxide and oxygen induced gap state, suggesting the creation of oxygen radicals by light illumination as a possible microscopic driving force for enhanced degradation.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2020

Tracking nanoparticle growth in pulsed carbon arc discharge

The dynamics of nanoparticle growth in pulsed anodic arc discharge has been studied in time-resolved mode. To this end, a fast moving probe was employed to extract the material generated in a pulsed arc plasma held between two graphite electrodes. The probe motion was synchronized with the pulse phase and the exposure time to the plasma was set to 10 ms. The graphite anode was eroded in a helium atmosphere (300 Torr) by an arc plasma pulsed at 1 Hz with a 10% duty cycle and showing 250 A of peak current. The structure and morphology of the probe depositions were characterized by Raman spectroscopy, scanning electron microscopy, and focused ion beam. A maximal deposition rate of 260 μm/s was measured 5 mm away from the arc core during the active 0.1 s of the pulse. Such a rate yields a growth flux of 1.3 × 10 21 cm –2 s –1 , rich in carbon nanostructures (graphene platelets, nanotubes) with a characteristic aggregate size within 1–10 μm. The deposition during the inactive 0.9 s of the pulse was several orders of magnitude slower and consisted of amorphous carbon traces. Furthermore, the nanoparticle distribution along the collecting probe is correlated with the pulse phase, thereby providing information on particle transport. Pulsed nanosynthesis can be modeled as a periodical growth process, where the volume and propagation velocity of the growth region can be adjusted through modulation of the pulse signal waveform. The proposed model constitutes a suitable framework to investigate the pulsed arc synthesis of nanomaterials with tailored physical and chemical properties.

42 ENGINEERING↗
DOE OSTI2024

Comparison of Mg-based liquid metal ion sources for scalable focused-ion-implantation doping of GaN

We compare the suitability of various magnesium-based liquid metal alloy ion sources (LMAISs) for scalable focused-ion-beam (FIB) implantation doping of GaN. We consider GaMg, MgSO 4 $\bullet$7H 2 O, MgZn, AlMg, and AuMgSi alloys. Although issues of oxidation (GaMg), decomposition (MgSO 4 $\bullet$7H 2 O), and excessive vapor pressure (MgZn and AlMg) were encountered, the AuMgSi alloy LMAIS operating in a Wien-filtered FIB column emits all Mg isotopes in singly and doubly charged ionization states. We discuss the operating conditions to achieve <20 nm spot size Mg FIB implantation and present Mg depth profile data from time-of-flight secondary ion mass spectrometry. We also provide insight into implantation damage and recovery based on cathodoluminescence spectroscopy before and after rapid thermal processing. Prospects for incorporating the Mg LMAIS into high-power electronic device fabrication are also discussed.

36 MATERIALS SCIENCE↗
DOE OSTI2025

Monofluorinated acetal electrolyte for high-performance lithium metal batteries

High degree of fluorination for ether electrolytes has resulted in improved cycling stability of lithium metal batteries due to stable solid electrolyte interphase (SEI) formation and good oxidative stability. However, the sluggish ion transport and environmental concerns of high fluorination degree drive the need to develop less fluorinated structures. Here, we depart from the traditional ether backbone and introduce bis(2-fluoroethoxy)methane (F2DEM), featuring monofluorination of the acetal backbone. High coulombic efficiency and stable long-term cycling in Li||Cu half cells can be achieved with F2DEM even under fast Li metal plating conditions. The performance of F2DEM is further compared with diethoxymethane (DEM) and 2-[2-(2,2-difluoroethoxy)ethoxy]-1,1,1-trifluoroethane (F5DEE). A significantly lower overpotential is observed with F2DEM, which improves energy efficiency and enables its application in high-rate conditions. Comparative studies of F2DEM with DEM and F5DEE in anode-free lithium iron phosphate (LiFePO4) LFP pouch cells and high-loading LFP coin cells further show improved capacity retention of F2DEM electrolyte, demonstrating its practical applicability. More importantly, we also extensively investigate the underlying mechanism for the superior performance of F2DEM through various techniques, including X-ray photoelectron spectroscopy, scanning electron microscopy, cryogenic electron microscopy, focused ion beam, electrochemical impedance spectroscopy, and titration gas chromatography. Overall, F2DEM facilitates improved Li deposition morphology with reduced amount of dead Li. This enables F2DEM to show superior performance, especially under higher charging and slower discharging rate conditions.

25 ENERGY STORAGE↗
DOE OSTI2025

Water content modulation enables selective ion transport in 2D MXene membranes

Separation membranes are critical for a range of processes, including but not limited to water desalination, chemical and fuel production, and recycling and recovery applications. Fundamentally, there are intrinsic trade-offs between permeability and selectivity. Local water organization and content can impact membrane structure (short- and long-range) in laminar transition metal carbide (MXene) membranes and impact selective ion permeation. Intercalation of chaotropic cesium (Cs + ) ions within the layers reduces the water content in the membrane and at the surface which cannot be found in the intercalation of other ions. Additionally, 3D imaging using focused ion beam scanning electron microscopy showed fewer defects in the Cs-MXene membrane, due to reduced local water content, leading to more efficient ion sieving. X-ray diffraction and density functional theory calculations on the nanochannel structure demonstrated that the chaotropic ion results in the smallest nanochannel size and induces a stronger resistance to water-induced nanochannel swelling. With a narrower nanochannel, the Cs-MXene membrane limits ion transport pathways, resulting in more selective transport of lithium over other metal cations, as evidenced in both experiment and molecular dynamics simulations. In conclusion, our findings highlight the potential for controlling the structural organization of 2D MXene membranes to enable on-demand transport of ions for diverse applications.

36 MATERIALS SCIENCE↗
DOE OSTI2022

Determination of the characteristic magnetic pre-sheath length at divertor surfaces using micro-engineered targets on DiMES at DIII-D

The magnetic pre-sheath (MPS) width, L MPS , is a critical parameter to define the sheath potential, which controls the ion trajectory of low-Z species (D, T, He, and C), as well as the prompt re-deposition of high-Z species. In this work, to determine L MPS , we fabricated micro-trenches (30×30×4 µm) via focused ion beam (FIB) milling on a silicon surface and exposed them to L-mode deuterium plasmas in DIII-D via the Divertor Material Evaluation System (DiMES) removable sample exposure probe. The areal distribution of impurity depositions, mainly consisting of carbon, was measured by energy-dispersive X-ray spectroscopy (EDS) to reveal the deuterium ion shadowing effect on the trench floors. The carbon deposition profiles showed that the erosion was maximized for the azimuthal direction of φ = -40° (referenced to the toroidal magnetic field direction) as well as the polar angle of θ = 80°. A Monte Carlo equation-of-motion model, based on a collisionless MPS, was used to calculate the azimuthal and polar deuterium ion angle distributions (IADs) for a range of L MPS = k × ρ i , where ρ i is the ion gyro radius and k = 0.5-4. Then, gross erosion profiles were calculated by a Monte Carlo micro-patterning and roughness (MPR) code for ion sputtering using as input the calculated azimuthal and polar IADs for each value of k . Good agreement with the experimental C deposition profiles was obtained for the case k = 2.5-3.5. This result is consistent with a previous kinetic modeling prediction of k ~ 3, as well as previous analytical investigations that predicted the L MPS to be several ion gyro radii. A validation of theoretical sheath models supports its applicability to ITER and pilot plant divertors to successfully predict plasma-materials interactions.

Erosion↗
DOE OSTI2024

Atom Probe Tomography Investigation of Clustering in Model P 2 O 5 -Doped Borosilicate Glasses for Nuclear Waste Vitrification

Atom probe tomography (APT) has been utilized to investigate the microstructure of two model borosilicate glasses designed to understand the solubility limits of phosphorous pentoxide (P 2 O 5 ). This component is found in certain high-level radioactive defence wastes destined for vitrification, where phase separation can potentially lead to a number of issues relating to the processing of the glass and its long-term chemical and structural stability. The development of suitable focused ion beam (FIB)-preparation routes and APT analysis conditions were initially determined for the model glasses, before examining their detailed microstructures. In a 3.0 mol% P 2 O 5 -doped glass, both visual inspection and sensitive statistical analysis of the APT data show homogeneous microstructures, while raising the content to 4.0 mol% initiates the formation of phosphorus-enriched nanoscale precipitates. This study confirms the expected inhomogeneities and phase separation of these glasses and offers routes to characterizing these at near-atomic scale resolution using APT.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗
DOE OSTI2025

Designing Antifouling and Antimicrobial Interfaces: Structural Characterization using CryoEM, Automated Microscopy, and AI Image Segmentation

The design of functionalized surfaces for interactions with biological systems is critical across sectors such as healthcare, energy, and agriculture. Tailoring materials for specific applications, such as antifouling and antimicrobial surfaces, demands a comprehensive understanding of topology and chemistry across multiple length and time scales on both biological and materials systems. This work presents the development and characterization of nanostructured surfaces with controlled topographies and chemistries that enhance bacterial membrane disruption, reduce biofilm formation, and improve antimicrobial and antifouling capabilities. Two specific use cases will be presented - the use of cellulose nanocrystals (CNCs) for bacterial growth inhibition and the development of antifouling surfaces to prevent protein and bacterial adsorption [1-4]. By leveraging large language models (LLMs) for image segmentation and training [5], we enable automated analysis of terabyte-scale cryogenic electron microscopy (cryoEM) datasets. This analysis provides statistical insights into the biotic/abiotic interface and facilitates automated electron microscopy experiments to mitigate time and dose. The integration of cryogenic electron tomography (cryoET) and cryogenic focused ion beam (cryoFIB) milling enables high-resolution, near-native-state imaging and 3D reconstructions of bio/material interfaces [6]. Orthogonal characterization techniques and computational modeling further enhances our understanding, offering a robust platform for the design and optimization of next-generation functional surfaces [7].

Williams, Alexis [ORNL] (ORCID:0000000252835822)↗
DOE OSTI2024

Conjugate Multimode Heat Transfer Analysis of Cryogenic EXLO Manipulation

Abstract In this study, a conjugate radiation/conduction multimode heat transfer analysis of cryogenic focused ion beam (FIB) milling steps necessary for producing ex situ lift out specimens under cryogenic conditions (cryo-EXLO) is performed. Using finite volume for transient heat conduction and enclosure theory for radiation heat transfer, the analysis shows that as long as the specimen is attached or touching the FIB side wall trenches, the specimen will remain vitreous indefinitely, while actively cooled at liquid nitrogen (LN2) temperatures. To simulate the time needed to perform a transfer step to move the bulk sample containing the FIB-thinned specimen from the cryo-FIB to the cryo-EXLO cryostat, the LN2 temperature active cooling is turned off after steady-state conditions are reached and the specimen is monitored over time until the critical devitrification temperature is reached. Under these conditions, the sample will remain vitreous for >3 min, which is more than enough time needed to perform the cryo-transfer step from the FIB to the cryostat, which takes only ∼10 s. Cryo-transmission electron microscopy images of a manipulated cryo-EXLO yeast specimen prepared with cryo-FIB corroborates the heat transfer analysis.

Materials Science↗
DOE OSTI2023

Electric Field Analysis in a Cold-Ion Source Using Stark Spectroscopy of Rydberg Atoms

Here, we analyze electric fields in ion sources generated by quasicontinuous photoionization of cold Rb atoms trapped in the focal spot of a near-concentric, in-vacuum cavity for 1064-nm laser light. Ion streams are extracted with an external electric field, F. Stark effects of Rb 57F and of nearby high-angular-momentum Rydberg levels, which exhibit large, linear Stark shifts, are employed to study the net electric-field probability distribution within the ion-source region over an extraction-field range of 0 < F < 0.35 V/cm. For F = 0, we also investigate ion-field-induced Stark spectra of the 60P 1/2 state, which exhibits a (lesser) quadratic electric-field response that affords a simplified electric-field analysis. Experimental Rydberg spectra are compared with theoretical Stark spectra, which are weighted with net electric-field distributions obtained from classical ion-trajectory simulations that include Coulomb interactions. Experiments and models are in good agreement. At small F and high ion-source rates, the field approximately follows a Holtsmark distribution, and the ion streams are degraded by the Coulomb microfields. With increasing F and at lower ion-source rates, the fields become narrowly distributed around F, resulting in directional ion streams that are less degraded by microfields. Our results are of interest for monitoring cold-ion sources for focused-ion-beam applications, where Coulomb interactions are of concern, and for studies of electric fields in cold plasmas.

74 ATOMIC AND MOLECULAR PHYSICS↗
DOE OSTI2025

Control of wetting and uniformity via ZrSi x formation in ceramic-to-metal joints fabricated using Ag-Zr brazes

The deposition of a 2.0 µm SiO 2 film on the alumina surface in Kovar TM /94% alumina joints enables the formation of a silicide reaction layer on the alumina during brazing with 97Ag2Zr1Cu. Additionally, the average and standard deviation of joint thickness decrease from 50 to 15 and 29 to 4 µm, respectively compared to joints without added SiO 2 . Finally, the average failure stress of these braze joints was 45 MPa, while that of similar joints without added SiO 2 was 90 MPa. Sessile drop experiments of 98Ag2Zr on SiO 2 and 99.6% Al 2 O 3 substrates show that the braze wets and spreads to 3x its original area on SiO 2 with a wetting angle near 0°, but remains the same area on 99.6% Al 2 O 3 with a wetting angle of 106.6°. Focused-ion-beam scanning electron microscopy analysis of a cross-section of the 98Ag2Zr sessile drop on the SiO 2 substrate has shown that Zr reacts with SiO 2 to form Zr oxide and silicide layers. Scanning transmission electron microscopy diffraction and energy dispersive X-ray spectroscopy analysis indicate this silicide layer contains tetragonal Zr 5 Si 4 . In conclusion, analysis shows the silicide layer enhances wetting and joint uniformity while unreacted SiO 2 embrittles the joint and degrades strength.

alumina↗
DOE OSTI2023

High-temperature oxidation behavior of the SiC layer of TRISO particles in low-pressure oxygen

Surrogate tristructural-isotropic (TRISO)-coated fuel particles were oxidized in 0.2 kPa O 2 at 1200–1600°C to examine the behavior of the SiC layer and understand the mechanisms. The thickness and microstructure of the resultant SiO 2 layers were analyzed using scanning electron microscopy, focused ion beam, and transmission electron microscopy. The majority of the surface comprised smooth, amorphous SiO 2 with a constant thickness indicative of passive oxidation. The apparent activation energy for oxide growth was 188 ± 8 kJ/mol and consistent across all temperatures in 0.2 kPa O 2 . The relationship between activation energy and oxidation mechanism is discussed. Raised nodules of porous, crystalline SiO 2 were dispersed across the surface, suggesting that active oxidation and redeposition occurred in those locations. These nodules were correlated with clusters of nanocrystalline SiC grains, which may facilitate active oxidation. So these findings suggest that microstructural inhomogeneities such as irregular grain size influence the oxidation response of the SiC layer of TRISO particles and may influence their accident tolerance.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
DOE OSTI2022

Submicrometer spectromicroscopy of UO 2 aged under high humidity conditions

We report the oxidation of uranium dioxide is a complicated process, depending on factors including humidity, temperature, and microstructure. To further determine the characteristics of this process, UO 2 particles were allowed to age and agglomerate under 98% relative humidity at room temperature for 378 days. A focused ion beam (FIB) section of this agglomeration was then measured at the O K-edge, U N 5 -edge, and C K-edge using the scanning transmission x-ray microscope (STXM) at the Advanced Light Source. O K-edge and U N 5 -edge x-ray absorption measurements allowed for the elemental and chemical species mapping of the agglomerates and indicated the formation of schoepite at the submicrometer scale in specific locations. Non-negative matrix factorization was employed to elucidate the main components at the O K-edge, which were uranyl (schoepite) formed primarily at the interface of the sample with controlled atmosphere, a UO 2 -like bulk component present in the majority of the sample, and an oxygen species present at the surface of the FIB section, which is likely adsorbed water. STXM spectromicroscopy measurements at the U N 5 -edge measurements also confirmed the location of oxidized uranium. This analysis is a valuable insight into the formation of schoepite on UO 2 and shows the sensitivity to and utility of STXM spectromicroscopy for uranium speciation.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2022

Design principles for heterointerfacial alloying kinetics at metallic anodes in rechargeable batteries

How surface chemistry influences reactions occurring thereupon has been a long-standing question of broad scientific and technological interest. Here, we consider the relation between the surface chemistry at interfaces and the reversibility of electrochemical transformations at rechargeable battery electrodes. Using Zn as a model system, we report that a moderate strength of chemical interaction between the deposit and the substrate—neither too weak nor too strong—enables highest reversibility and stability of the plating/stripping redox processes. Focused ion beam and electron microscopy were used to directly probe the morphology, chemistry, and crystallography of heterointerfaces of distinct natures. Analogous to the empirical Sabatier principle for chemical heterogeneous catalysis, our findings arise from competing interfacial processes. Using full batteries with stringent negative electrode–to–positive electrode capacity (N:P) ratios, we show that such knowledge provides a powerful tool for designing key materials in highly reversible battery systems based on Earth-abundant, low-cost metals such as Zn and Na.

25 ENERGY STORAGE↗
DOE OSTI2026

Human NLRP3 inflammasome activation leads to formation of condensate at the microtubule organizing center

The NLRP3 inflammasome is a multiprotein molecular machine that drives inflammatory responses in innate immunity. Although its dysregulation is implicated in numerous human diseases, its structural organization in cells remains poorly understood. Here, we used precise fluorescence-guided cryo–focused ion beam (cryo-FIB) milling and cryo–electron tomography (cryo-ET) to visualize NLRP3 inflammasomes in situ within human macrophages at various stages of activation. After priming and activation, we observed expansion and dispersion of Golgi cisternae, along with the emergence of 50-nanometer NLRP3-associated vesicles, which likely transport NLRP3 to the MTOC. Dense NLRP3-containing condensates then formed in and around the MTOC. In later stages, the condensates solidified, coincident with widespread mitochondrial damage, autophagy, and pyroptotic cell death.

Wang, Jue [Division of Chemistry and Chemical Engi↗
DOE OSTI2025

Foundation Models for Zero-Shot Segmentation of Scientific Images without AI-Ready Data

Zero-shot and prompt-based models have excelled at visual reasoning tasks by leveraging large-scale natural image corpora, but they often fail on sparse and domain-specific scientific image data. We introduce Zenesis, a no-code interactive computer vision platform designed to reduce data readiness bottlenecks in scientific imaging workflows. Zenesis integrates lightweight multimodal adaptation for zero-shot inference on raw scientific data, human-in-the-loop refinement, and heuristic-based temporal enhancement. We validate our approach on Focused Ion Beam Scanning Electron Microscopy (FIB-SEM) datasets of catalyst-loaded membranes. Zenesis outperforms baselines, achieving an average accuracy of 0.947, Intersection over Union (IoU) of 0.858, and Dice score of 0.923 on amorphous catalyst samples; and 0.987 accuracy, 0.857 IoU, and 0.923 Dice on crystalline samples. These results represent a significant performance gain over conventional methods such as Otsu thresholding and standalone models like the Segment Anything Model (SAM). Zenesis enables effective image segmentation in domains where annotated datasets are limited, offering a scalable solution for scientific discovery.

Mukherjee, Shubhabrata↗
DOE OSTI2022

Methods—Kintsugi Imaging of Battery Electrodes: Distinguishing Pores from the Carbon Binder Domain using Pt Deposition

The mesostructure of porous electrodes used in lithium-ion batteries strongly influences cell performance. Accurate imaging of the distribution of phases in these electrodes would allow this relationship to be better understood through simulation. However, imaging the nanoscale features in these components is challenging. While scanning electron microscopy is able to achieve the required resolution, it has well established difficulties imaging porous media. This is because the flat imaging planes prepared using focused ion beam milling will intersect with the pores, which makes the images hard to interpret as the inside walls of the pores are observed. It is common to infiltrate porous media with resin prior to imaging to help resolve this issue, but both the nanoscale porosity and the chemical similarity of the resins to the battery materials undermine the utility of this approach for most electrodes. In this study, a technique is demonstrated which uses in situ infiltration of platinum to fill the pores and thus enhance their contrast during imaging. Reminiscent of the Japanese art of repairing cracked ceramics with precious metals, this technique is referred to as the kintsugi method. The images resulting from applying this technique to a conventional porous cathode are presented and then segmented using a multi-channel convolutional method. We show that while some cracks in active material particles were empty, others appear to be filled (perhaps with the carbon binder phase), which will have implications for the rate performance of the cell. Energy dispersive X-ray spectroscopy was used to validate the distribution of phases resulting from image analysis, which also suggested a graded distribution of the binder relative to the carbon additive. The equipment required to use the kintsugi method is commonly available in major research facilities and so we hope that this method will be rapidly adopted to improve the imaging of electrode materials and porous media in general.

25 ENERGY STORAGE↗
DOE OSTI2020

Micrometer-accuracy 2D displacement interferometer with plasmonic metasurface resonators

In this Letter, a high-accuracy, two-dimensional displacement sensor is proposed, designed, and demonstrated based on the concept of an extrinsic Fabry–Perot Interferometer. The sensor is composed of two bundled single-mode optic fibers in parallel and two plasmonic metasurface resonators inscribed on a gold substrate via a focused ion beam. The fiber end surface and the metasurface are in parallel with a small cavity between. The cavity change or Z -component displacement is determined from the pattern of interference fringes. The X -component displacement, perpendicular to the Z component, is identified from wavelength-selective metasurface resonators, which possess unique resonant wavelengths due to different nanostructure designs. The sensor was calibrated with six displacements applied through a three-axis precision linear stage. Test results indicated that the proposed interferometer can measure displacements with a maximum error of 5.4 µm or 2.2%.

Guo, Chuanrui (ORCID:0000000271412972)↗