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DOE OSTI2023

In operando cryo-STEM of pulse-induced charge density wave switching in TaS 2

The charge density wave material 1T-TaS 2 exhibits a pulse-induced insulator-to-metal transition, which shows promise for next-generation electronics such as memristive memory and neuromorphic hardware. However, the rational design of TaS 2 devices is hindered by a poor understanding of the switching mechanism, the pulse-induced phase, and the influence of material defects. Here, we operate a 2-terminal TaS 2 device within a scanning transmission electron microscope at cryogenic temperature, and directly visualize the changing charge density wave structure with nanoscale spatial resolution and down to 300 μs temporal resolution. We show that the pulse-induced transition is driven by Joule heating, and that the pulse-induced state corresponds to the nearly commensurate and incommensurate charge density wave phases, depending on the applied voltage amplitude. With our in operando cryogenic electron microscopy experiments, we directly correlate the charge density wave structure with the device resistance, and show that dislocations significantly impact device performance. This work resolves fundamental questions of resistive switching in TaS 2 devices, critical for engineering reliable and scalable TaS 2 electronics.

36 MATERIALS SCIENCE↗

DOE OSTI2020

Origin and Suppression of Beam Damage-Induced Oxygen-K Edge Artifact from γ-Al 2 O 3 using Cryo-EELS

Gamma-alumina (γ-Al 2 O 3 ), like other low-Z oxides, is readily damaged when exposed to an electron beam. This typically results in the formation of a characteristic pre-edge peak in the oxygen-K edge of electron energy-loss spectra (EELS) acquired during or after the damage process. This artifact can mask the presence of intrinsic O-K edge fine structure that would reveal chemical properties of the material; therefore, its suppression is key. In this work, we systematically investigate the conditions that give rise to the damage-induced O-K pre-edge peak and show that it can be effectively suppressed by performing EELS experiments at cryogenic (cryo) temperatures. Prolonged exposure of γ-Al 2 O 3 to a focused electron beam results in a hole bored through the sample; this was used as a reproducible beam damage condition. O-K edge EELS spectra were collected from a single-crystal γ-Al 2 O 3 sample both during and after focused 2 electron beam hole drilling, and at room and cryo temperatures, using a monochromated scanning transmission electron microscope (STEM). Furthermore, the characteristic 531 eV pre-edge peak visible in the room temperature EELS spectra was completely suppressed in the cryo-EELS spectra, even in the presence of a visible drilled hole. We then correlated these experimental observations with multiple-scattering EELS simulations to determine the likely atomistic origin of the damage-induced O-K pre-edge peak. The findings indicate that the pre-edge peak is caused primarily by the presence of surface O dimer (O-O) bonds formed during beam damage, and that operating at cryo temperature suppresses the formation of surface O-O bonds, thus preventing formation of the O-K pre-edge peak. Additionally, Al-L 2,3 edge EELS spectra revealed Al loss primarily from tetrahedral sites during hole drilling.

77 NANOSCIENCE AND NANOTECHNOLOGY↗

NASA NTRS2016

Spectral Monitoring of Volatiles During Drilling into Frozen Lunar Simulant

NASA's Resource Prospector (RP) project intends to characterize the 3D distribution of volatiles in permanently shadowed regions at the lunar poles. One RP remote sensing instrument is a near-infrared spectrometer with an associated camera and radiometer, called the Near-InfraRed Volatile Spectrometer System (NIRVSS). In May 2016, NIRVSS, a Honeybee Robotics drill, and an Inficon mass spectrometer were placed in a vacuum chamber at Glenn Research Center. Also inside was a tube (1.2 m high x 25 cm diameter) filled with lunar simulant NU-LHT-3M, initially doped with a homogeneous water abundance of ~5%, chilled to cryogenic temperatures and exposed to a vacuum (~10e-6 Torr). During drilling, the NIRVSS instruments observed the cuttings pile as subsurface materials were emplaced on the surface. Spectral features associated with water ice, near 2000 and 3000 nm, were measured by the spectrometer during drilling. The spectral data documents development of a desiccated soil layer in the tube down to ~25-30 cm (confirmed by post-test soil analyses), formed during the initial pump down to vacuum. Drilling occurred in 10 cm segments, with the drill stem extracted and flutes brushed after each 10 cm depth. One exception to this was the 40 cm depth segment where the soil was delivered to a sample capture mechanism, and sealed for post-test analyses. To ~30 cm depth the greatest 2000 and 3000 nm signatures were associated with brushing of the drill flutes above the surface. At depths >40 cm the strongest ice signatures were associated with the drill clearing soil from the existing hole, or beginning to encounter new material. For these greater depths, brushing the flutes after extraction produced much weaker ice signatures than for shallower depths. This suggests that the soil may remain trapped in the exit funnel and is not emplaced on the surface. After each event creating strong ice signatures, these signatures decreased to near background levels in 5 minutes or less, due to surface exposure to vacuum.

lunar poles↗

DOE OSTI2026

Multiscale Cryo Electron Microscopy Reveals Interfacial Degradation and Stabilization in Battery Electrodes

Electrochemical interfaces are dynamic systems, evolving based on their local environment and reactant surface structures. The electrode-electrolyte interface in Li-ion batteries can be protective, limiting parasitic reactions with the electrolyte to passivate the surface [1]. Additionally, this interphase has an impact on the Li-ion transport through that layer based on its composition, bonding environment, and thickness. These parameters are challenging to collect and may vary depending on the electrode surface site investigated relative to its spatial position in a coin cell. This study will detail a multiscale cryogenic electron microscopy approach where millimeter-scale cross-sections through the coin cell batteries were made using a cryogenic stage within a fs-laser plasma focused ion beam (laser PFIB) with complementary energy dispersive X-ray spectroscopy able to detect variations in the composition at electrode interfaces [2]. Microscale cross-sectioning and lamella sample preparation of battery electrodes was conducted at the Center for Integrated Nanotechnologies using a Ga-ion focused ion beam (FIB) with air-free and cryo-transfer [3], followed by nanoscale mapping of composition and bonding within the CEI through cryo-scanning transmission electron microscopy (cryo-STEM) electron energy loss spectroscopy [4]. This multiscale approach enabled identification of millimeter-scale features of a battery stack with visualization of degradation in electrodes such as cracks in cathode particles, gas evolution, and SEI evolution; microscale interfacial characteristics, such as heterogeneity in the SEI or barrier layer and identification of electrolyte networks to the electrode surfaces; and nanoscale measurement of the CEI thickness, mapping of transition metal bonding within the cathode particles to identify loss of active materials, and identification of beneficial electrolyte additives incorporated into the CEI structure. This multiscale approach allows for a statistical understanding of the primary mechanisms and parasitic degradation pathways that impact performance by limiting the ion transport pathways within Li+ batteries.

36 MATERIALS SCIENCE↗

DOE OSTI2026

Systems-To-Atoms (S2A): enabling hydrogen for climate security

The project addresses a critical gap in hydrogen infrastructure by integrating system-level energy models with atomic-scale material simulations in a unified Systems-to-Atoms (S2A) framework. The motivation stems from the need to develop efficient, cost-effective, and durable hydrogen transport and utilization technologies to support decarbonization of hard-to-electrify sectors such as heavy-duty transportation. Current system models lack awareness of material performance mechanisms, while material-scale models do not account for system-level usage and variability. To bridge this divide, the team developed a co-simulation capability linking techno-economic analyses, reactor/process-flow modeling, and molecular-scale catalysis simulations. Applied to hydrogen delivery in California, the framework enabled comparative evaluations of compressed, cryogenic, and liquid organic hydrogen carrier (LOHC) pathways, highlighting how catalyst operation and unit process efficiency influence overall performance. The results demonstrate that no single material or transport mode is universally optimal; instead, heterogeneous solutions tuned to specific operational contexts deliver better performance. The project delivers a new capability for cross-scale material co-design, advancing hydrogen infrastructure readiness and informing DOE and LLNL missions in climate and energy resilience.

organic↗

NASA NTRSDate not supplied

2024 Nasa Lunabotics University Competition: Site Preparation With Bulk Regolith

Introduction: Lunabotics provides accredited institutions of higher learning students (vocational-technical, college, university) an opportunity to apply the NASA systems engineering process to design and build a prototype robot. This robot would be capable of performing the proposed operations on the Lunar surface in support of future Artemis mission goals. Lunabotics features a systems engineering design challenge to engage students in the next phase of hu-man space exploration supporting the Artemis missions. This two-semester event encourages students to design and build an autonomous or telerobotic robot designed to traverse the simulated Lunar surface and complete the assigned construction tasks. The number of teams accepted into this challenge is not predetermined but is based on the scores and overall quality of the Project Management Plans received and other factors. The culmination of the Lunabotics virtual challenge will be the design, build and operation of a functional prototype Lunar robot. Teams are required to submit the following: (1) Project Management Plan, (2) Systems Engineering Paper, a (3) STEM Engage-ment Report, and a (4) Proof of Life Video. This is an optional item, but to qualify for the grand prize a team must also submit a: (5) Presentation and Demonstration. Background: The NASA Lunabotics University Competition was first held in 2010 as a follow on to the NASA Regolith Excavation Challenge [1]. The high level of interest and participation from over 50 universities each year has led to a sustained annual competi-ion cadence: it has been held every May for the past 14 years [2,3]. Over 6,000 students have participated and been inspired to pursue Science, Technology, En-gineering and Mathematics careers (STEM). 2024 Competition: The necessary lunar surface tasks are evolving to meet the NASA Artemis Mission requirements. In the past Lunabotics challenges we gathered data to support Lunar mining for consuma-bles in the Lunar regolith. Now, in 2024, the task is to gather data on Lunar site preparation and construction by designing and building a robot that will traverse the chaotic Lunar terrain and construct a regolith-based berm. The goal is to build a berm structure which would be useful to the Artemis Mission for blast and ejecta protection during lunar landings and launches, shading cryogenic propellant tank farms, providing radiation protection around a nuclear power plant and other mission critical uses. Lunabotics will consist of three separate events this year. The first event is NASA’s Lunabotics Project Development Challenge, where teams submit various deliverables to be scored by judges. The second event will be the University of Central Florida (UCF) Lunabotics Qualification challenge, in the Exolith laboratory, where teams will put their de-signs to the test. The top ten scoring teams from the Qualification challenge are then invited to the third and final event, NASA’s Lunabotics On-Site Challenge at Kennedy Space Center in Florida. This presentation will summarize the results and lessons learned from the NASA Lunabotics University Competition held in May 2024.

Lunabotics↗

DOE OSTI2025

Heat load measurements for the PIP-II pHB650 cryomodule

This study presents a brief overview of the 1st and 2nd phases and an in-depth analysis of the 3rd phase heat load testing performed on the pHB650 (prototype High Beta 650 MHz) cryomodule at PIP2IT (PIP-II Injector Test Facility), with a focus on both the results and the methodological advancements that have improved testing efficiency and accuracy. A key challenge identified in the testing campaign is the higher-than-expected heat loads observed in the first PIP-II (Proton Improvement Plan II) prototype cryomodules (pSSR1 and pHB650) tested at PIP2IT. Elevated heat loads are concerning given the fixed capacity of the PIP-II cryoplant that is currently being installed at Fermilab. However, understanding the sources of these elevated heat loads offers a critical opportunity to implement effective heat load mitigations on upcoming PIP-II cryomodules to stay within the available capacity of the PIP-II cryoplant. The study includes a summary of test results, descriptions of measurement procedures, and key observations on parameters directly and indirectly related to heat load measurements. Direct observations include measured heat loads and the effectiveness of JT heat exchanger under varying conditions, while indirect observation analyze factors such as the temperature distribution on the two-phase pipe and relief piping under varying conditions. Thermal acoustic oscillations (TAO) were identified during testing, which was mitigated by replacing the original G10 stem with a stainless steel stem equipped with wipers for the cryomodule cooldown valve. A major innovation during pHB650 Phase 3 testing was the development of an automated Python script to streamline data acquisition, analysis, and reporting of heat load results. This script automatically retrieved data from ACNET (Accelerator Control Network), performed heat load calculations, and generated detailed reports featuring plots and tables. This advancement significantly reduced manual labor and enhanced the thoroughness of data analysis compared to earlier campaigns. The heat load test reports were promptly uploaded to the electronic logbook shortly after each test, enabling rapid feedback and collaboration between the SRF and cryogenic teams. The heat load measurements included various components: HTTS (high-temperature thermal shield), LTTS (low-temperature thermal shield), 2K isothermal and non-isothermal heat loads. Results were recorded both within the cryomodule and between the bayonet can supply and return. Measurements were conducted under different operating conditions such as "standard", "linac", and "simulated dynamic". Additionally, HTTS and LTTS heat loads were calculated in real time, allowing for the tracking of thermal stability and identification of changes during testing, both in steady-state and transient conditions. The results of this testing campaign not only provide valuable insights into the performance of the pHB650 cryomodule but also highlight best practices and lessons learned that will inform future cryomodule testing at PIP2IT. These include adopting automated tools for data analysis, refining real-time measurement capabilities, and emphasizing detailed pre-test planning. The framework established in this campaign aims to set an improved standard for cryomodule testing and heat load reporting in future cryomodule test campaigns.

Porwisiak, D. [Fermilab; Wroclaw Tech. U.]↗

NASA NTRS2017

Heat Loads Due to Small Penetrations in Multilayer Insulation Blankets

The main penetrations (supports and piping) through multilayer insulation systems for cryogenic tanks have been previously addressed by heat flow measurements. Smaller penetrations due to fasteners and attachments are now experimentally investigated. The use of small pins or plastic garment tag fasteners to each the handling and construction of multilayer insulation (MLI) blankets goes back many years. While it has long been understood that penetrations and other discontinuities degrade the performance of the MLI blanket, quantification of this degradation has generally been lumped into gross performance multipliers (often called degradation factors or scale factors). Small penetrations contribute both solid conduction and radiation heat transfer paths through the blanket. The conduction is down the stem of the structural element itself while the radiation is through the hole formed during installation of the pin or fastener. Analytical models were developed in conjunction with MLI perforation theory and Fouriers Law. Results of the analytical models are compared to experimental testing performed on a 10 layer MLI blanket with approximately 50 small plastic pins penetrating the test specimen. The pins were installed at 76-mm spacing inches in both directions to minimize the compounding of thermal effects due to localized compression or lateral heat transfer. The testing was performed using a liquid nitrogen boil-off calorimeter (Cryostat-100) with the standard boundary temperatures of 293 K and 78 K. Results show that the added radiation through the holes is much more significant than the conduction down the fastener. The results are shown to be in agreement with radiation theory for perforated films.

Structural attachments↗

DOE OSTI2026

Numerical Investigation of Fluid Flow and Space Charge in Liquid Argon Time Projection Chamber (LArTPC) Detectors

Overview This project focused on developing a high-fidelity numerical framework to simulate the multiphysics environment within Liquid Argon Time Projection Chamber (LArTPC) detectors. The primary objective was to characterize the complex interplay between ion transport, background fluid dynamics, and electric field distortions—a critical factor for the calibration and sensitivity of next-generation High Energy Physics experiments, such as DUNE. Technical Achievements The research successfully yielded a hybrid numerical space-charge solver utilizing a Cell-Centered Finite Volume Method (FVM) for ion transport coupled with a Finite Element Method (FEM) for electric potential. Key accomplishments include: • Verification & Validation: The 3-D solver was rigorously verified against 1-D analytical solutions, demonstrating high numerical accuracy in predicting space-charge-induced field deviations. • Field Distortion Analysis: 3D simulations revealed that space charge effects introduce significant non-uniformities in the electric field. Critically, the research identified that background LAr flow velocities, when comparable to ion drift velocities, markedly exacerbate these distortions. • Technology Transfer: The resulting source code and comprehensive user manuals were successfully transferred to collaborators at Fermilab, providing a portable computational tool for the broader scientific community. Challenges and Future Directions While the space-charge solver achieved all performance metrics, the integrated fluid dynamics modeling encountered convergence challenges stemming from the extreme 200-fold disparity in length scales between the detector's 37 mm inlet pipes and the 8-meter global domain. To address this, the project has identified a clear technical pivot toward Hierarchical Geometric Adaptive Mesh Refinement (HG-AMR). By implementing an h-type refinement strategy with hanging nodes, future iterations of this solver will be capable of resolving localized high-gradient inlet flows without the prohibitive computational costs of regular grids. This advancement, combined with data-driven uncertainty quantification based on MicroBooNE-style calibration, will enable the precise modeling of detector responses in large-scale cryogenic environments where direct measurement remains difficult. Impact The computational tools developed under this award provide a foundation for enhancing the energy resolution and spatial reconstruction of noble liquid detectors. By bridging the gap between theoretical fluid dynamics and experimental field calibration, this work supports the DOE’s mission to advance the frontiers of neutrino physics and dark matter detection.

42 ENGINEERING↗

DOE OSTI2021

Ambient-Temperature Hydrogen Storage via Vanadium(II)-Dihydrogen Complexation in a Metal-Organic Framework

In this report, the widespread implementation of H 2 as a fuel is currently hindered by the high pressures or cryogenic temperatures required to achieve reasonable storage densities. In contrast, the realization of materials that strongly and reversibly adsorb hydrogen at ambient temperatures and moderate pressures could transform the transportation sector and expand adoption of fuel cells in other applications. To date, however, no adsorbent has been identified that exhibits a binding enthalpy within the optimal range of -15 to -25 kJ/mol for ambient-temperature hydrogen storage. Here, we report the hydrogen adsorption properties of the metal-organic framework (MOF) V 2 Cl 2.8 (btdd) (H 2 btdd, bis(1 H -1,2,3-triazolo[4,5- b ],[4',5'- i ])dibenzo[1,4]dioxin), which features exposed vanadium(II) sites capable of backbonding with weak π acids. Significantly, gas adsorption data reveal that this material binds H 2 with an enthalpy of -21 kJ/mol. This binding energy enables usable hydrogen capacities that exceed that of compressed storage under the same operating conditions. The Kubas-type vanadium(II)-dihydrogen complexation is characterized by a combination of techniques. From powder neutron diffraction data, a V-D 2 (centroid) distance of 1.966(8) Å is obtained, the shortest yet reported for a MOF. Using in situ infrared spectroscopy, the H-H stretch was identified, and it displays a red shift of 242 cm -1 . Electronic structure calculations show that a main contribution to bonding stems from the interaction between the vanadium d π and H 2 σ* orbital. Ultimately, the pursuit of MOFs containing high densities of weakly π-basic metal sites may enable storage capacities under ambient conditions that far surpass those accessible with compressed gas storage.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2024

Real-space visualization of a defect-mediated charge density wave transition

Here, we study the coupled charge density wave (CDW) and insulator-to-metal transitions in the 2D quantum material 1T-TaS 2 . By applying in situ cryogenic 4D scanning transmission electron microscopy with in situ electrical resistance measurements, we directly visualize the CDW transition and establish that the transition is mediated by basal dislocations (stacking solitons). We find that dislocations can both nucleate and pin the transition and locally alter the transition temperature T c by nearly ~75 K. This finding was enabled by the application of unsupervised machine learning to cluster five-dimensional, terabyte scale datasets, which demonstrate a one-to-one correlation between resistance—a global property—and local CDW domain-dislocation dynamics, thereby linking the material microstructure to device properties. This work represents a major step toward defect-engineering of quantum materials, which will become increasingly important as we aim to utilize such materials in real devices.

4D-STEM↗

NASA NTRS2013

Massively Clustered CubeSats NCPS Demo Mission

Technologies under development for the proposed Nuclear Cryogenic Propulsion Stage (NCPS) will require an un-crewed demonstration mission before they can be flight qualified over distances and time frames representative of a crewed Mars mission. In this paper, we describe a Massively Clustered CubeSats platform, possibly comprising hundreds of CubeSats, as the main payload of the NCPS demo mission. This platform would enable a mechanism for cost savings for the demo mission through shared support between NASA and other government agencies as well as leveraged commercial aerospace and academic community involvement. We believe a Massively Clustered CubeSats platform should be an obvious first choice for the NCPS demo mission when one considers that cost and risk of the payload can be spread across many CubeSat customers and that the NCPS demo mission can capitalize on using CubeSats developed by others for its own instrumentation needs. Moreover, a demo mission of the NCPS offers an unprecedented opportunity to invigorate the public on a global scale through direct individual participation coordinated through a web-based collaboration engine. The platform we describe would be capable of delivering CubeSats at various locations along a trajectory toward the primary mission destination, in this case Mars, permitting a variety of potential CubeSat-specific missions. Cameras on various CubeSats can also be used to provide multiple views of the space environment and the NCPS vehicle for video monitoring as well as allow the public to "ride along" as virtual passengers on the mission. This collaborative approach could even initiate a brand new Science, Technology, Engineering and Math (STEM) program for launching student developed CubeSat payloads beyond Low Earth Orbit (LEO) on future deep space technology qualification missions. Keywords: Nuclear Propulsion, NCPS, SLS, Mars, CubeSat.

Robertson, Glen A.↗

DOE OSTI2023

Kinetic pathways of fast lithium transport in solid electrolyte interphases with discrete inorganic components

The transport of lithium ions in the solid electrolyte interphase (SEI) has been previously accepted to proceed in two steps: a fast pore diffusion through the outer, porous organic layer followed by a slow knock-off or vacancy diffusion in the inner, dense inorganic layer. The second step is believed to be the rate-limiting step during fast-charging. In this study, we have intentionally constructed a thicker SEI (SEI-rich) structure on the surface of monoclinic Nb 2 O 5 (H-Nb 2 O 5 ) by adding LiNO 3 into a conventional ethylene carbonate based electrolyte. The electrochemical performance of two electrodes, one SEI-rich and one with few SEI (SEI-lean), was found to be almost the same, including their fast-charging capability and cycling stability, despite the significant difference in their SEI structure. Importantly, analysis using cryogenic scanning/transmission electron microscopy showed the discrete decoration of individual inorganic particles (e.g., Li 2 O) and amorphous species (LiN x O y /organic components) over the surface of H-Nb 2 O 5 . These discrete inorganic particles are in contradiction to the formation of dense inner inorganic layer, which has been commonly postulated. Based on these findings, we propose a new mechanism for Li ion transport through the SEI: one-step pore diffusion, without the second step slow diffusion. This one-step pore diffusion process provides an extremely fast Li ion transport, and effectively removes the kinetic limitation of Li ion transport in the SEI for fast charging. Finally, these results strongly suggest that the influence of SEI structure on the transport kinetics of lithium ions is much less significant than previously accepted. These results offer a new understanding of possible lithium ion transport pathway within SEI and may have implications for the future designs of fast-charging battery materials.

25 ENERGY STORAGE↗

DOE OSTI2026

Freeze It or Leave It? Evaluating the Role of Cryo-Electron Microscopy in Battery Research

Cryogenic electron microscopy (cryo-EM) continues to gain prominence in materials science, particularly in battery research where it has enabled high-resolution, multimodal characterization of electrode materials and interfaces that otherwise degrade quickly under electron beam irradiation. But as anyone who has attempted cryo-EM techniques knows, freezing comes at a cost; cryo-EM experiments are time-consuming, highly sensitive, and carry an increased risk of artifacts due to issues such as frost contamination. Thus, when planning new characterization of battery materials or other beam-sensitive samples, it is critical to consider whether (and which) cryo-EM techniques are appropriate, based on study goals and an understanding of electron beam-sample interactions. Here we review such considerations for battery materials to elucidate the questions of when, why, and how to freeze to achieve high-quality characterization.

25 ENERGY STORAGE↗