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All sourcesNASA NTRSDOE OSTI
DOE OSTI2024

Field-resolved space–time characterization of few-cycle structured light pulses

Accompanied by the rapid development of ultrafast laser platforms in recent decades, the spatiotemporal manipulation of ultrashort laser pulses has attracted much attention due to the potential for cutting-edge applications of structured light, including optical tweezers, optical communications, super-resolution imaging, time-resolved spectroscopy in molecules and quantum materials, and strong-field physics. Today, techniques capable of characterizing the full spatial, temporal, and polarization state properties of structured light are strongly desired. Here, we demonstrate a technique, termed 3D TIPTOE, for characterizing structured mid-infrared waveforms, which uses only a two-dimensional silicon-based image sensor as both the detector and the nonlinear medium. By combining the advantages of the sub-cycle time resolution afforded by nonlinear excitation and the spatial resolution inherent to the two-dimensional sensor, the 3D TIPTOE technique allows full characterization of structured electric fields, significantly reducing the complexity of detection compared to other techniques. The validity of the technique is established by measuring both few-cycle Bessel–Gaussian pulses and radially polarized femtosecond vector beams.

Liu, Yangyang (ORCID:0000000335205332)↗
NASA NTRS1992

Multi-Mode Excitation and Data Reduction for Fatigue Crack Characterization in Conducting Plates

Advances in the technique of fatigue crack characterization by resonant modal analysis have been achieved through a new excitation mechanism and data reduction of multiple resonance modes. A non-contacting electromagnetic device is used to apply a time varying Lorentz force to thin conducting sheets. The frequency and direction of the Lorentz force are such that resonance modes are generated in the test sample. By comparing the change in frequency between distinct resonant modes of a sample, detecting and sizing of fatigue cracks are achieved and frequency shifts caused by boundary condition changes can be discriminated against. Finite element modeling has been performed to verify experimental results.

Wincheski, B.↗
DOE OSTI2024

An Investigation of Oxides of Tantalum Produced by Pulsed Laser Ablation and Continuous Wave Laser Heating

Recent progress has seen multiple Ta 2 O 5 polymorphs generated by different synthesis techniques. However, discrepancies arise when these polymorphs are produced in widely varying thermodynamic conditions and characterized using different techniques. This work aimed to characterize and compare Ta 2 O 5 particles formed at high and low temperatures using nanosecond pulsed laser ablation (PLA) and continuous wave (CW) laser heating of a local area of tantalum in either air or an 18 O 2 atmosphere. Scanning electron microscopy (SEM) and Raman spectroscopy of the micrometer-sized particles generated by PLA were consistent with either a localized amorphous Ta 2 O 5 phase or a similar, but not identical, crystalline β-Ta 2 O 5 phase. The Raman spectrum of the material formed at the point of CW laser impingement was in good agreement with the previously established ceramic “H-Ta 2 O 5 ” phase. TEM and electron diffraction analysis of these particles indicated the phase structure matched an oxygen-vacated superstructure of monoclinic H-Ta 2 O 5 . Further from the point of laser impingement, CW heating produced particles with a Raman spectrum that matched β-Ta 2 O 5 . We confirmed that the high-temperature ceramic phase characterized in previous work by Raman spectroscopy was the same monoclinic phase characterized in different work by TEM and could be produced by direct laser heating of metal in air.

36 MATERIALS SCIENCE↗
DOE OSTI2026

Revealing Local Structures through Machine-Learning-Fused Multimodal Spectroscopy

Atomistic structures of materials offer valuable insights into their functionality. Determining these structures remains a fundamental challenge in materials science, especially for systems with defects. While both experimental and computational methods exist, each has limitations in resolving nanoscale structures. Core-level spectroscopies, such as X-ray absorption (XAS) or electron energy-loss spectroscopies (EELS), have been used to determine the local bonding environment and structure of materials. Recently, machine learning (ML) methods have been applied to extract structural and bonding information from XAS/EELS data. However, frameworks relying solely on a single data stream, defined as characterization data derived from a single element using one technique, are often insufficient because multiple local environments can yield similar spectral features, making it challenging to differentiate between competing structural hypotheses. Here, in this work, we address this challenge by integrating multimodal ab initio simulations, experimental data acquisition, and ML techniques for structure characterization. Our goal is to determine local structures and properties using EELS and XAS data from multiple elements and edges. To showcase our approach, we use various lithium nickel manganese cobalt (NMC) oxide compounds which are used for lithium ion batteries, including those with oxygen vacancies and antisite defects, as the sample material system. We successfully inferred local element content, ranging from lithium to transition metals, with quantitative agreement with experimental data. Beyond local element inference, we find that ML model based on multimodal spectroscopic data is able to determine whether local defects such as oxygen vacancy and antisites are present, a task which is impossible for single mode spectra or other experimental techniques. Furthermore, our framework is able to provide physical interpretability, bridging spectroscopy with the local atomic and electronic structures.

battery↗
DOE OSTI2022

LLNL FY22 Aging and Lifetimes Exit Criteria (Milestone 8118, GC#5)

This report introduces a novel characterization tool that can rapidly collect in-situ time-dependent oxide thickness and hydride growth data together with spatial data using while-light interferometry. White-light interferometry is a non-destructive and non-contact optical surface profiling technique for materials characterization that offers excellent lateral and vertical resolution. A depleted uranium sample was used to assess the ability of white-light interferometry to provide quantitative corrosion reaction rates at metal surfaces for by hydriding and oxidation and compare this technique to existing characterization tools for capturing early-stage hydride and oxide growth kinetics.

36 MATERIALS SCIENCE↗
DOE OSTI2024

Continuously tunable uniaxial strain control of van der Waals heterostructure devices

Uniaxial strain has been widely used as a powerful tool for investigating and controlling the properties of quantum materials. However, existing strain techniques have so far mostly been limited to use with bulk crystals. Although recent progress has been made in extending the application of strain to two-dimensional van der Waals (vdW) heterostructures, these techniques have been limited to optical characterization and extremely simple electrical device geometries. Here, we report a piezoelectric-based in situ uniaxial strain technique enabling simultaneous electrical transport and optical spectroscopy characterization of dual-gated vdW heterostructure devices. Critically, our technique remains compatible with vdW heterostructure devices of arbitrary complexity fabricated on conventional silicon/silicon dioxide wafer substrates. We demonstrate a large and continuously tunable strain of up to –0.15% at millikelvin temperatures, with larger strain values also likely achievable. We quantify the strain transmission from the silicon wafer to the vdW heterostructure, and further demonstrate the ability of strain to modify the electronic properties of twisted bilayer graphene. Our technique provides a highly versatile new method for exploring the effect of uniaxial strain on both the electrical and optical properties of vdW heterostructures and can be easily extended to include additional characterization techniques.

Electrical properties and parameters↗
NASA NTRS2016

Characterization of Carbon Dioxide Washout Measurement Techniques in the Mark-III Space Suit

Providing adequate carbon dioxide (CO2) washout is essential to the reduction of risk in performing suited operations. Long term CO2 exposure can lead to symptoms such as headache, lethargy, dizziness, and in severe cases can lead to unconsciousness and death. Thus maintaining adequate CO2 washout in both ground testing and during in flight EVAs is a requirement of current and future suit designs. It is necessary to understand the inspired CO2 of suit wearers such that future requirements for space suits appropriately address the risk of inadequate washout. Testing conducted by the EVA Physiology Laboratory at the NASA Johnson Space Center aimed to characterize a method for noninvasively measuring inspired oronasal CO2 under pressurized suited conditions in order to better inform requirements definition and verification techniques for future CO2 washout limits in space suits. Prior work conducted by the EPL examined several different wearable, respirator style, masks that could be used to sample air from the vicinity surround the nose and mouth of a suited test subject. Previously published studies utilized these masks, some being commercial products and some novel designs, to monitor CO2 under various exercise and flow conditions with mixed results for repeatability and/or consistency between subjects. Based on a meta-analysis of those studies it was decided to test a nasal cannula as it is a commercially available device that is placed directly in the flow path of the user as they breathe. A nasal cannula was used to sample air inhaled by the test subjects during both rest and exercise conditions. Eight subjects were tasked with walking on a treadmill or operating an arm ergometer to reach target metabolic rates of 1000, 2000, and 3000 BTU/hr. Suit pressure was maintained at 4.3 psid for all tests, with supply flow rates of 6, 4, and 2 actual cubic feet per minute depending on the test condition. Each test configuration was conducted twice with subjects breathing either through their nose only, or however they felt comfortable. By restricting breathing through a single orifice, we are able to more accurately define exactly what flow stream the sampled CO2 is taken from. Oronasal CO2 was monitored using real time infrared gas analyzers fed via sample tubes connected to the nasal cannula within the suit. Two additional sampling tubes were placed at the head and chin of the test subject, in an effort to capture CO2 concentrations across the entire flow stream of the Mark-III vent system (flow path is head to neck). Metabolic rate was calculated via the exhaust CO2 concentration and used to adjust subject workload on either the treadmill or arm ergometer until the target was reached. Forward work will aim to characterize the historically accepted minimum ppCO2 in suit during EVA by repeating this study in the Extravehicular Mobility Unit (EMU) space suit. This will help to define washout requirements for future suits, be they NASA (e.g. Z-2) or Commercial Crew designed. Additionally it is important to determine the functional consequences of CO2 exposure during EVA. Severe CO2 symptoms are a result of very high concentration, acute exposures. While long term, low concentration exposures have been shown to result in slight cognitive decline, symptoms resolve upon quickly returning to nominal concentrations and it remains unknown the impact that minor deficits in cognitive performance can have on EVA performance.

Norcross, J.↗
DOE OSTI2025

Multiscale Characterization of Additive Manufacturing Components with Computed Tomography, 3D X-ray Microscopy, and Deep Learning

Additive manufacturing (AM) facilitates the creation of complex-geometry parts, driving advancements in lightweight aerospace components, high-efficiency engine cooling channels, and customized medical implants. However, ensuring the quality and reliability of AM parts remains challenging due to internal defects, surface irregularities, porosity, and residual trapped powder, which are often inaccessible to traditional inspection methods. Recent developments in X-ray computed tomography (XCT) and 3D X-ray microscopy (XRM), particularly systems equipped with resolution-at-a-distance (RaaD™) capabilities, enable high-resolution, non-destructive evaluation of AM components across multiple scales, from sub-micrometer to macroscopic levels. This paper explores modern XCT and XRM techniques for multiscale characterization of AM parts, focusing on their ability to detect and analyze defects such as porosity, cracks, inclusions, and surface roughness, while offering insights into defect formation mechanisms, material properties, and process-induced variations. The integration of deep learning (DL) frameworks, including Simurgh, DeepRecon, and DeepScout, enhances XCT/XRM workflows by reducing scan times, improving resolution recovery, and enabling accurate defect detection even with limited projection data. These DL-based methods overcome limitations of traditional reconstruction techniques, enabling faster, more reliable characterization of dense materials like Inconel 718 and novel alloys such as AlCe. Applications include process parameter optimization, high-throughput quality control, and multistage AM process evaluation, with DL-enhanced workflows accelerating analysis times from weeks to days. Correlative imaging approaches further validate XCT and XRM data against scanning electron microscopy (SEM) images of physically sectioned samples, confirming the accuracy of DL-based reconstructions and enabling comprehensive defect analysis. While challenges remain in generalizing DL models to diverse materials and imaging conditions, improvements in resolution, noise reduction, and defect detection highlight the transformative potential of these methods. This multiscale and correlative approach enables precise identification and correlation of microstructural features with the overall performance of AM components. By integrating advanced XCT, XRM, and DL techniques, this paper demonstrates a significant leap forward in AM characterization, offering valuable insights into the relationships between processing parameters, microstructure, and part performance, and driving innovations that enhance the quality and reliability of AM products for demanding industrial applications.

Additive manufacturing↗
NASA NTRS1986

RF characterization of monolithic microwave and mm-wave ICs

A number of fixturing techniques compatible with automatic network analysis are presented. The fixtures are capable of characterizing GaAs Monolithic Microwave Integrated Circuits (MMICs) at K and Ka band. Several different transitions are used to couple the RF test port to microstrip. Fixtures which provide chip level de-embedding are included. In addition, two advanced characterization techniques are assessed.

Romanofsky, R. R.↗
NASA NTRS1993

Synopsis of timing measurement techniques used in telecommunications

Historically, Maximum Time Interval Error (MTIE) and Maximum Relative Time Interval Error (MRTIE) have been the main measurement techniques used to characterize timing performance in telecommunications networks. Recently, a new measurement technique, Time Variance (TVAR) has gained acceptance in the North American (ANSI) standards body. TVAR was developed in concurrence with NIST to address certain inadequacies in the MTIE approach. The advantages and disadvantages of each of these approaches are described. Real measurement examples are presented to illustrate the critical issues in actual telecommunication applications. Finally, a new MTIE measurement is proposed (ZTIE) that complements TVAR. Together, TVAR and ZTIE provide a very good characterization of network timing.

Zampetti, George↗
NASA NTRS2016

Characterization of Carbon Dioxide Washout Measurement Techniques in the Mark-III Space Suit

It is essential to provide adequate carbon dioxide (CO2) washout in a space suit to reduce the risks associated with manned operations in space suits. Symptoms of elevated CO2 levels range from reduced cognitive performance and headache to unconsciousness and death at high levels of CO2. Because of this, NASA imposes limits on inspired CO2 levels for space suits when they are used in space and for ground testing. Testing and/or analysis must be performed to verify that a space suit meets CO2 washout requirements. Testing for developmental space suits has traditionally used an oronasal mask that collects CO2 samples at the left and rights sides of the mouth. Testing with this mask resulted in artificially elevated CO2 concentration measurements, which is most likely due to the dead space volume at the front of the mask. The mask also extends outward and into the supply gas stream, which may disrupt the washout effect of the suit supply gas. To mitigate these problems, a nasal cannula was investigated as a method for measuring inspired CO2 based on the assumptions that it is low profile and would not interfere with the designed suit gas flow path, and it has reduced dead space. This test series compared the performance of a nasal cannula to the oronasal mask in the Mark III space suit. Inspired CO2 levels were measured with subjects at rest and at metabolic workloads of 1000, 2000, and 3000 BTU/hr. Workloads were achieved by use of an arm ergometer or treadmill. Test points were conducted at air flow rates of 2, 4, and 6 actual cubic feet per minute, with a suit pressure of 4.3 psid. Results from this test series will evaluate the accuracy and repeatability across subjects of the nasal cannula collection method, which will provide rationale for using a nasal cannula as the new method for measuring inspired CO2 in a space suit. Proper characterization of sampling methods and of suit CO2 washout capability will better inform requirements definition and verification techniques for future CO2 washout limits in space suits

Meginnis, I↗
NASA NTRS1977

Ceramics in gas turbine: Powder and process characterization

Some of the intrinsic properties of various forms of Si3N4 and SiC are listed and limitations of such materials' availability are pointed out. The essential features/parameters to characterize a batch of powder are discussed including the standard techniques for such characterization. In process characterization, parameters in sintering, reaction sintering, and hot pressing processes are discussed including the factors responsible for strength limitations in ceramic bodies. Significant improvements in material properties can be achieved by reducing or eliminating the strength limiting factors with consistent powder and process characterization along with process control.

Dutta, S.↗
NASA NTRS2004

Ionic Liquids and New Proton Exchange Membranes for Fuel Cells

There is currently a great surge of activity in fuel cell research as laboratories across the world seek to take advantage of the high energy capacity provided by &el cells relative to those of other portable electrochemical power systems. Much of this activity is aimed at high temperature fie1 cells, and a vital component of such &el cells must be the availability of a high temperature stable proton-permeable membrane. NASA Glenn Research Center is greatly involved in developing this technology. Other approaches to the high temperature fuel cell involve the use of single- component or almost-single-component electrolytes that provide a path for protons through the cell. A heavily researched case is the phosphoric acid fuel cell, in which the electrolyte is almost pure phosphoric acid and the cathode reaction produces water directly. The phosphoric acid fie1 cell delivers an open circuit voltage of 0.9 V falling to about 0.7 V under operating conditions at 170 C. The proton transport mechanism is mainly vehicular in character according to the viscosity/conductance relation. Here we describe some Proton Transfer Ionic Liquids (PTILs) with low vapor pressure and high temperature stability that have conductivities of unprecedented magnitude for non-aqueous systems. The first requirement of an ionic liquid is that, contrary to experience with most liquids consisting of ions, it must have a melting point that is not much above room temperature. The limit commonly suggested is 100 C. PTILs constitute an interesting class of non-corrosive proton-exchange electrolyte, which can serve well in high temperature (T = 100 - 250 C) fuel cell applications. We will present cell performance data showing that the open circuit voltage output, and the performance of a simple H2(g)Pt/PTIL/Pt/O2(g) fuel cell may be superior to those of the equivalent phosphoric acid electrolyte fuel cell both at ambient temperature and temperatures up to and above 200 C. My work at NASA Glenn Research Center during this summer is to develop and characterize proton exchange membranes doped with ionic liquids. The main techniques used to characterize these materials are: Impedance Spectroscopy, NMR, DSC, TGA, DMA, IR, and SEM ...

Belieres, Jean-Philippe↗
DOE OSTI2023

Emergent Quantum Magnetism and Cryogenic Spin-Memory in Twisted Bilayer Graphene

Recently developed techniques for assembling moiré heterostructures have enabled unprecedented control of the interlayer interactions within the heterostructure, allowing for the realization of strongly correlated electronic states. The experimentally realized states, to date, include a variety of topological states, superconductivity, and strange metal behavior. However, the phenomenology varies significantly from sample to sample. Here we will present microscopy techniques for further characterization of both the progenitor exfoliated materials and the composite moiré heterostructure. The application of these techniques has allowed for an unprecidented degree of characterization in ambient conditions. Additionally we will explore the use of resistively detected electron spin resonance (ESR) as a novel probe for spin order in moirés. While our results do not show clearly dispersive features that would unambiguously evince spin excitations within the sample, the technique is still promising.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2023

Small Angle X-Ray Scattering and Polymers

Polymers are some of the most versatile and useful materials on this planet. Properties of polymers are a result of their processing history, chemical makeup, and physical structure. Therefore, characterization is necessary to develop new polymer formulations and processes. Many established techniques for polymer characterization are destructive, and alternative methods that don’t destroy samples are in high demand. Thermal analysis techniques such as differential scanning calorimetry (DSC) and thermogravimetric analysis (TGA) yield important characteristic information for polymer samples while destroying the sample. Non-destructive strategies such as X ray diffraction (XRD) or small angle X-ray scattering (SAXS) can also find polymer characteristics while preserving a sample’s attributes. Sample preservation is desirable when investigating novel formulation and processing methods. SAXS analysis will be done on two different polymers: polyethylene, and a triblock copolymer. Using these two polymers allows for confidence between tests as polyethylene is very common, and well understood. Polyethylene analysis will be done first, and when methods have been refined so that the SAXS data matches accepted thermal analysis values for HDPE, there will be confidence to use the same analysis on block copolymers. Block copolymers remain relatively unexplored, so SAXS data will yield valuable information on their characteristics. Understanding the mechanical properties of these polymers is paramount to their application in upcycling, a process by which waste plastic can be converted into a higher value commodity. For this project, the upcycling process will be done via 3-dimensional (3d) printing.

36 MATERIALS SCIENCE↗
NASA NTRS2000

Mixing of an Airblast-atomized Fuel Spray Injected into a Crossflow of Air

The injection of a spray of fuel droplets into a crossflow of air provides a means of rapidly mixing liquid fuel and air for combustion applications. Injecting the liquid as a spray reduces the mixing length needed to accommodate liquid breakup, while the transverse injection of the spray into the air stream takes advantage of the dynamic mixing induced by the jet-crossflow interaction. The structure of the spray, formed from a model plain-jet airblast atomizer, is investigated in order to determine and understand the factors leading to its dispersion. To attain this goal, the problem is divided into the following tasks which involve: (1) developing planar imaging techniques that visualize fuel and air distributions in the spray, (2) characterizing the airblast spray without a crossflow, and (3) characterizing the airblast spray upon injection into a crossflow. Geometric and operating conditions are varied in order to affect the atomization, penetration, and dispersion of the spray into the crossflow. The airblast spray is first characterized, using imaging techniques, as it issues into a quiescent environment. The spray breakup modes are classified in a liquid Reynolds number versus airblast Weber number regime chart. This work focuses on sprays formed by the "prompt" atomization mode, which induces a well-atomized and well-dispersed spray, and which also produces a two-lobed liquid distribution corresponding to the atomizing air passageways in the injector. The characterization of the spray jet injected into the crossflow reveals the different processes that control its dispersion. Correlations that describe the inner and outer boundaries of the spray jet are developed, using the definition of a two-phase momentum-flux ratio. Cross-sections of the liquid spray depict elliptically-shaped distributions, with the exception of the finely-atomized sprays which show kidney-shaped distributions reminiscent of those obtained in gaseous jet in crossflow systems. A droplet trajectory analysis overpredicts the liquid mass penetration, and indicates a need for a more rigorous model to account for the three-dimensional mixing field induced by the jet-crossflow interaction. Nonetheless, the general procedures and criteria that are outlined can be used to efficiently assess and compare the quality of sprays formed under different conditions.

Leong, May Y.↗
DOE OSTI2021

Rapid Open-Air Processing of Low-Cost Perovskite Solar Modules

We report an industrially relevant approach to both scalable and fast open-air perovskite photovoltaic (PV) module production. This work resolves some of the most formidable barriers to module-level scaling that the perovskite community has been facing. Key advances include scalable large-area spray deposition, new monolithic integration scribing techniques, advanced photoluminescence characterization, and reproducible high-throughput manufacturability. Our rapid spray processing techniques enabled the highest perovskite PV efficiency produced in open-air. Innovations in scribing techniques enabled the first single-source laser process to achieve perovskite module monolithic integration and technoeconomic analysis led to a comprehensive cost model for perovskite module manufacturing. We report significant progress in reducing perovskite manufacturing costs necessary to potentially compete with incumbent Si-based PV for utility-scale power generation.

cost modeling↗
NASA NTRS1977

Ceramics in gas turbines - Powder and process characterization

The role of powder and process characterization in producing high quality silicon nitride and silicon carbide components, for gas turbine applications, is described. Some of the intrinsic properties of various forms of Si3N4 and SiC are listed and limitations of such materials' availability have been pointed out. The essential features/parameters to characterize a batch of powder have been discussed including the standard techniques for such characterization. In process characterization, parameters in sintering, reaction sintering, and hot pressing processes are discussed including the factors responsible for strength limitations in ceramic bodies. It is inevitable that significant improvements in material properties can be achieved by reducing or eliminating the strength limiting factors with consistent powder and process characterization along with process control.

Dutta, S.↗