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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 19 records
All sourcesNASA NTRSDOE OSTI
DOE OSTI2025

Quantitative Modeling of High-Energy Electron Scattering in Thick Samples Using Monte Carlo Techniques

Cryo-electron microscopy (cryo-EM) is a powerful tool for imaging biological samples but is typically limited by sample thickness, which is restricted to a few hundred nanometers depending on the electron energy. However, there is a growing need for imaging techniques capable of studying biological samples up to 10 µm in thickness while maintaining nanoscale resolution. This need motivates the use of mega-electron-volt scanning transmission electron microscopy (MeV-STEM), which leverages the high penetration power of MeV electrons to generate high-resolution images of thicker samples. In this study, we employ Monte Carlo simulations to model electron–sample interactions and explore the signal decay of imaging electrons through thick specimens. By incorporating material properties, interaction cross-sections for energy loss, and experimental parameters, we investigate the relationship between the incident and transmitted beam intensities. Key factors such as detector collection angle, convergence semi-angle, and the material properties of samples were analyzed. Our results demonstrate that the relationship between incident and transmitted beam intensities follows the Beer–Lambert law over thicknesses ranging from a few microns to several tens of microns, depending on material composition, electron energy, and collection angles. The linear depth of silicon dioxide reaches 3.9 µm at 3 MeV, about 6 times higher than that at 300 keV. Meanwhile, the linear depth of amorphous ice reaches 17.9 µm at 3 MeV, approximately 11.5 times higher than that at 300 keV. These findings are crucial for advancing the study of thick biological and semiconductor samples using MeV-STEM.

36 MATERIALS SCIENCE↗
DOE OSTI2024

Effect of Sample Thickness on the Tensile Strength of Small Graphite Discs

This report formally documents the completion of the Advanced Reactor Technologies (ART) Level 3 Milestone (M3TG-24OR0501054), “Continue activities related to Split Disc-DIC - complete analysis of effect of sample thickness on one fine grain graphite,” due May 31, 2024. Details within this report outline the status of activities aimed at elucidating the effect of sample thickness on the tensile strength measurement using the small-disc, split-disc testing standard in support of the US Department of Energy’s ART Graphite R&D Program. The ASTM D8289, Standard Test Method for Tensile Strength Estimate by Disc Compression of Manufactured Graphite, was developed to provide an alternative means for testing tensile strength on smaller specimens, which are compatible with available irradiation capsule volumes, and other compatibility measurements. ASTM D8289 specifies that acceptable specimen diameter can range from 6 to 12.7 mm and that the maximum allowed sample thickness should be half of the diameter. However, information is limited with respect to the effect of thickness on the measured splitting tensile strength. This report documents efforts to understand the effect of sample thickness on splitting tensile strength. The work involved testing Ø12.7 mm samples of fine-grain graphites 2114 and IG-110 of different thicknesses (6.35, 5, 4, and 3 mm). The digital image correlation (DIC) method was applied to the samples, along with the ASTM D8289 Standard, to help interpret the measured results.

36 MATERIALS SCIENCE↗
DOE OSTI2021

A numerical and experimental approach to compare the effect of sample thickness in small in-situ SEM and large ex-situ tensile testing in Alloy 709

ASTM standards for tensile tests define specific sample size requirements regardless of grain size of the material. However, sample size requirements for testing should be considered in conjunction with the number of grains within its reduced cross-sectional area. This is particularly important for in-situ Scanning Electron Microscope (SEM) tensile tests, as they have to be conducted on smaller samples. In this study, a comprehensive experimental and numerical evaluation of the effect of specimen thickness (and the resulting number of grains within the cross-section) were conducted using in-situ SEM tensile test (on submillimeter thick samples) and ex-situ tensile tests (on samples of 0.68–5.9 mm thickness) and the results are compared with FEM simulations outcome. All tests were conducted at room temperature and the results are correlated to the number of grains within the thickness of specimens. The tensile test results indicated that even though the 0.2% proof stress and the tensile strength do not vary for the current range of thicknesses (with number of grains in the cross-section varying from 13 to 118), a difference in necking mechanism exists. Post tensile strength, thinner samples undergo more shear failure and diagonal localized necking whereas thicker samples experience more diffuse necking indicated by decreased area of shear failure at the edges and increased area of dimpled tensile failure at the center of the sample. Further, FEM results complement the experimental findings by showing the formation of conjugated localized shear bands on the upper and lower surface in the 0.68 mm thick sample and shear bands combining to form singular shear bands in thicker samples. These results also confirm the validity of the in-situ SEM tensile tests conducted on thinner samples as long as the required minimum number of grains exist within the cross-section.

36 MATERIALS SCIENCE↗
NASA NTRS1997

Pulse-Echo Ultrasonic Imaging Method for Eliminating Sample Thickness Variation Effects

A pulse-echo, immersion method for ultrasonic evaluation of a material which accounts for and eliminates nonlevelness in the equipment set-up and sample thickness variation effects employs a single transducer and automatic scanning and digital imaging to obtain an image of a property of the material, such as pore fraction. The nonlevelness and thickness variation effects are accounted for by pre-scan adjustments of the time window to insure that the echoes received at each scan point are gated in the center of the window. This information is input into the scan file so that, during the automatic scanning for the material evaluation, each received echo is centered in its time window. A cross-correlation function calculates the velocity at each scan point, which is then proportionalized to a color or grey scale and displayed on a video screen.

Roth, Don J.↗
NASA NTRS1995

Pulse-echo ultrasonic imaging method for eliminating sample thickness variation effects

A pulse-echo, immersion method for ultrasonic evaluation of a material is discussed. It accounts for and eliminates nonlevelness in the equipment set-up and sample thickness variation effects employs a single transducer, automatic scanning and digital imaging to obtain an image of a property of the material, such as pore fraction. The nonlevelness and thickness variation effects are accounted for by pre-scan adjusments of the time window to insure that the echoes received at each scan point are gated in the center of the window. This information is input into the scan file so that, during the automatic scanning for the material evaluation, each received echo is centered in its time window. A cross-correlation function calculates the velocity at each scan point, which is then proportionalized to a color or grey scale and displayed on a video screen.

Roth, Don J.↗
NASA NTRS1977

A technique to correct for sample thickness variations for use with IDAPS X-ray radiograph analysis

The Image Data Processing System (IDAPS) at the Marshall Space Flight Center is used to analyze radiographs of metal samples to qualitatively and quantitatively map compositional variations across the samples. When the X-ray radiographs are of samples having thickness variations, corrections must be made to accomplish compositional analysis. A correction technique is described for cylindrical samples and is applied to radiographs of SPAR Experiment 74-18. Uncorrected and corrected images are shown.

Schafer, C. F.↗
DOE OSTI2025

Experimental study of energy-dependent angular broadening of MeV electron beams for high-resolution imaging in thick samples

In scanning transmission electron microscopy (STEM), spatial resolution is primarily influenced by the projected size of the electron probe within the specimen. In thin samples, a large semi-convergence angle enables a tightly focused beam and sub-nanometer resolution. However, in thick specimens, resolution is fundamentally limited by transverse beam broadening from multiple large-angle scattering events—for example, a probe with 10 mrad angular divergence can broaden by ∼100 nm over a 10 μm path. Since this broadening scales inversely with beam energy, MeV-STEM offers a promising route for high-resolution imaging in thick materials. To quantitatively assess this effect, we performed high-precision measurements at UCLA’s PEGASUS beamline, characterizing beam divergence and intensity profiles for 3–8 MeV electrons transmitted through a wedged-silicon sample of varying thickness. Our results reconcile discrepancies among analytical models and validate Monte Carlo simulations. Here, we find that increasing beam energy from 3.0 to 5.8 MeV reduces angular broadening by a factor of 2.6, with diminishing returns observed at 7.6 MeV. These findings provide a quantitative framework for optimizing MeV-STEM parameters in high-resolution imaging of thick biological and microelectronic specimens, and for guiding beam energy selection in other advanced imaging modes beyond STEM.

36 MATERIALS SCIENCE↗
NASA NTRSDate not supplied

Vehicle Modeling During the Burning of Thermally Thick Samples in the Saffire V Experiments

In order to design a safer spacecraft in terms of fire prevention, detection and cleanup, the transport of combustion products and heat must be predicted. Large-scale fire data was provided by the Saffire payload within Northrup Grumman’s Cygnus vehicle after a resupply mission to the ISS. Solid materials, including thick thermoplastic samples were ignited to study flame spread and the effect a fire has on a vehicle. Sensors that measured species and temperature were placed within Cygnus. A model using Pyrosim was developed to predict the thick fuel burn events from Saffire V by using sensor data from Cygnus. The heat transfer coefficient between the cabin air and cargo was previously calibrated using the cotton fuel burn event, and provided a good prediction of the temperature response within the vehicle during the two thick fuel experiments. The difference between the Saffire inlet CO 2 sensor, and the forward port standoff CO 2 sensor, which is the closest to the Saffire outlet, was used as an input into the model. This method provided an excellent prediction of the CO 2 response in the other parts of the Cygnus.

fire safety↗
DOE OSTI2023

Relationship between Grain Size and Sample Thickness on the Creep-Rupture Performance of Thin Metallic Sheets of INCONEL Alloy 740H

A study was conducted on INCONEL® alloy 740H® to examine the role of grain size and sheet thickness on the alloy’s creep-rupture behavior. Three different starting sheet thicknesses were utilized and multiple heat-treatment conditions anticipated for compact heat exchanger (CHX) manufacturing were applied to produce a range of grain sizes. Creep-rupture testing was conducted at 750 °C for times up to about 6000 h and the results were compared to wrought databases. The data show that both creep strength and ductility were important factors in the overall creep performance of the sheets. Reductions in performance were observed due either to accelerated creep when grain size was fine or loss of rupture ductility when grain sizes approached the sheet thickness. Some combinations of heat-treatment and thickness were able to produce typical expected wrought creep properties. Historically a ‘rule-of-thumb’ requirement for creep testing suggests 3-5 grains per sample minimum dimension to ensure homogeneous behavior. This research shows that to ensure representative wrought creep performance (i.e. no effect of sample size), the sample minimum cross-section should be 10 times the average ASTM grain size. Statistical analysis of the microstructures suggests the population of larger grains as a controlling feature in creep failure.

14 SOLAR ENERGY↗
DOE OSTI2020

A three-dimensional reconstruction algorithm for scanning transmission electron microscopy data from thick samples

Increasing interest in three-dimensional nanostructures adds impetus to electron microscopy techniques capable of imaging at or below the nanoscale in three dimensions. We present a reconstruction algorithm that takes as input a focal series of four-dimensional scanning transmission electron microscopy (4D-STEM) data and transcends the prevalent structure retrieval algorithm assumption of a very thin specimen homogenous along the optic axis. We demonstrate this approach by reconstructing the different layers of a lead iridate (Pb$_2$Ir$_2$O$_7$) and yttrium-stabilized zirconia (Y$_{0.095}$Zr$_{0.905}$O$_2$) heterostructure from data acquired with the specimen in a single plan-view orientation, with the epitaxial layers stacked along the beam direction.

Brown, Hamish G↗
DOE OSTI2025

Enhanced Monte Carlo Simulations for Electron Energy Loss Mitigation in Real-Space Nanoimaging of Thick Biological Samples and Microchips

High-resolution imaging using Transmission Electron Microscopy (TEM) is essential for applications such as grain boundary analysis, microchip defect characterization, and biological imaging. However, TEM images are often compromised by electron energy spread and other factors. In TEM mode, where the objective and projector lenses are positioned downstream of the sample, electron–sample interactions cause energy loss, which adversely impacts image quality and resolution. This study introduces a simulation tool to estimate the electron energy loss spectrum (EELS) as a function of sample thickness, covering electron beam energies from 300 keV to 3 MeV. Leveraging recent advances in MeV-TEM/STEM technology, which includes a state-of-the-art electron source with 2-picometer emittance, an energy spread of 3 × 10 -5 , and optimized beam characteristics, we aim to minimize energy spread. By integrating EELS capabilities into the BNL Monte Carlo (MC) simulation code for thicker samples, we evaluate electron beam parameters to mitigate energy spread resulting from electron–sample interactions. Based on our simulations, we propose an experimental procedure for quantitively distinguishing between elastic and inelastic scattering. The findings will guide the selection of optimal beam settings, thereby enhancing resolution for nanoimaging of thick biological samples and microchips.

36 MATERIALS SCIENCE↗
DOE OSTI2024

Simulation Study of High-Precision Characterization of MeV Electron Interactions for Advanced Nano-Imaging of Thick Biological Samples and Microchips

The resolution of a mega-electron-volt scanning transmission electron microscope (MeV-STEM) is primarily governed by the properties of the incident electron beam and angular broadening effects that occur within thick biological samples and microchips. A precise understanding and mitigation of these constraints require detailed knowledge of beam emittance, aberrations in the STEM column optics, and energy-dependent elastic and inelastic critical angles of the materials being examined. This simulation study proposes a standardized experimental framework for comprehensively assessing beam intensity, divergence, and size at the sample exit. This framework aims to characterize electron-sample interactions, reconcile discrepancies among analytical models, and validate Monte Carlo (MC) simulations for enhanced predictive accuracy. Our numerical findings demonstrate that precise measurements of these parameters, especially angular broadening, are not only feasible but also essential for optimizing imaging resolution in thick biological samples and microchips. By utilizing an electron source with minimal emittance and tailored beam characteristics, along with amorphous ice and silicon samples as biological proxies and microchip materials, this research seeks to optimize electron beam energy by focusing on parameters to improve the resolution in MeV-STEM/TEM. This optimization is particularly crucial for in situ imaging of thick biological samples and for examining microchip defects with nanometer resolutions. Our ultimate goal is to develop a comprehensive mapping of the minimum electron energy required to achieve a nanoscale resolution, taking into account variations in sample thickness, composition, and imaging mode.

36 MATERIALS SCIENCE↗
DOE OSTI2025

Drying of strawberries with airborne ultrasound and other integrated dehydration mechanisms

This article presents a comprehensive investigation into the drying of strawberries using multiple dehydration methods with an emphasis on energy efficiency and sustainability. Initially, an airborne ultrasonic transducer with a frequency of 21 kHz was employed in batch operations to examine the effects of controlling parameters, including applied power, distance from the transducer plate, sample thickness, and sample holder type. The Energy Ratio, defined as the ratio of thermal energy required to evaporate moisture to ultrasonic energy, was observed to reach up to 2.2, particularly during the initial stages of drying. Subsequently, the Smart Dryer integrated airborne ultrasound (US) dehydration, slot jet reattachment (SJR) nozzle convective drying, infrared (IR) drying, and their combinations, enabling a systematic exploration of various drying conditions on the drying time and quality of strawberries. The integration of airborne US with SJR nozzles and IR drying demonstrates a promising approach for optimizing drying processes. This method not only preserves the quality of dried strawberries but also improves the energy factor to 0.88, reducing drying time by 89% compared with other conditions. Key quality attributes of the dried strawberries, such as color and water activity, were evaluated to understand the influence of each drying method. The findings highlight the potential of these integrated drying techniques as sustainable solutions for efficient and high-quality strawberry dehydration.

42 ENGINEERING↗
DOE OSTI2023

Optimize electron beam energy toward in-situ imaging of large thick bio-samples with nanometer resolution

To optimize electron energy toward in-situ imaging large bio-samples up to 10-μm thickness with nanoscale resolution, we implemented an analytical model based on elastic and inelastic characteristic angles 1. This model can be used to predict the transverse beam size broadening as a function of electron energy while the probe beam traverses through the sample. As result, the optimal choice of the electron beam energy can be realized. While the sample thickness is less than 10 μm, there exists an optimal electron beam energy below 10 MeV regarding a specific sample thickness. However, for samples thicker than 10 μm, the optimal beam energy is 10 MeV, and the ultimate resolution could become worse with the increase of the sample thickness.

43 PARTICLE ACCELERATORS↗
DOE OSTI2022

How to avoid multiple scattering in strongly scattering SANS and USANS samples

Small Angle Neutron Scattering (SANS) and Ultra Small Angle Neutron Scattering (USANS) are the only available experimental techniques to provide seamless non-destructive measurements of the geometry of the accessible and inaccessible pore structure of rocks from sub-nanopore size to the scale of macropores. They have therefore become the measurement of choice for tight reservoir rocks such as organic rich shales. A simplifying assumption in the analysis is, however, that during the path of neutrons through the sample each neutron is only scattered once. Shales are samples with a high scattering power and Multiple Scattering (MS) may occur which requires special modelling for deconvolution of the results. The approach to avoid MS is to simply reduce the sample thickness to <0.15–0.5 mm. Here, in this work, we present a systematic method on wavelength selection and preparation of samples to optimise extraction of microstructural data and minimise parasitic errors. Experimentally measured SAS transmission (TSAS) values are used as a practical criterion for estimation of the extent of MS. Generous beamtime allocations allowed robust testing revealing that sample thicknesses can be twice as thick as predicted using the standard protocol. Analysing thicker samples is particularly beneficial for statistically relevant characterisation of heterogeneous samples making the new protocol the method of choice for such samples.

(U)SANS↗
DOE OSTI2024

Temperature Dependent Early-Stage Oxidation Dynamics of Cu(100) Film with Faceted Holes

Fundamental understanding of surface oxidation dynamics is critical for rational corrosion protection and advanced manufacturing of nanostructured oxides. In situ environmental TEM (ETEM) provides high spatial (nano- to atomic- scale) and temporal (< 0.1 s) resolution to investigate the early-stage oxidation/corrosion dynamics of metals and alloys. Thin samples with facets are widely used to enable cross-sectional observation of the oxidation dynamics in ETEM. However, how different facet orientations oxidize under the same conditions, and how these facets change the oxidation process, has not been investigated before. Here, using in situ ETEM, we systematically compare the oxidation dynamics of Cu(001) thin films, with faceted holes exposing {100} and {110} facets at temperatures ranging from 250–600 °C under 0.03 Pa O 2 . Oxidation preference is observed to change, from Cu(110) facets at lower temperatures to Cu(100) facets at ~ 500 °C. Oxide growth mechanisms change from outward growth on Cu 2 O surfaces at low temperatures, to inward growth on Cu-Cu 2 O interfaces at high temperatures. At high temperatures (500–600 °C), a rod-like Cu 2 O morphology is observed, with side facets of ~ {024} and top facets of {100} on Cu(100). This differs from the square-shaped Cu 2 O exposing {110} facets formed on Cu(001) surfaces. Rod-like oxides exhibit directional growth along their lengths with linear growth rates, regardless of rod length and width. This suggests that O from Cu(001) surfaces, rather than Cu(100) facets, serves as an O source for oxide growth. These results show a direct comparison of oxidation at different orientations with temperature, underscoring the temperature dependence of oxidation preference. Our results also suggest future in situ ETEM experiments viewing oxidation corrosion cross-sectionally should be cautious when oxide size is comparable with sample thickness, as the oxidizing mechanism may change due to sample thickness.

36 MATERIALS SCIENCE↗