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Results for “Sample thickness optimization”

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 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 OSTI2024

Optimize Electron Beam Energy toward In Situ Imaging of Thick Frozen Bio-Samples with Nanometer Resolution Using MeV-STEM

To optimize electron energy for in situ imaging of large biological samples up to 10 μm in thickness with nanoscale resolutions, we implemented an analytical model based on elastic and inelastic characteristic angles. This model has been benchmarked by Monte Carlo simulations and 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 a result, the optimal choice of the electron beam energy can be realized. In addition, the impact of the dose-limited resolution was analysed. 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 or higher depending on the sample thickness, and the ultimate resolution could become worse with the increase in the sample thickness. Moreover, a MeV-STEM column based on a two-stage lens system can be applied to reduce the beam size from one micron at aperture to one nanometre at the sample with the energy tuning range from 3 to 10 MeV. In conjunction with the state-of-the-art ultralow emittance electron source that we recently implemented, the maximum size of an electron beam when it traverses through an up to 10 μm thick bio-sample can be kept less than 10 nm . This is a critical step toward the in situ imaging of large, thick biological samples with nanometer resolution.

36 MATERIALS SCIENCE↗
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

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

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 OSTI2025

Microstructural evaluation of thin-wall sections of 316L stainless steel produced by laser powder-bed fusion processing

The synthesis of thin wall sections that are only 0.4 mm thick is achieved with LPBF AM. Sample preparation is optimized using metallographic polishing to produce samples with only 0.3 um rms roughness for scanning electron microanalysis with EBSD and EDS. A fully austenitic 316L phase is found without evidence of secondary phases. Unlike some AM products that can readily evidence composition segregation due to solute rejection as attributable to temperature gradients within the solidification

Jankowski, Alan F. [Sandia National Laboratories (↗
DOE OSTI2023

Optically Active Spin Defects in Few-Layer Thick Hexagonal Boron Nitride

Optically active spin defects in hexagonal boron nitride (hBN) are promising quantum systems for the design of two-dimensional quantum sensing units offering optimal proximity to the sample being probed. In this Letter, we first demonstrate that the electron spin resonance frequencies of boron vacancy centers ($V$$^{–}_{B}$) can be detected optically in the limit of few-atomic-layer thick hBN flakes despite the nanoscale proximity of the crystal surface that often leads to a degradation of the stability of solid-state spin defects. We then analyze the variations of the electronic spin properties of $V$$^{–}_{B}$ centers with the hBN thickness with a focus on (i) the zero-field splitting parameters, (ii) the optically induced spin polarization rate and (iii) the longitudinal spin relaxation time. Furthermore, this Letter provides important insights into the properties of $V$$^{–}_{B}$ centers embedded in ultrathin hBN flakes, which are valuable for future developments of foil-based quantum sensing technologies.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗
DOE OSTI2025

Site-specific plan-view (S)TEM sample preparation from thin films using a dual-beam FIB-SEM

To fully evaluate the atomic structure, and associated properties of materials using transmission electron microscopy, examination of samples from three non-collinear orientations is needed. This is particularly challenging for thin films and nanoscale devices built on substrates due to limitations with plan-view sample preparation. In this work, a new method for preparation of high-quality, site-specific, plan-view TEM samples from thin-films grown on substrates, is presented and discussed. Here, it is based on using a dual-beam focused ion beam scanning electron microscope (FIB-SEM) system. To demonstrate the method, the samples were prepared from thin films of perovskite oxide BaSnO 3 grown on a SrTiO 3 substrate and metal oxide IrO 2 on a TiO 2 substrate, ranging from 20–80 nm in thicknesses using molecular beam epitaxy. While the method is optimized for the thin films, it can be extended to other site-specific plan-view samples and devices build on wafers. Aberration-corrected STEM was used to evaluate the quality of the samples and their applicability for atomic-resolution imaging and analysis.

BaSnO3↗
DOE OSTI2024

Viability of Miniature Discs in LFA-427

Miniature disc samples pose challenging measuring conditions for laser flash analysis. With reductions in signal from lower radiosity and lower half-rise times from low thicknesses, optimal selections of coatings and laser parameters are critical in a successful measurement. This report explains the methodology in successfully measuring two different material types—metals and ceramics—in proper coating selection, laser parameters, and post analysis for each material, as well as applying it to un-irradiated uranium samples of each type (U-metal, UO 2 ). This was done through a combination of analysis techniques combining automatic commercial methods (Neztech) and manual methods for correcting laser pulse impact aberrations.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
DOE OSTI2024

Cold Spray Technology Applications for SRF Cavity Thermal and Mechanical Stabilization

The overall objective of the project is the development of a method allowing increased thermal and mechanical stabilization of SRF cavities by depositing a thick layer on the outer surface by cold-spray. Coating and testing of bi-metallic Nb/Cu and Nb/CuW samples were carried out to optimize the process parameters. The process developed on samples was applied to a single cell SRF cavity for proof-of-principle demonstration of improved thermal and mechanical stability.

36 MATERIALS SCIENCE↗
DOE OSTI2026

Optimizing aluminum oxide passivation layers—Laser-induced plasmas for layer formation, real-time diagnostics, and layer evaluation

Molten salts have beneficial thermophysical and electrolytic properties, but the aggressive nature of molten salts requires corrosion mitigation strategies, such as structural material surface treatment. In this study, a laser-induced breakdown spectroscopy (LIBS) system was used to simultaneously ablate and monitor de-excitation spectra to form and identify dense alumina passivation layers. Additionally, high-frequency (kHz) LIBS imaging allowed rapid elemental mapping and depth profiling for surface O/Al ratios via minimally destructive analysis. The paired t-test rejected the null hypothesis that air and Ar cover gases were equivalent (p = 0.00012), and the analysis of variance (ANOVA) showed that overlap between shots (p = 0.03112) and cover gas flow rate (p = 0.02729) were statistically significant. At 75% overlap, the O/Al ratio increased to 10% ± 2%, and 90% overlap rose further to 31% ± 2%. Regardless of overlap, tuning the gas flow from 0.5 to 2.5 L min −1 enhanced the O/Al ratio by 24% ± 4%. LIBS depth profiling showed a 3× increase in layer thickness from 75% to 90% overlap. Molecular band peaks of AlO, a precursor to Al 2 O 3 found during treatment, suggest that band intensity could be used for real-time Al 2 O 3 optimization. Ultimately, by adjusting laser spot overlap and cover gas flow rate, a 266 nm laser was shown to form Al 2 O 3 layers on an Al6061 sample, with cover gas flow rate primarily affecting the O/Al ratio and layer thickness correlating with laser spot overlap. This combination of molecular spectra collection, imaging, and depth profiling demonstrated the robust layer analysis capabilities of LIBS.

Corrosion↗
DOE OSTI2024

Characterization and Optimization of Skipper CCDs for the SOAR Integral Field Spectrograph

We present results from the characterization and optimization of Skipper charge-coupled devices (CCDs) for use in a focal plane prototype for the Southern Astrophysical Research Integral Field Spectrograph (SIFS). We tested eight Skipper CCDs and selected six for SIFS based on performance results. The Skipper CCDs are 6k × 1k, 15 μm pixels, thick, fully depleted, p-channel devices that have been thinned to ~250 μm, backside processed, and treated with an anti-reflective coating. We demonstrate a single-sample readout noise of <4.3 e - rms pixel -1 in all amplifiers. We optimize the readout sequence timing to achieve a readout noise of 0.5 e - rms pixel -1 after 74 non-destructive measurements, which can be accomplished in a region covering 5% of the detector area in a readout time of <4 minutes. We demonstrate single-photon-counting in all 24 amplifiers (four amplifiers per detector) with a readnoise of σ N ~ 0.18 e - rms pixel -1 after N samp = 400 samples, and we constrain the degree of nonlinearity to be ≲1% at low signal levels (0 e - to 50 e - ). Clock-induced charge (CIC) remains an important issue when the Skipper CCD is configured to provide a large full-well capacity. We achieve a CIC rate of <1.45 × 10 -3 e - pixel -1 frame -1 for a full-well capacity of ~900 e - , which increases to a CIC rate of ~3 e - pixel -1 frame -1 for full-well capacities ~40,000-65,000 e - . We also perform conventional CCD characterization measurements such as charge transfer inefficiency (3.44 × 10 -7 on average), dark current (~2 × 10 -4 e - pixel -1 s -1 ), photon transfer curves, cosmetic defects (<0.45% “bad” pixels), and charge diffusion (point-spread function < 7.5 μm) to verify that these properties are consistent with expectations from conventional p-channel CCDs used for astronomy. Furthermore, we provide the first measurements of the brighter-fatter effect and absolute quantum efficiency (≳80% between 450 and 980 nm; ≳90% between 600 and 900 nm) using Skipper CCDs.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗
DOE OSTI2022

Ultra-rapid, physics-based development pathway for reactor-relevant RF antenna materials

This paper presents a rapid, atomistically-informed, experimental development pathway for fusion reactor-relevant radio frequency (RF) antenna materials in the Cu-Cr-(Nb,Al,Zr) composition system, with the goal of improving upon GRCop-84. RF antennas in a tokamak fusion reactor will face a unique set of challenges as both structural and functional materials. The desired material must simultaneously achieve and maintain high electrical conductivity, high strength, high thermal conductivity, resist high temperatures, possess low nuclear activation, and incur low damage due to neutron bombardment. The GRCop-84 alloy serves as a starting point for iterative improvement, with the desire to reduce or eliminate Nb from the material to minimize nuclear activation. The rapid development pathway makes use of a multi-target combinatorial thick film sputtering process to produce full ternary phase diagrams on a Si wafer substrate. Transient grating spectroscopy (TGS), a laser-ultrasonic method, will determine spatially-varying thermo-elastic properties, while four terminal electrical conductivity measurements will map out the best per- forming regions of the sample for in-depth study at larger length scales. High energy proton and self-ion irradiation emulates the effects of neutron damage on the thermal/electric properties. With rapid turnaround time (∼days) in terms of mapping radiation damage-induced material property changes in the full ternary system, these techniques allow rapid iteration towards an optimal material, testing hundreds of nearby compositions in the time it took to test one. Focused testing of larger, single composition samples (produced in an arc furnace or by laser sintering) provides data on structural and high power RF properties, and validates our thick-film based workflow.

70 PLASMA PHYSICS AND FUSION TECHNOLOGY↗
DOE OSTI2022

Structured illumination with thermal imaging (SI-TI): A dynamically reconfigurable metrology for parallelized thermal transport characterization

The recent push for the “materials by design” paradigm requires synergistic integration of scalable computation, synthesis, and characterization. Among these, techniques for efficient measurement of thermal transport can be a bottleneck limiting the experimental database size, especially for diverse materials with a range of roughness, porosity, and anisotropy. Traditional contact thermal measurements have challenges with throughput and the lack of spatially resolvable property mapping, while non-contact pump-probe laser methods generally need mirror smooth sample surfaces and also require serial raster scanning to achieve property mapping. Here, we present structured illumination with thermal imaging (SI-TI), a new thermal characterization tool based on parallelized all-optical heating and thermometry. Experiments on representative dense and porous bulk materials as well as a 3D printed thermoelectric thick film (~50 μm) demonstrate that SI-TI (1) enables paralleled measurement of multiple regions and samples without raster scanning; (2) can dynamically adjust the heating pattern purely in software, to optimize the measurement sensitivity in different directions for anisotropic materials; and (3) can tolerate rough (~3 μm) and scratched sample surfaces. Here, this work highlights a new avenue in adaptivity and throughput for thermal characterization of diverse materials.

42 ENGINEERING↗
DOE OSTI2023

First Results From Nb3Sn Coatings of 2.6 GHz Nb SRF Cavities Using DC Cylindrical Magnetron Sputtering System

A DC cylindrical magnetron sputtering system has been commissioned and operated to deposit Nb3Sn onto 2.6 GHz Nb SRF cavities. After optimizing the deposition conditions in a mock-up cavity, Nb-Sn films are deposited first on flat samples by multilayer sequential sputtering of Nb and Sn, and later annealed at 950 °C for 3 hours. X-ray diffraction of the films showed multiple peaks for the Nb3Sn phase and Nb (substrate). No peaks from any Nb- Sn compound other than Nb3Sn were detected. Later three 2.6 GHz Nb SRF cavities are coated with ~1 μm thick Nb3Sn. The first Nb3Sn coated cavity reached close to Eacc = 8 MV/m, demonstrating a quality factor Q0 of 3.2 × 108 at Tbath = 4.4 K and Eacc = 5 MV/m, about a factor of three higher than that of Nb at this temperature. Q0 was close to 1.1 × 109, dominated by the residual resistance, at 2 K and Eacc = 5 MV/m. The Nb3Sn coated cavities demonstrated Tc in the range of 17.9 – 18 K. Here we present the commissioning experience, s ystem optimization, and the first results from the Nb3Sn fabrication on flat samples and SRF cavities.

72 PHYSICS OF ELEMENTARY PARTICLES AND FIELDS↗
DOE OSTI2023

FIRST RESULTS FROM Nb3Sn COATINGS OF 2.6 GHz Nb SRF CAVITIES USING DC CYLINDRICAL MAGNETRON SPUTTERING SYSTEM

A DC cylindrical magnetron sputtering system has been commissioned and operated to deposit Nb3Sn onto 2.6 GHz Nb SRF cavities. After optimizing the deposition conditions in a mock-up cavity, Nb-Sn films are deposited first on flat samples by multilayer sequential sputtering of Nb and Sn, and later annealed at 950 °C for 3 hours. X-ray diffraction of the films showed multiple peaks for the Nb3Sn phase and Nb (substrate). No peaks from any Nb-Sn compound other than Nb3Sn were detected. Later three 2.6 GHz Nb SRF cavities are coated with ~1 µm thick Nb3Sn. The first Nb3Sn coated cavity reached close to Eacc = 8 MV/m, demonstrating a quality factor Q0 of 3.2 × 108 at Tbath = 4.4 K and Eacc = 5 MV/m, about a factor of three higher than that of Nb at this temperature. Q0 was close to 1.1 × 109, dominated by the residual resistance, at 2 K and Eacc = 5 MV/m. The Nb3Sn coated cavities demonstrated Tc in the range of 17.9 ? 18 K. Here, we present the commissioning experience, system optimization, and the first results from the Nb3Sn fabrication on flat samples and SRF cavities.

Shakel, M.S.↗
DOE OSTI2023

FIRST RESULTS FROM Nb3Sn COATINGS OF 2.6 GHz Nb SRF CAVITIES USING DC CYLINDRICAL MAGNETRON SPUTTERING SYSTEM

A DC cylindrical magnetron sputtering system has been commissioned and operated to deposit Nb3Sn onto 2.6 GHz Nb SRF cavities. After optimizing the deposition conditions in a mock-up cavity, Nb-Sn films are deposited first on flat samples by multilayer sequential sputtering of Nb and Sn, and later annealed at 950 °C for 3 hours. X-ray diffraction of the films showed multiple peaks for the Nb3Sn phase and Nb (substrate). No peaks from any Nb-Sn compound other than Nb3Sn were detected. Later three 2.6 GHz Nb SRF cavities are coated with ~1 µm thick Nb3Sn. The first Nb3Sn coated cavity reached close to Eacc = 8 MV/m, demonstrating a quality factor Q0 of 3.2 × 108 at Tbath = 4.4 K and Eacc = 5 MV/m, about a factor of three higher than that of Nb at this temperature. Q0 was close to 1.1 × 109, dominated by the residual resistance, at 2 K and Eacc = 5 MV/m. The Nb3Sn coated cavities demonstrated Tc in the range of 17.9 ? 18 K. Here, we present the commissioning experience, system optimization, and the first results from the Nb3Sn fabrication on flat samples and SRF cavities.

Shakel, M. S.↗
DOE OSTI2023

First Results From Nb3Sn Coatings of 2.6 GHz Nb SRF Cavities Using DC Cylindrical Magnetron Sputtering System

A DC cylindrical magnetron sputtering system has been commissioned and operated to deposit Nb3Sn onto 2.6 GHz Nb SRF cavities. After optimizing the deposition conditions in a mock-up cavity, Nb-Sn films are deposited first on flat samples by multilayer sequential sputtering of Nb and Sn, and later annealed at 950°C for 3 hours. X-ray diffraction of the films showed multiple peaks for the Nb3Sn phase and Nb (substrate). No peaks from any Nb- Sn compound other than Nb3Sn were detected. Later three 2.6 GHz Nb SRF cavities are coated with ~1 μm thick Nb3Sn. The first Nb3Sn coated cavity reached close to Eacc = 8 MV/m, demonstrating a quality factor Q0 of $3.2 \times 108$ at Tbath = 4.4 K and Eacc = 5 MV/m, about a factor of three higher than that of Nb at this temperature. Q0 was close to $1.1 \times 109$, dominated by the residual resistance, at 2 K and Eacc = 5 MV/m. The Nb3Sn coated cavities demonstrated Tc in the range of $17.9 -- 18$ K. Here we present the commissioning experience, system optimization, and the first results from the Nb3Sn fabrication on flat samples and SRF cavities.

72 PHYSICS OF ELEMENTARY PARTICLES AND FIELDS↗