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DOE OSTI2020

A coded aperture microscope for X-ray fluorescence full-field imaging

The design and construction of an instrument for full-field imaging of the X-ray fluorescence emitted by a fully illuminated sample are presented. The aim is to produce an X-ray microscope with a few micrometers spatial resolution, which does not need to scan the sample. Since the fluorescence from a spatially inhomogeneous sample may contain many fluorescence lines, the optic which will provide the magnification of the emissions must be achromatic, i.e. its optical properties must be energy-independent. The only optics which fulfill this requirement in the X-ray regime are mirrors and pinholes. The throughput of a simple pinhole is very low, so the concept of coded apertures is an attractive extension which improves the throughput by having many pinholes, and retains the achromatic property. Modified uniformly redundant arrays (MURAs) with 10 µm openings and 50% open area have been fabricated using gold in a lithographic technique, fabricated on a 1 µm-thick silicon nitride membrane. The gold is 25 µm thick, offering good contrast up to 20 keV. The silicon nitride is transparent down into the soft X-ray region. MURAs with various orders, from 19 up to 73, as well as their respective negative (a mask where open and closed positions are inversed compared with the original mask), have been made. Having both signs of mask will reduce near-field artifacts and make it possible to correct for any lack of contrast.

36 MATERIALS SCIENCE↗

DOE OSTI2020

Modeling synergistic fuel cell membrane degradation with mitigating effects of cerium

During operation, polymer-electrolyte fuel cells undergo mechanical and chemical degradation, which behave synergistically and lead to accelerated membrane deterioration over time. This study builds upon previous modeling work on mechanical degradation, as described by a pinhole in the membrane, and chemical degradation mitigation by using cerium. By combining these two models, analysis can be carried out on the coupled degradation methods and how the mitigation effects of cerium disrupt the degradation cycle. The model results show how the presence of a pinhole in the membrane changes the distribution of cerium in the cell and modifies chemical degradation rates. In addition, the model shows how cerium affects the rate of pinhole growth by slowing down the rate of change in mechanical properties due to chemical degradation. Finally, the model shows how cerium modifies the mechanical and chemical degradation rates of the membrane under humidity- and voltage-cycling conditions.

Ehlinger, VM↗

DOE OSTI2020

Modeling Synergistic Fuel Cell Membrane Degradation with Mitigating Effects of Cerium

During operation, polymer-electrolyte-membrane (PEM) fuel cells undergo mechanical and chemical degradation mechanisms, which behave synergistically and lead to accelerated membrane degradation over time. This study builds upon previous modeling work on mechanical degradation as described by a pinhole in the membrane and the effects of cerium on chemical degradation.1 By combining these two models, analysis can be carried out on the coupled degradation methods and how the mitigation effects of cerium disrupt the degradation cycle. The mechanical model represents a pinhole in the membrane using an effective void fraction, which allows for increased gas crossover through the membrane and impacts the membrane transport and mechanical properties. A microkinetic model for the chemical degradation is included in the model, including attack of the membrane polymer by hydroxyl radicals as well as the mitigation reaction for quenching of hydroxyl radicals with cerium. A concentrated solution theory approach is used to model the transport of cerium ions throughout the cell.2 The model results show how the location of cerium in the cell can be used to prevent chemical degradation. In addition, the model shows how cerium slows down the rate of pinhole growth by reducing the gas crossover and membrane thinning rate. Finally, the model can be used to optimize the distribution of cerium in the membrane and catalyst layers by balancing trade-offs between lowering degradation rates and decreasing fuel cell performance.

25 ENERGY STORAGE↗

DOE OSTI2024

Validation Study of Experimental Insulating and Air-Sealing Technology for Enclosed Roof Cavities

Validation Study of Experimental Insulating and Air-Sealing Technology for Enclosed Roof Cavities, explores a new minimally invasive system known as Pinhole Insulation ® for retroft insulation of cathedral ceilings, flat roofs, dormer roofs, and other enclosed roof cavities. It also explores the validation of the associated equipment, software, and materials used in this application. The Pinhole Insulation process essentially consists of drilling a ¼” hole in the ceiling surface and then injecting closed cell polyurethane foam such that the foam is deposited on the interior surface of the exterior roof sheathing. In a typical cathedral ceiling with R19 batts, the R value will be improved by at least 60% and the cavity will become completely air sealed. The system is quick, minimally invasive and at least an order of magnitude less expensive than alternatives such as removing the ceiling surface and spraying closed cell foam.

32 ENERGY CONSERVATION, CONSUMPTION, AND UTILIZATI↗

DOE OSTI2020

Design of a neutron microscope based on Wolter mirrors

The predominant geometry for a neutron imaging experiment is that of a pinhole camera. Here, this is primarily due to the difficulty in focusing neutrons due to the weak refractive index, which is also strongly chromatic. Proof of concept experiments demonstrated that neutron image forming lenses based on reflective Wolter mirrors can produce quantitative, high spatial resolution neutron images while also increasing the time resolution compared to the conventional pinhole camera geometry. Motivated by these results, we report the design of a neutron microscope where two Wolter mirrors replace condensing and objective lenses, in direct analogy with typical visible light microscopes. Ray tracing results indicate that this system will yield 3 µm spatial resolution images with an acquisition time of order <1 s (10 4 faster than currently possible at this spatial resolution) with a field of view of about 5 mm in diameter.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗

DOE OSTI2024

Solution-processed tungsten diselenide as an inorganic hole transport material for moisture-stable perovskite solar cells in the n-i-p architecture

Some of the obstacles to the commercialization of perovskite solar cells (PSCs) are their long-term moisture stability and material cost of the constituent layers, such as the commonly used spiro-OMeTAD hole transport layer (HTL). Replacing the spiro-OMeTAD with low-cost inorganic hole transport materials (HTMs) are important to further elevate the attractiveness of PSCs for commercialization. Perovskite-compatible, solution-exfoliated two-dimensional (2D) transition metal dichalcogenides (TMDCs) are being considered as viable candidates for inorganic HTMs. We consider one such TMDC, WSe 2 which was chemically exfoliated using dichlorobenzene (DCB), a perovskite-compatible solvent, as it was integrated with triple cation perovskite absorbers within the solar cell stack. Here, the WSe 2 HTL required heat treatment processes to be maintained below 100°C in order to preserve the integrity of the underlying perovskite; despite this lower temperature post treatment process, the structural morphology of the film revealed its dense and pinhole-free nature. Temperature-dependent transport studies conducted on the WSe 2 film provided evidence of its semiconducting character and its ability to extract holes well from the underlying triple-cation Cs 0.05 FA 0.79 MA 0.16 PbI 2.45 Br 0.55 absorber. The inorganic HTL offered better environmental stability in moisture-rich environments of up to 60% relative humidity, in comparison to spiro-OMeTAD HTL-based devices which degraded faster as a result of pinholes

14 SOLAR ENERGY↗

DOE OSTI2024

Experimental and modeling study of the effect of confinement on the thermal decomposition of organic materials

Simultaneous Thermal Analysis is widely used to study thermal decomposition of a variety of organic materials, and the choice of experimental conditions is very important to obtain reliable mass loss and heat flow curves. Here in this work we investigate the effect of confinement on the thermal decomposition of organic materials. As an example, we explore high-density polyethylene (HDPE) and one of its pyrolysis products, namely eicosane (C 20 H 42 ), through experiments and modeling in open crucibles and crucibles closed with a pierced lid. A new model is developed for evaporation and sublimation from open and pinhole thermal-analysis pans. It considers the kinetic resistance of evaporation at the liquid-vapor interface, inhibition of evaporation by buildup of vapor inside the pan, thermal expansion of vapor inside the pan, and diffusion of vapor from the pan. The model is validated using simultaneous heat-flow and mass-loss measurements of n-eicosane evaporation for various pinhole sizes, down to 50 µm. The importance of product evaporation inhibition for measuring polymer decomposition was demonstrated using HDPE. This study sheds light on the effect of confinement on the mass loss rate of organic materials.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2022

Elucidating Diiodomethane-Induced Improvement in Photonically Cured MAPbI 3 Solar Cells

Diiodomethane (CH 2 I 2 ) has been reported to improve the photonically cured perovskite solar cell (PSC) device performance by reducing pinholes. Here we show that even for pinhole-free methylammonium lead iodide (MAPbI 3 ) made by photonic curing, adding CH 2 I 2 promotes significant performance improvement. We elucidate the mechanisms behind the observed improvement. In addition to current-density versus voltage measurements, we perform a wide variety of characterization to compare the crystallinity, grain structure, optical, chemical, and electrical properties of the photonically cured samples with and without CH 2 I 2 in the MAPbI 3 layer to those of thermally annealed devices. Here, the addition of CH 2 I 2 promotes grain growth in the vertical direction, increases the I/Pb ratio in the final film, and removes the I - ionic diffusion and defect signature associated with iodine interstitials. As a result, we achieve a champion efficiency of 15.04% with MAPbI 3 conversion time of 20 ms, comparable to PSCs that have MAPbI 3 layer thermally annealed for 10 min. Understanding the mechanisms behind additive-induced improvements for non-thermal annealing processes is critical to enabling high-speed PSC manufacturing.

14 SOLAR ENERGY↗

DOE OSTI2020

Enhanced stability of silicon for photoelectrochemical water oxidation through self-healing enabled by an alkaline protective electrolyte

Alkaline electrolytes impede the corrosion of Si photoanodes under positive potentials and/or illumination, due to the formation of a SiO x layer that etches 2–3 orders of magnitude more slowly than Si. Hence during water oxidation under illumination, pinholes in protection layers on Si photoanodes result in the local formation of a protective, stabilizing passive oxide on the Si surface. However, operation under natural diurnal insolation cycles additionally requires protection strategies that minimize the dark corrosive etching rate of Si at pinholes. We show herein that addition of [Fe(CN) 6 ] 3- to 1.0 M KOH(aq) results in a self-healing process that extends the lifetime to >280 h of an np + -Si(100) photoanode patterned with an array of Ni catalyst islands operated under simulated day/night cycles. The self-healing [Fe(CN) 6 ] 3- additive caused the exposed Si(100) surface to etch >180 times slower than the Si etch rate in 1.0 M KOH(aq) alone. No appreciable difference in etch rate or facet preference was observed between Si(100) and Si(111) surfaces in 1.0 M KOH(aq) with [Fe(CN) 6 ] 3- , indicating that the surface conformally oxidized before Si dissolved. The presence of [Fe(CN) 6 ] 3- minimally impacted the faradaic efficiency or overpotential of p + -Si/Ni electrodes for the oxygen-evolution reaction.

25 ENERGY STORAGE↗

DOE OSTI2021

A 1D Lyman-alpha profile camera for plasma edge neutral studies on the DIII-D tokamak

A one dimensional, absolutely calibrated pinhole camera system was installed on the DIII-D tokamak to measure edge Lyman-alpha (Ly-α) emission from hydrogen isotopes, which can be used to infer neutral density and ionization rate profiles. The system is composed of two cameras, each providing a toroidal fan of 20 lines of sight, viewing the plasma edge on the inboard and outboard side of DIII-D. The cameras’ views lie in a horizontal plane 77 cm below the midplane. At its tangency radius, each channel provides a radial resolution of ~2 cm full width at half maximum (FWHM) with a total coverage of 22 cm. Each camera consists of a rectangular pinhole, Ly-α reflective mirror, narrow-band Ly-α transmission filter, and a 20 channel AXUV photodetector. The combined mirror and transmission filter have a FWHM of 5 nm, centered near the Ly-α wavelength of 121.6nm and is capable of rejecting significant, parasitic carbon-III (C-III) emission from intrinsic plasma impurities. To provide a high spatial resolution measurement in a compact footprint, the camera utilizes advanced engineering and manufacturing techniques including 3D printing, high stability mirror mounts, and a novel alignment procedure. Absolutely calibrated, spatially resolved Ly-α brightness measurements utilize a bright, isolated line with low parasitic surface reflections and enable quantitative comparison to modeling to study divertor neutral leakage, main chamber fueling, and radial particle transport.

Ionization Rate↗

DOE OSTI2022

Bootstrap estimation of the effect of instrument response function uncertainty on the reconstruction of fusion neutron sources

Neutron imagers are important diagnostics for the inertial confinement fusion implosions at the National Ignition Facility. They provide two- and three-dimensional reconstructions of the neutron source shape that are key indicators of the overall performance. To interpret the shape results properly, it is critical to estimate the uncertainty in those reconstructions. There are two main sources of uncertainties: limited neutron statistics, leading to random errors in the reconstructed images, and incomplete knowledge of the instrument response function (the pinhole-dependent point spread function). While the statistical errors dominate the uncertainty for lower yield deuterium-tritium (DT) shots, errors due to the instrument response function dominate the uncertainty for DT yields on the order of 10 16 neutrons or higher. In this work, a bootstrapping method estimates the uncertainty in a reconstructed image due to the incomplete knowledge of the instrument response function. The main reconstruction is created from the fixed collection of pinhole images that are best aligned with the neutron source. Additional reconstructions are then built using subsets of that collection of images. Variations in the shapes of these additional reconstructions originate solely from uncertainties in the instrument response function, allowing us to use them to provide an additional systematic uncertainty estimate.

47 OTHER INSTRUMENTATION↗

DOE OSTI2022

Crystal response measurement of the x-ray transmission crystals used by the Imaging Spectroscopy Snout at the National Ignition Facility

The Imaging Spectroscopy Snout (ISS) used at the National Ignition Facility is able to simultaneously collect neutron pinhole images, 1D spatially resolved x-ray spectra, and time resolved x-ray pinhole images. To measure the x-ray spectra, the ISS can be equipped with up to four different transmission crystals, each offering different energy ranges from ∼7.5 to ∼12 keV and different resolutions. Characterizing and calibrating such instruments is of paramount importance in order to extract meaningful results from experiments. More specifically, we characterized different ISS transmission-type alpha-Quartz crystals by measuring their responses as a function of photon energy, from which we inferred the angle-integrated reflectivity for each crystal’s working reflections. These measurements were made at the Lawrence Livermore National Laboratory calibration station dedicated to the characterization of x-ray spectrometers. The sources used covered a wide x-ray range—from a few to 30 keV; the source diameter was ∼0.6 mm. The experimental results are discussed alongside theoretical calculations using the pyTTE model.

Dozieres, M. (ORCID:0000000286401459)↗

DOE OSTI2023

Imaging suprathermal x-rays from a laboratory plasma jet using PIN-diode-based and scintillator-based 1D pinhole/coded aperture cameras

A PIN-diode-based 1D x-ray camera and a scintillator-based 1D x-ray camera, both with a microsecond to submicrosecond time resolution, have been developed to perform time-resolved imaging of transient, low-intensity, suprathermal x-rays associated with magnetohydrodynamic instabilities disrupting a plasma jet. These cameras have a high detection efficiency over a broad x-ray band, a wide field of view, and the capability to produce >50 time-resolved frames with a ≤1 μs time resolution. The x-ray images are formed by a pinhole or by a coded aperture placed outside a vacuum chamber in which the plasma jet is launched. The 1D imaging shows that the location of the x-ray source is either a few centimeters away from an inner disk electrode or near a spatially translatable metal frame that is 30–40 cm away from the electrode. Compared to a pinhole, a coded aperture increases the signal collection efficiency but also introduces unwanted artifacts.

Instruments & Instrumentation↗

DOE OSTI2024

Source shape estimation for neutron imaging systems using convolutional neural networks

Neutron imaging systems are important diagnostic tools for characterizing the physics of inertial confinement fusion reactions at the National Ignition Facility (NIF). In particular, neutron images give diagnostic information on the size, symmetry, and shape of the fusion hot spot and surrounding cold fuel. Images are formed via collection of neutron flux from the source using a system of aperture arrays and scintillator-based detectors. Currently, reconstruction of fusion source geometry from the collected neutron images is accomplished by solving a computationally intensive maximum likelihood estimation problem via expectation maximization. In contrast, it is often useful to have simple representations of the overall source geometry that can be computed quickly. In this work, we develop convolutional neural networks (CNNs) to reconstruct the outer contours of simple source geometries. We compare the performance of the CNN for penumbral and pinhole data and provide experimental demonstrations of our methods on both non-noisy and noisy data.

Machine learning, neutron imaging, source reconstr↗

DOE OSTI2026

Development of a broadband hard x-ray radiography platform for pulsed-power experiments

In this article, we develop and demonstrate a broadband hard x-ray radiography platform at the Zebra Pulsed Power Laboratory that integrates point-projection radiography, bremsstrahlung measurements, and hard x-ray pinhole imaging, designed to diagnose current-driven, cylindrically compressed matter. Initial laser-pulsed-power coupled experiments revealed that intense background radiation generated during 1 MA Zebra current shots overwhelmed laser-produced hard x-rays, obscuring radiographic images. Using combined spectral and spatial diagnostics, we identify energetic electrons accelerated by return currents as the dominant source of background hard x-rays, with electron energies inferred to be 3–4 MeV based on Monte Carlo simulations, and demonstrate mitigation through modifications to the radiation shielding and return-current configuration. The diagnostic platform was validated using a wire-pinch hard x-ray source, allowing radiographs of static 1-mm-diameter aluminum wires to be obtained while simultaneously measuring x-ray source spectra and spatial emission distributions within a single shot. Measured wire transmission profiles were quantitatively reconstructed using radiation transport simulations that incorporate an experimentally inferred two-temperature exponential x-ray spectrum from bremsstrahlung signal analysis and spatially distributed emission sources identified by pinhole imaging. Agreement between measured and simulated transmission profiles demonstrates the validity of the radiographic and x-ray source characterization approach, establishing this diagnostic platform as a promising tool for diagnosing magnetically driven, high-density plasmas relevant to warm dense matter and inertial fusion energy research.

70 PLASMA PHYSICS AND FUSION TECHNOLOGY↗

DOE OSTI2025

How transparent is graphene? A surface science perspective on remote epitaxy

Remote epitaxy is the synthesis of a single crystalline film on a graphene-covered substrate, where the film adopts epitaxial registry to the substrate as if the graphene is transparent. Despite many exciting applications for flexible electronics, strain engineering, and heterogeneous integration, an understanding of the fundamental synthesis mechanisms remains elusive. Here we offer a perspective on the synthesis mechanisms, focusing on the foundational assumption of graphene transparency. We identify challenges for quantifying the strength of the remote substrate potential that permeates through graphene, and propose Fourier and beating analysis as a bias-free method for decomposing the lattice potential contributions from the substrate, from graphene, and from surface reconstructions, each at different frequencies. We highlight the importance of graphene-induced reconstructions on epitaxial templating, drawing comparison to moiré epitaxy. We highlight the role of the remote potential in tuning surface diffusion and adatom kinetics on graphene, which are crucial for navigating the competition between remote epitaxy and defect-seeded mechanisms like pinhole epitaxy. In light of this weak remote potential, we re-evaluate the current state-of-the-art experimental evidence, highlighting why it remains challenging to experimentally validate a ‘remote’ epitaxy mechanism that cannot be explained by alternatives, such as pinhole-seeded epitaxy or serial van der Waals epitaxy. We end with one experimental example that, to out knowledge, cannot be explained by competing mechanisms: a different long-range epitaxial relationship for GdPtSb films grown on graphene/sapphire, compared to direct epitaxy on sapphire. We suggest for future experiments that directly measure the remote potential and impact of tuneable growth kinetics.

epitaxy↗

DOE OSTI2020

Source size measurement options for low-emittance light sources

Radiation-based techniques for measuring electron source sizes are widely used as emittance diagnostics at existing synchrotron sources. Three of these techniques, namely, pinhole imaging, double-slit interferometry, and a K-edge filter-based beam position and size monitor system (ps-BPM), are evaluated for measuring source sizes at low-emittance storage rings. Each technique is reviewed with a detailed system description, design optimization, and practical considerations targeted for small source sizes. Pinhole imaging has the simplest setup and gives the beam profile in both transverse dimensions but with limited resolution. Double-slit interferometry has the highest resolution but with a limited detectable size range. The ps-BPM system shows reasonable resolution for monitoring small source sizes and divergence and can give real-time information of the source position and angle. New facilities may consider an integrated system that combines some or all of these techniques.

43 PARTICLE ACCELERATORS↗

DOE OSTI2021

Fabrication of Poly-Si on Locally Etched SiOx as Passivating Contacts for c-Si Solar Cells

Polysilicon on silicon oxide (poly-Si/SiO x ) passivating contacts with predominant charge-carrier transport via pinholes were prepared with room temperature metal-assisted chemical etching. Pinhole areal densities in the range of 2.8 x 10^4 to 4.5 x 10^7 cm^-2 were imaged by SEM. Contact resistivity of 32 m-ohm-cm^2 and implied open circuit voltage of 729 mV were obtained for symmetric n+ poly-Si/SiOx grown onto randomly textured n-Cz. We also show preliminary data pertaining boron-doped polysilicon on nitride/oxide passivating contacts, with which we achieved implied open circuit voltage above 730 mV and recombination current of 0.2 fA/cm^2.

amorphous Si↗