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DOE OSTI2026

Fast and bright scintillators for ultrafast materials dynamics using 4th generation synchrotron

We present recent advances in fast and bright scintillators for ultrafast X-ray phase contrast imaging of dynamic materials experiments at the upgraded Advanced Photon Source (APS-U), a fourth generation synchrotron. APS-U enables hard X-ray imaging at frame rates of at least 13 MHz (corresponding to 77 ns or shorter interframe intervals), creating a new need for scintillators with faster response and higher light output than lutetium yttrium oxyorthosilicate (LYSO). For indirect imaging and diffraction with ultrafast cameras, commercial lanthanum bromide (LaBr3) and cerium bromide (CeBr3) are promising candidates. These materials exhibit decay times approximately a factor of two shorter than LYSO (around 40 ns) and lutetium oxyorthosilicate (LSO), while maintaining comparable light yield per incident X-ray photon. However, their implementation at APS-U requires addressing several challenges, including material limitations due to hygroscopicity, efficient optical coupling to imaging systems, and high quantum efficiency for conversion of scintillation light, predominantly at wavelengths below 400 nm, into detectable electronic signals. We report results from material characterization, detector integration and packaging, and beamline experiments of materials with impact. In addition, emerging scintillator classes, including perovskites and high-entropy materials, are discussed as potential alternatives for next-generation ultrafast X-ray diagnostics.

Wang, Zhehui [Los Alamos] (ORCID:0000000178264063)↗

DOE OSTI2023

Unsupervised classification for region of interest in X-ray ptychography

X-ray ptychography offers high-resolution imaging of large areas at a high computational cost due to the large volume of data provided. To address the cost issue, we propose a physics-informed unsupervised classification algorithm that is performed prior to reconstruction and removes data outside the region of interest (RoI) based on the multimodal features present in the diffraction patterns. The preprocessing time for the proposed method is inconsequential in contrast to the resource-intensive reconstruction process, leading to an impressive reduction in the data workload to a mere 20% of the initial dataset. This capability consequently reduces computational time dramatically while preserving reconstruction quality. Through further segmentation of the diffraction patterns, our proposed approach can also detect features that are smaller than beam size and correctly classify them as within the RoI.

97 MATHEMATICS AND COMPUTING↗

NASA NTRS2015

How to Directly Image a Habitable Planet Around Alpha Centauri with a 30-45 cm Space Telescope

Several mission concepts are being studied to directly image planets around nearby stars. It is commonly thought that directly imaging a potentially habitable exoplanet around a Sun-like star requires space telescopes with apertures of at least 1m. A notable exception to this is Alpha Centauri (A and B), which is an extreme outlier among FGKM stars in terms of apparent habitable zone size: the habitable zones are approximately 3x wider in apparent size than around any other FGKM star. This enables a approximately 30-45cm visible light space telescope equipped with a modern high performance coronagraph or star shade to resolve the habitable zone at high contrast and directly image any potentially habitable planet that may exist in the system. The raw contrast requirements for such an instrument can be relaxed to 1e-8 if the mission spends 2 years collecting tens of thousands of images on the same target, enabling a factor of 500-1000 speckle suppression in post processing using a new technique called Orbital Difference Imaging (ODI). The raw light leak from both stars is controllable with a special wave front control algorithm known as Multi-Star Wave front Control (MSWC), which independently suppresses diffraction and aberrations from both stars using independent modes on the deformable mirror. This paper will present an analysis of the challenges involved with direct imaging of Alpha Centauri with a small telescope and how the above technologies are used together to solve them. We also show an example of a small coronagraphic mission concepts to take advantage of this opportunity called "ACESat: Alpha Centauri Exoplanet Satellite" submitted to NASA's small Explorer (SMEX) program in December of 2014.

exoplanets↗

DOE OSTI2024

Fe-carbide/Fe-oxide-based nanocomposites synthesized as magnetic nanomaterials via laser ablation synthesis in solution (LASiS)

Magnetic nanostructured materials (MNMs) have gained prominence in materials technology developments owing to their potential biomedical applications for hyperthermia cancer treatment, and transplant organ cryopreservation. Herein, we report the facile and cost-effective synthesis of Fe-based composite MNMs, comprising both Fe@Fe 2 O 3 and Fe 3 C@C core-shell nanoparticles (NPs), via Laser Ablation Synthesis in Solution (LASiS) using Fe targets ablated under acetone and toluene. Detailed materials characterizations using electron microscopy-based imaging, diffraction studies, and spectroscopic analyses - including Raman and Mössbauer spectroscopy - relate the structure-composition properties for different Fe-oxide/carbide phases in the aforesaid MNMs to their respective magnetic responses. Specifically, we confirm the presence of ultra-small (2–10 nm) amorphous Fe-oxide NPs, as well as Fe@Fe 2 O 3 core-shell NPs (20–40 nm) in the samples synthesized by ablating Fe under acetone. In contrast, samples synthesized under toluene indicate a higher concentration of Fe 3 C@C core-shell NPs (20–40 nm) with a relatively low concentration of Fe 2 O 3 NPs (2–10 nm). Furthermore, the crystallinity of the metallic phases and carbonaceous shell coatings are systematically increased by carrying out LASiS under heated toluene (up to ~95 °C). Importantly, mössbauer spectroscopy results indicate that the elevation in toluene temperature leads to an increase in the concentrations of Fe 3 C@C NPs from ~40 % to ~53 % (at.).

36 MATERIALS SCIENCE↗

DOE OSTI2023

Extensive 3D mapping of dislocation structures in bulk aluminum

Abstract Thermomechanical processing such as annealing is one of the main methods to tailor the mechanical properties of materials, however, much is unknown about the reorganization of dislocation structures deep inside macroscopic crystals that give rise to those changes. Here, we demonstrate the self-organization of dislocation structures upon high-temperature annealing in a mm-sized single crystal of aluminum. We map a large embedded 3D volume ( $$100\times 300\times 300$$ 100 × 300 × 300 $$\upmu$$ μ m $$^3$$ 3 ) of dislocation structures using dark field X-ray microscopy (DFXM), a diffraction-based imaging technique. Over the wide field of view, DFXM’s high angular resolution allows us to identify subgrains, separated by dislocation boundaries, which we identify and characterize down to the single-dislocation level using computer-vision methods. We demonstrate how even after long annealing times at high temperatures, the remaining low density of dislocations still pack into well-defined, straight dislocation boundaries (DBs) that lie on specific crystallographic planes. In contrast to conventional grain growth models, our results show that the dihedral angles at the triple junctions are not the predicted 120 $$^{\circ }$$ ∘ , suggesting additional complexities in the boundary stabilization mechanisms. Mapping the local misorientation and lattice strain around these boundaries shows that the observed strain is shear, imparting an average misorientation around the DB of $$\approx$$ ≈ 0.003 to 0.006 $$^{\circ }$$ ∘ .

36 MATERIALS SCIENCE↗

NASA NTRS1987

Nature and origin of mineral coatings on volcanic rocks of the Black Mountain, Stonewall Mountain, and Kane Springs, Wash volcanic centers, Southern Nevada

LANDSAT Thematic Mapper imagery was evaluated over 3 Tertiary calderas in southern Nevada. Each volcanic center derived from a highly evolved silici magmatic system represented today by well exposed diverse lithologies. Distinctive imagery contrast between some of the late ash flows and earlier units follows from the high relative reflectance in longer wavelength bands (bands 5 and 7) of the former. Enhancement techniques provide color composite images which highlight some of the units in remarkable color contrast. Inasmuch as coatings on the tuffs are incompletely developed and apparently largely dependent spectrally on rock properties independent of petrochemistry, it is felt that the distinctive imagery characteristics are more a function of primary lithologic or petrochemical properties. Any given outcrop is backdrop for a variety of cover types, of which coatings, at various stages of maturity, are one. Petrographic and X-ray diffraction analysis of the outer air-interface zone of coatings reveal they are composed chiefly of amorphous compounds, probably with varying proportions of iron and manganese. Observations support an origin for some outer (air-interface) coating constituents exogenous to the underlying host.

Taranik, James V.↗

NASA NTRS2021

Results From The Laboratory Demonstration Of A PIAACMC Coronagraph With A Segmented Aperture

The phase-induced amplitude apodization complex mask coronagraph (PIAACMC) provides high throughput and small inner working angle with little loss in image quality. Coronagraph compatibility with segmented apertures is essential for the success of habitable planet characterization with future large aperture space telescopes, such as the Large UV/Optical/Infrared (LUVOIR) and HabEx telescope mission concepts. The PIAACMC is compatible with such segmented telescope apertures with little loss of performance. We report the contrast and other performance results of a PIAACMC coronagraph with a LUVOIR-like pupil mask assembled and tested in a vacuum chamber at the JPL high contrast imaging testbed (HCIT). The goals of the demonstration were to achieve 1e-9 mean contrast over a semi-annular field of view from 2 λ/D to 8 λ/D, first with monochromatic light at 650nm, and then over a 10% spectral bandwidth. In addition, the measurement of jitter and its effect on PIAACMC performance will be discussed. As the success of electric field conjugation (EFC) to achieve best contrast on the testbed is dependent upon a diffraction model of the coronagraph, we will also discuss variations of the testbed and its diffraction model with the PIAACMC design, including suspected sources of knowledge error in the EFC diffraction model.

Wilson, Daniel↗

DOE OSTI2024

Systematic discovery of new nano-scale metastable intermetallic eutectic phases in laser rapid solidified Aluminum-Germanium alloy

Laser surface remelting of as-cast Al-Ge eutectic alloy is shown to produce ultrafine lamellar eutectic morphology with interlamellar spacing refined up to ∼60 nm and composed of FCC Al solid solution and unusual Al x Ge y intermetallic phases that do not form during near-equilibrium solidification. The microstructures are characterized and analyzed using a combination of selected area electron diffraction, high-resolution scanning transmission electron microscopy, energy dispersive X-ray spectroscopy to obtain high-resolution elemental maps, and atomistic modeling using density functional theory followed by atomic-scale image simulation. Depending on the local solidification conditions, the crystallography of the Al x Ge y intermetallic phases in the eutectic microstructure is either monoclinic (C 2/c) or monoclinic (P 2 1 ), with high densities of defects in both cases. This is in sharp contrast to the as-cast alloys that showed nominally pure Al and Ge phases with significant solute partitioning and equilibrium FCC and diamond cubic crystal structures, respectively. Corresponding kinetic phase diagrams are proposed to interpret the evolution of nano-lamellar eutectic morphologies with equilibrium Al and metastable Al x Ge y phases, and to explain increased solid solubility in the Al phases manifested by precipitation of ultrafine clusters of Ge. Furthermore, the reasons for the formation of these metastable eutectics under laser rapid solidification are discussed from the perspective of the competitive growth criterion.

Al-Ge eutectic↗

DOE OSTI2023

Toward accurate measurement of electromagnetic field by retrieving and refining the center position of non-uniform diffraction disks in Lorentz 4D-STEM

Recent advancement in scanning transmission electron microscopy (STEM) allows the use of 4D-STEM, a technique that captures an electron diffraction pattern at each scan point in STEM, to measure electrostatic and magnetic potential and field in materials. However, accurate measurement, separation of the magnetic and electric signals, and removal of artifacts remain challenging, especially in the presence of complex non-uniform diffraction contrast within the disks. In this work, based on dynamic simulations of 4D-STEM patterns built upon superstructures consisting of millions of atoms to account for different sample thickness and edge geometries, we show how the shape and intensity distribution of the central disk are affected by multiple scattering. We propose a robust refinement procedure through iteration of the spin-sensitive peak position of the disk-center in the circular Hough transform filtered images from experimental Lorentz 4D-STEM dataset after minimizing the possible artifacts, such as those due to the change of thickness, dynamic scattering, and scanning process. We verify that caution must be taken as in practice the rigid-disk-shift model used to reconstruct induction maps can easily break down due to disk-protrusion when there exists a nonconstant phase gradient or thickness within the width of the probe. Through quantitative analysis and comparing experiment with calculation the effect of the non-spin-related intensity distribution inside the disk as well as that causes the disk shift due to the intensity-protrusion can be removed, and high-quality magnetic field mapping is possible.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

DOE OSTI2021

Neutron Radiography and Computed Tomography of Biological Systems at the Oak Ridge National Laboratory's High Flux Isotope Reactor

Neutrons have historically been used for a broad range of biological applications employing techniques such as small-angle neutron scattering, neutron spin echo, diffraction, and inelastic scattering. Unlike neutron scattering techniques that obtain information in reciprocal space, attenuation-based neutron imaging measures a signal in real space that is resolved on the order of tens of micrometers. The principle of neutron imaging follows the Beer-Lambert law and is based on the measurement of the bulk neutron attenuation through a sample. Greater attenuation is exhibited by some light elements (most notably, hydrogen), which are major components of biological samples. Contrast agents such as deuterium, gadolinium, or lithium compounds can be used to enhance contrast in a similar fashion as it is done in medical imaging, including techniques such as optical imaging, magnetic resonance imaging, X-ray, and positron emission tomography. For biological systems, neutron radiography and computed tomography have increasingly been used to investigate the complexity of the underground plant root network, its interaction with soils, and the dynamics of water flux in situ. Moreover, efforts to understand contrast details in animal samples, such as soft tissues and bones, have been explored. This manuscript focuses on the advances in neutron bioimaging such as sample preparation, instrumentation, data acquisition strategy, and data analysis using the High Flux Isotope Reactor CG-1D neutron imaging beamline. The aforementioned capabilities will be illustrated using a selection of examples in plant physiology (herbaceous plant/root/soil system) and biomedical applications (rat femur and mouse lung).

Bilheux, Hassina↗

NASA NTRS1986

Performance comparison of Malvern instruments laser diffraction drop size analyzer

The performance of ten laser diffraction particle sizing instruments (Malvern models 2200 and 2600) has been evaluated using a synthetic particle size reference standard in a round-robin test at nine independent laboratories. A calibration reticle consisting of a two-dimensional array of opaque, circular particle images photoetched in chrome thin film deposited on a glass substrate was used as the reference. Mean diameters (e.g., D32) for the reticle measured by the ten unmodified instruments varied by 27 percent. In contrast, data from six instruments with individually calibrated photodetector correction factors demonstrated much better agreement and were within 2.6 percent of the actual reticle properties.

Hirleman, E. D.↗

DOE OSTI2023

Solving complex nanostructures with ptychographic atomic electron tomography

Abstract Transmission electron microscopy (TEM) is essential for determining atomic scale structures in structural biology and materials science. In structural biology, three-dimensional structures of proteins are routinely determined from thousands of identical particles using phase-contrast TEM. In materials science, three-dimensional atomic structures of complex nanomaterials have been determined using atomic electron tomography (AET). However, neither of these methods can determine the three-dimensional atomic structure of heterogeneous nanomaterials containing light elements. Here, we perform ptychographic electron tomography from 34.5 million diffraction patterns to reconstruct an atomic resolution tilt series of a double wall-carbon nanotube (DW-CNT) encapsulating a complex ZrTe sandwich structure. Class averaging the resulting tilt series images and subpixel localization of the atomic peaks reveals a Zr 11 Te 50 structure containing a previously unobserved ZrTe 2 phase in the core. The experimental realization of atomic resolution ptychographic electron tomography will allow for the structural determination of a wide range of beam-sensitive nanomaterials containing light elements.

36 MATERIALS SCIENCE↗

NASA NTRS2022

JWST/MIRI Coronagraphic Performances as Measured on-Sky

Context . Characterization of directly imaged exoplanets is one of the most eagerly anticipated science functions of the James Webb Space Telescope . MIRI, the mid-IR instrument, has the capability to provide unique spatially resolved photometric data points in a spectral range never before achieved for such objects. Aims . We aim to present the very first on-sky contrast measurements of the MIRI coronagraphs. In addition to a classical Lyot coronagraph at the longest wavelength, this observing mode implements the concept of the four-quadrant phase mask for the very first time in a space telescope. Methods . We observed single stars together with a series of reference stars to measure raw contrasts as they are delivered on the detector, as well as reference-subtracted contrasts. Results . The MIRI coronagraphs achieve raw contrasts better than 10 −3 at the smallest angular separations (within 1″) and about 10 −5 farther out (beyond 5 ~ 6″). Subtracting the residual diffracted light left behind the coronagraph has the potential to bring the final contrast down to the background- and detector-limited noise floor at most angular separations (a few times 10 −5 at less than 1″). Conclusions . The MIRI coronagraphs behave as expected from simulations. In particular, the raw contrasts for all four coronagraphs are fully consistent with the diffractive model. Contrasts obtained by subtracting reference stars also meet expectations and are fully demonstrated for two four-quadrant phase masks (F1065C and F1140C). The worst contrast, measured at F1550C, is very likely due to a variation in the phase aberrations at the primary mirror during the observations, and not an issue with the coronagraph itself. We did not perform reference star subtraction with the Lyot mask at F2300C, but we anticipate that it would bring the contrast down to the noise floor.

High angular resolution instrumentation↗

NASA NTRS2013

HCIT Contrast Performance Sensitivity Studies: Simulation Versus Experiment

Using NASA's High Contrast Imaging Testbed (HCIT) at the Jet Propulsion Laboratory, we have experimentally investigated the sensitivity of dark hole contrast in a Lyot coronagraph for the following factors: 1) Lateral and longitudinal translation of an occulting mask; 2) An opaque spot on the occulting mask; 3) Sizes of the controlled dark hole area. Also, we compared the measured results with simulations obtained using both MACOS (Modeling and Analysis for Controlled Optical Systems) and PROPER optical analysis programs with full three-dimensional near-field diffraction analysis to model HCIT's optical train and coronagraph.

space telescopes↗

DOE OSTI2023

Hollow Ptychography: Toward Simultaneous 4D Scanning Transmission Electron Microscopy and Electron Energy Loss Spectroscopy

With the recent development of high-acquisition-speed pixelated detectors, 4D scanning transmission electron microscopy (4D-STEM) is becoming routinely available in high-resolution electron microscopy. 4D-STEM acts as a “universal” method that provides local information on materials that is challenging to extract from bulk techniques. It extends conventional STEM imaging to include super-resolution techniques and to provide quantitative phase-based information, such as differential phase contrast, ptychography, or Bloch wave phase retrieval. However, an important missing factor is the chemical and bonding information provided by electron energy loss spectroscopy (EELS). 4D-STEM and EELS cannot currently be acquired simultaneously due to the overlapping geometry of the detectors. Here, the feasibility of modifying the detector geometry to overcome this challenge for bulk specimens is demonstrated, and the use of a partial or defective detector for ptycholgaphic structural imaging is explored. Here, results show that structural information beyond the diffraction-limit and chemical information from the material can be extracted together, resulting in simultaneous multi-modal measurements, adding the additional dimensions of spectral information to 4D datasets.

4D-scanning transmitting electron microscopy (STEM↗

NASA NTRS2022

Atomic-Scale Structure and Non-Stoichiometry of Meteoritic Hibonite: A Transmission Electron Microscope Study

Hibonite (CaAl_12O_19) is a common refractory mineral in Ca-Al-rich inclusions (CAIs) in primitive meteorites. Transmission electron microscope (TEM) studies have identified enigmatic planar defects in different occurrences of hibonite in the Allende meteorite that give rise to strong streaking along c* in electron diffraction patterns. Atomic resolution high-angle annular dark-field (HAADF) imaging and energy-dispersive X-ray (EDX) analyses were used to determine the nature and origin of these planar features. HAADF images of hibonite grains reveal lamellar intergrowths of common 1.6 nm spacing, and less commonly 2.0 and 2.5 nm spacings, interspersed in stoichiometric hibonite showing 1.1 nm (002) spacing. Stoichiometric hibonite consists of alternating Ca-containing (“R”) and spinel-structured (“S”) blocks stacked in a sequence RS. In contrast, the 1.6 nm layers result from a doubled S block such that the stacking sequence is RSS, while in the widest defect observed, the stacking sequence is RSSSS. These intergrowths are epitaxial and have coherent, low-strain boundaries with the host hibonite Meteoritic hibonite shows common Ti and Mg substitution for Al in its structure. Atomic-resolution EDX maps of hibonite grains in the Allende CAI confirm the preferred site occupancy of Mg on tetragonal M3 sites in S blocks and of Ti on trigonal bipyramidal M2 and octahedral M4 sites in R blocks. Mg is highly concentrated, but Ti is absent in the planar defects where wider S blocks show Al-rich compositions compared to stoichiometric MgAl_2O_4 spinel. Therefore, Mg likely played the major role in the formation and metastability of planar defects in hibonite. Electron energy loss spectroscopy data from the Ti L_2,3 edge show the presence of mixed Ti oxidation states with ~ 15–20% of Ti as Ti^(3+) in hibonite, suggesting a direct substitution of Ti^(3+) ↔ Al^(3+) in hibonite. The remaining ~ 80–85% of Ti is present as Ti^(4+) and corresponding EDX analyses are consistent with the well-known coupled substitution 2Al^(3+) ↔ Ti^(4+) + Mg^(2+) being the major mechanism for Ti and Mg substitution in hibonite. The formation of planar defects in hibonite occurred during high-temperature nebular condensation or melting/crystallization processes. The occurrence of non-stoichiometric hibonite in the Allende CAI deviates from the mineral formation sequence predicted from equilibrium condensation models. Overall, our atomic resolution TEM observations signify non-equilibrium, kinetic-controlled crystal growth during the high-temperature formation of refractory solids in the early solar nebula.

hibonite↗

NASA NTRS2021

ExEP: Initial super-Nyquist wavefront control experiments in the Decadal Survey Testbed

In order to characterize exoplanets around nearby stars, upcoming and proposed space telescopes are being designed with high contrast coronagraph instruments. Coronagraphs are generally designed to suppress only a single, on-axis star, but there are numerous binary star systems within our observational range. Multi-star wavefront correction (MSWC) is a technique that uses deformable mirror(s) to simultaneously suppress light from more than one star to create a high contrast dark zone in the image. MSWC has already been well demonstrated in simulation and in air-based testbeds. In this paper, we describe our prepatory vacuum experiments in the Decadal Survey Testbed (DST) at the Jet Propulsion Laboratory. First we implemented super-Nyquist wavefront control (SNWC, a critical component of MSWC), and then we proceeded to simultaneous sub- and super-Nyquist control. With our existing calibration methods, SNWC reached a contrast of $8.6{\times}10^{-9}$ in a 10\% bandpass around a first-order diffraction spot; calibration improvements are needed to improve model agreement for higher-order spots. We have also implemented changes to our software (the open-source package FALCO) required for MSWC, and identified the necessary changes in hardware. Here we report our best SNWC lab results and our plans for implementing MSWC during a future set of experiments.

Bendek, Eduardo↗

DOE OSTI2021

Ex Situ Photoelectron Emission Microscopy of Polycrystalline Bismuth and Antimony Telluride Surfaces Exposed to Ambient Oxidation

The surfaces of textured polycrystalline N-type bismuth telluride and P-type antimony telluride materials were investigated using ex situ photoelectron emission microscopy (PEEM). PEEM enabled imaging of the work function for different oxidation times due to exposure to air across sample surfaces. The spatially averaged work function was also tracked as a function of air exposure time. N-type bismuth telluride showed an increase in the work function around grain boundaries relative to grain interiors during the early stages of air exposure-driven oxidation. At longer time exposure to air, the surface became homogenous after a ~5 nm-thick oxide formed. X-ray photoemission spectroscopy was used to correlate changes in PEEM imaging in real space and work function evolution to the progressive growth of an oxide layer. The observed work function contrast is consistent with the pinning of electronic surface states due to the defects at a grain boundary.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗