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DOE OSTI2024

Structure–performance relationships of lithium-ion battery cathodes revealed by contrast-variation small-angle neutron scattering

Lithium-ion battery cathodes are porous composites of active material, conductive carbon, and polymer binder. Controlling the cathode microstructure is key to achieving high energy density and cycling stability. Current characterization techniques lack the nanoscale resolution over representative volumes necessary to relate cathode microstructure to cycling performance. To address this challenge, we utilize contrast-variation small-angle neutron scattering to quantify the chemical and structural features of cathodes wet by dimethyl carbonate, representing a relevant solvent environment. Using neutron scattering measurements, we identify an expansion in carbon and polymer structures that arises after calendering and wetting with solvent. Further, we deconvolute the carbon and binder phases to obtain the solvent-accessible carbon black surface area, which we correlate to diminished capacity retention driven by electrolyte decomposition on exposed carbon. This technique provides nanoscale insight into composite cathode microstructures and resulting cycling performance, promising future applications to a broad range of porous materials that exist in energy storage systems.

25 ENERGY STORAGE↗

DOE OSTI2025

Strain-driven oxygen vacancy ordering in LaNiO 3 thin films revealed by integrated differential phase contrast imaging in scanning transmission electron microscopy

Rare-earth nickelates, such as LaNiO 3 (LNO), exhibit complex electronic properties, with ordered oxygen vacancies (OOV) influencing conductivity and magnetic behavior. We investigate the structural stability of strain-induced OOV phases in LNO thin films grown on SrTiO 3 substrates and the impact of Ruddlesden–Popper (RP) faults. Using high-angle annular dark-field scanning transmission electron microscopy (HAADF-STEM) and integrated differential phase contrast (iDPC) STEM imaging, we conducted atomic-scale structural and compositional analyses of OOV. Geometric phase analysis (GPA) was employed to measure the strain in fault-free and RP fault regions, while density functional theory (DFT) calculations explored different OOV arrangements in the LNO phase. Simulated iDPC-STEM imaging of energy-stabilized structures was performed to correlate with experimental results. Here, our findings reveal superstructure modulation in the chemical composition and atomic-scale lattice structure in LNO, primarily due to the formation of the OOV in Ni–O layers of the LaNiO 2.5 phase. The out-of-plane compressive strain of about 2% stabilizes this phase, reducing the strain, diminishing OOV, and transforming them into LNO.

36 MATERIALS SCIENCE↗

DOE OSTI2021

Fluorescence intensity correlation imaging with high spatial resolution and elemental contrast using intense x-ray pulses

We theoretically investigate the fluorescence intensity correlation (FIC) of Ar clusters and Mo-doped iron oxide nanoparticles subjected to intense, femtosecond, and sub-femtosecond x-ray free-electron laser pulses for high-resolution and elemental contrast imaging. We present the FIC of Kα and Kαh emission in Ar clusters and discuss the impact of sample damage on retrieving high-resolution structural information and compare the obtained structural information with those from the coherent diffractive imaging (CDI) approach. We found that, while sub-femtosecond pulses will substantially benefit the CDI approach, few-femtosecond pulses may be sufficient for achieving high-resolution information with the FIC. Furthermore, we show that the fluorescence intensity correlation computed from the fluorescence of the Mo atoms in Mo-doped iron oxide nanoparticles can be used to image dopant distributions in the nonresonant regime.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗

DOE OSTI2025

Statistically elucidated responses from low-signal contrast mechanisms in ultrafast electron microscopy

The emergence of ultrafast electron microscopy (UEM) has enabled the discovery of strongly correlated dynamic mechanisms, including electron–phonon coupling, structural phase transitions, thermal transport, and electromagnetic deflection. Most UEM systems operate stroboscopically, meaning that the technique is susceptible to artifacts, mistakes, and misinterpretation of the data due to extensive experimental effort. In contrast to the ultrafast designation, data acquisition is extraordinarily slow because the electron beam has significantly reduced signal compared to traditional transmission electron microscopy due to pulsing the electron beam. Consequently, the sample may drift, tilt, or undergo irreversible structural changes that are independent of the time-resolved dynamics throughout the experimental time frame. Furthermore, these datasets require significant user interpretation that can be problematic when proper controls are not implemented thoroughly. Here, we demonstrate a new algorithm designed to separate ultrafast structural dynamics from long-term artifacts using a LiNbO 3 sample experiencing electrically driven surface acoustic wave propagation. Additionally, we provide examples of the impact of user bias when analyzing the data and provide a methodology, which enables the extraction of time-resolved responses when the image signal is extraordinarily low. Overall, the goal of this publication is to provide methods that validate the experimental results and reduce researcher biases during UEM data interpretation.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

DOE OSTI2022

High spatial resolution and contrast radiography of hydrodynamic instabilities at the National Ignition Facility

In this work, we are developing techniques for studying the Rayleigh–Taylor (RT) and Richtmyer–Meshkov (RM) instabilities in a planar geometry at high-energy-densities at the National Ignition Facility (NIF). In particular, through the improvement of experimental imaging quality, we are progressing toward the study of the turbulent regime of the mixing regions in capsule implosion experiments for inertial confinement fusion, which requires few micrometers resolution. Using 60 NIF beams, a solid shock tube is driven launching a shock wave that crosses the interface between a dense and a light material pre-machined in the target to obtain sinusoidal ripples, which results in RM and RT instabilities that are imaged using the NIF Crystal Backlighter Imager. High-quality images were obtained with a mean resolution of 7 μm and improved contrast. While the obtained resolution does not allow the observation of the smallest scale of the “turbulent” energy spectrum, the generated image encompasses 63% of the total flow energy, a 50% improvement over previous studies, which is observed for the first time a roll-up feature in a high energy density-type RT experiment.

70 PLASMA PHYSICS AND FUSION TECHNOLOGY↗

DOE OSTI2023

Evaluation protocol for revealing magnonic contrast in TR-STXM measurements

We present a statistically motivated method to extract magnonic contrast from time-resolved scanning transmission x-ray microscopy (TR-STXM) measurements. TR-STXM is an element-specific method for resolving spin-dynamics in space and time. It offers nanometer spatial resolution and picosecond temporal resolution. The presented method makes it possible to obtain phase and amplitude profiles of spin-waves from STXM measurements. Furthermore, it allows for a rigorous transformation to reciprocal magnon k⃗-space, revealing k⃗-dependent magnon properties such as the magnon dispersion in three dimensions and for all directions of the magnetic anisotropy. We demonstrate our method using X-band ferromagnetic resonance on a micrometer-sized permalloy assembly.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗

DOE OSTI2023

Contrast optimization of Fresnel zone plate imaging

Fresnel zone plates (FZPs) are circular diffractive elements that operate as a lens for x-rays. They have gained interest in the field of laser-plasma physics due to their ability to achieve higher spatial resolution than pinholes. Their design and implementation are complicated by the fact that a significant amount of the x-rays passing through the FZP will not diffract (zeroth order) and present a background to the measurement. This background can be large and inhomogeneous depending on the geometric setup of the experiment. Furthermore, we present calculations of the diffracted (first order) and un-diffracted (zeroth order) flux profiles, which makes it possible to optimize the contrast between the first order imaging rays and the zeroth order background. Calculations for the implementation of a central block in the FZP, designed to block the zeroth from the entire field of view, are also presented.

47 OTHER INSTRUMENTATION↗

DOE OSTI2023

Quantitative x ray phase contrast imaging of oblique shock wave–interface interactions

Oblique shock wave–interface interactions of gases and liquids have been extensively studied in shock tubes using optical methods to measure equation-of-state (EOS) parameters. However, this is difficult with solids due to their opaqueness to visible light. X ray phase contrast imaging (XPCI) has the penetrative strength to probe solids while still being sensitive to mass density and enhancing the visibility of material boundaries. We investigate the accuracy and repeatability of measuring the mean value of the average mass density (areal density divided by thickness) over region S (B S ) and flow deflection angle (θ) from XPCI images of a sample. To that end, a Hough transform-based method for measuring θ is developed. To measure B S , the XPCI image intensity probability density function (PDF) is modeled accounting for the spatial distribution of x ray energy, scintillator response, and pulse-to-pulse variation in the x ray intensity. In addition, a Monte Carlo-based algorithm for computing the B S PDF is developed. Both methods are validated on an impact-generated oblique shock wave interacting at a solid polymer-to-polymer interface. Furthermore this is accomplished through a comparison to hydrodynamic simulations using well-established EOS. Under the modeling framework for the XPCI image intensity, B S is computed with an accuracy of < 0.1% and precision of 3%–5%, while θ has an uncertainty of 0.2°, respectively. This shows that the XPCI-based model that is developed here could be an invaluable tool for high-fidelity testing of hydrodynamic models in shock polar configurations.

72 PHYSICS OF ELEMENTARY PARTICLES AND FIELDS↗

DOE OSTI2024

Localized phase contrast imaging at the Wendelstein 7-X stellarator

In its basic form, phase contrast imaging (PCI) provides line-integrated measurements of electron density fluctuations in plasmas. As turbulent fluctuations in magnetically confined plasmas have wave vectors almost perpendicular to the background magnetic field, the signals scattered by fluctuations from different parts of the PCI line-of-sight (LoS) are spatially separated in focal planes of the plasma. This allows localized PCI measurements by placing a mask in such a plane, to only permit signals from specific parts of the LoS to reach the PCI detectors. The present paper describes modeling and design of localization masks for the PCI system at the Wendelstein 7-X (W7-X) stellarator as well as the first results obtained using the masks in the recent long-pulse W7-X experimental campaign. During this project, we have extended the theory describing the mask response within the Fraunhofer diffraction model. As a novel development, we show from first principles that the mask response is determined by the fraction of power of the scattered beam spots that passes the mask. These insights have been used to select the W7-X mask design, consisting of a circular cutout, allowing the unscattered beam spot to pass the mask, with wedges covering a fixed angular range outside the central cutout. In the recent W7-X experimental campaign, the masks have verified the location of the main turbulence features observed by the PCI system and provided new information about the location of short-wavelength magnetohydrodynamic modes.

Physics↗

DOE OSTI2026

Implementation of heterodyne detection of radio frequency waves using phase contrast imaging

An upgrade to the DIII–D phase contrast imaging (PCI) diagnostic for detection of radio frequency waves has been implemented using low-noise optical heterodyning. Electro-optical modulation allows detection of waves with frequencies up to 500 MHz with wide flexibility restricted only by the driver electronics, with continuous adjustability up to 100 MHz and fixed frequency drivers needed for higher frequencies. The PCI diagnostic images the line-integrated plasma density fluctuations and provides absolutely calibrated measurements with good wavenumber resolution.

Rost, J. C. [Massachusetts Institute of Technology↗

DOE OSTI2020

Utilisation of spatial derivative measurements in circular diffuse optical tomographic imaging to improve image resolution and contrast

The resolution of images recovered using diffuse optical tomography without spatial prior information is inherently limited due to the diffusive nature of light transport in scattering dominated biological tissue. Several studies have previously reported an improvement in depth sensitivity in near infrared spectroscopy by considering the subtraction of two neighbouring measurements. A nearest neighbour, spatial derivative based algorithm is presented, in which the difference between neighbouring source-sharing source – detector pairs is considered for tomographic reconstruction. Using a circular, inward-facing optode geometry, it is shown that deeper abnormalities in oxyhaemoglobin, deoxyhaemoglobin and water can be recovered with better localisation and contrast as compared to reconstructing using absolute values of multi-wavelength data. Relative improvements of up to 25 % in quantitative accuracy of recovered physiological values are demonstrated at better resolution for cancerous tissue in a heterogeneous breast model, when using this proposed spatial derivative based parameter reconstruction. (paper)

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗

DOE OSTI2020

Laser speckle contrast imaging of blood microcirculation in pancreatic tissues during laparoscopic interventions

Laser speckle contrast imaging of the microcirculatory bed of the pancreas is performed, which allows its condition to be assessed and thereby is an additional valuable tool for making a diagnostic decision and dynamically monitoring the effectiveness of the treatment for pathology of the abdominal organs. Laparoscopic operations on the pancreas are low-traumatic and in most cases avoid open surgical interventions. For the first time an experimental system for recording speckle images, combined with a commercially available five-millimetre rigid laparoscope, is presented. The sensitivity of the system to the fluid motion in a capillary at different velocities is determined, and the possibility of finding areas of blood microcirculation disturbance in modelling pancreatic ischemia in an experiment on laboratory animals is revealed. The laparoscope illumination channel is verified by comparison with speckle dynamics under external illumination of the studied object. (paper)

60 APPLIED LIFE SCIENCES↗

DOE OSTI2024

Upstream surface roughness and terrain are strong drivers of contrast in tornado potential between North and South America

Central North America is the global hotspot for tornadoes, fueled by elevated terrain of the Rockies to the west and a source of warm, moist air from equatorward oceans. This conventional wisdom argues that central South America, with the Andes to the west and Amazon basin to the north, should have a “tornado alley” at least as active as central North America. Central South America has frequent severe thunderstorms yet relatively few tornadoes. Here, we show that conventional wisdom is missing an important ingredient specific to tornadoes: a smooth, flat ocean-like upstream surface. Using global climate model experiments, we show that central South American tornado potential substantially increases if its equatorward land surface is smoothed and flattened to be ocean-like. Similarly, we show that central North American tornado potential substantially decreases if its equatorward ocean surface is roughened to values comparable to forested land. A rough upstream surface suppresses the formation of tornadic environments principally by weakening the poleward low-level winds, characterized by a weakened low-level jet east of the mountain range. Results are shown to be robust for any midlatitude landmass using idealized experiments with a simplified continent and mountain range. Our findings indicate that large-scale upstream surface roughness is likely a first-order driver of the strong contrast in tornado potential between North and South America.

54 ENVIRONMENTAL SCIENCES↗

DOE OSTI2020

Visualizing a viral genome with contrast variation small angle X-ray scattering

Despite the threat to human health posed by some single-stranded RNA viruses, little is understood about their assembly. The goal of this work is to introduce a new tool for watching an RNA genome direct its own packaging and encapsidation by proteins. Contrast variation small-angle X-ray scattering (CV-SAXS) is a powerful tool with the potential to monitor the changing structure of a viral RNA through this assembly process. The proteins, though present, do not contribute to the measured signal. As a first step in assessing the feasibility of viral genome studies, the structure of encapsidated MS2 RNA was exclusively detected with CV-SAXS and compared with a structure derived from asymmetric cryo-EM reconstructions. Additional comparisons with free RNA highlight the significant structural rearrangements induced by capsid proteins and invite the application of time-resolved CV-SAXS to reveal interactions that result in efficient viral assembly.

59 BASIC BIOLOGICAL SCIENCES↗

DOE OSTI2022

Development of a synthetic phase contrast imaging diagnostic for turbulence studies at Wendelstein 7-X

Abstract We present a synthetic phase contrast imaging (PCI) diagnostic for studying turbulence at the Wendelstein 7-X (W7-X) stellarator. We first describe the implemented instrument response model, which captures diffraction effects, detector noise, and the long-wavelength cutoff due to the phase plate of the PCI system. To verify the instrument response model, we show that it is capable of reproducing the PCI signal generated by the sound wave speaker used for calibration at W7-X. Next, we discuss the calculation of synthetic PCI signals based on the global, nonlinear gyrokinetic codes GENE-3D and EUTERPE, including results from some of the first stellarator simulations of this type with kinetic electrons (KEs) in GENE-3D. While the simulations used in this work lack a neoclassical radial electric field, which is crucial for reproducing experimental PCI signals, they do indicate that the dominant rotation direction and velocities of the turbulent fluctuations can be inferred from the wave number-frequency spectra of the PCI signals, as expected. The synthetic PCI wave number spectra are further shown to be similar to those of the line-integrated fluctuating electron density, with distinct differences between adiabatic and KE simulations, explainable by previously published turbulence models. For example, the wave number spectra of all adiabatic electron simulations analyzed here follow a power law with an exponent close to −5 for sufficiently large wave numbers. This indicates that universal features of electron density turbulence at W7-X may be studied using the PCI system.

EUTERPE↗

DOE OSTI2019

A combined Phase Contrast Imaging and heterodyne interferometer for multiscale fluctuation measurements in tokamak plasmas

An upgrade to the Phase Contrast Imaging (PCI) diagnostic on the DIII-D tokamak has successfully combined PCI with density interferometry to provide electron density fluctuation measurements across an unprecedented range in wavenumber. The combined diagnostic uses a single laser and a single beam path through the tokamak, minimizing machine resources in anticipation of future reactor-scale devices where port access will be at a premium. The PCI multichannel detector provides low-noise, wavenumber-resolved detection of moderate-wavenumber turbulence, while the interferometer channel is sensitive to long-wavelength turbulence, including the peak of ion-scale turbulence and MHD. The overlap in wavenumber range between the two schemes allows for an in situ absolute calibration of the PCI.

70 PLASMA PHYSICS AND FUSION TECHNOLOGY↗

DOE OSTI2021

The Wendelstein 7-X phase contrast imaging diagnostic

We report a phase contrast imaging (PCI) diagnostic has been developed for the Wendelstein 7-X (W7-X) stellarator. The PCI diagnostic provides a line-integrated measurement of turbulent electron density fluctuations, which is essential for understanding high performance scenarios that can lead to improved confinement at fusion-relevant temperatures and densities. The PCI system is also sensitive to coherent fluctuations, which arise from Alfvén eigenmodes or other MHD activity. This paper provides an overview of the hardware and the optical system and presents an example PCI measurement from the W7-X OP1.2b experimental campaign.

70 PLASMA PHYSICS AND FUSION TECHNOLOGY↗

DOE OSTI2021

Stimulation of Dissimilatory Sulfate Reduction in Response to Sulfate in Microcosm Incubations from Two Contrasting Temperate Peatlands near Ithaca, NY, USA

Abstract Peatlands are responsible for over half of wetland methane emissions, yet major uncertainties remain regarding carbon flow, especially when increased availability of electron acceptors stimulate competing physiologies. We used microcosm incubations to study the effects of sulfate on microorganisms in two temperate peatlands, one bog and one fen. Three different electron donor treatments were used (13C-acetate, 13C-formate, and a mixture of 12C short-chain fatty acids) to elucidate the responses of sulfate-reducing bacteria (SRB) and methanogens to sulfate stimulation. Methane production was measured and metagenomic sequencing was performed, with only the heavy DNA fraction sequenced from treatments receiving 13C electron donors. Our data demonstrate stimulation of dissimilatory sulfate reduction in both sites, with contrasting community responses. In McLean Bog (MB), hydrogenotrophic Deltaproteobacteria and acetotrophic Peptococcaceae lineages of SRB were stimulated, as were lineages with unclassified dissimilatory sulfite reductases. In Michigan Hollow Fen (MHF), there was little stimulation of Peptococcaceae populations, and a small stimulation of Deltaproteobacteria SRB populations only in the presence of formate as electron donor. Sulfate stimulated an increase in relative abundance of reads for both oxidative and reductive sulfite reductases, suggesting stimulation of an internal sulfur cycle. Together, these data indicate a stimulation of SRB activity in response to sulfate in both sites, with a stronger growth response in MB than MHF. This study provides valuable insights into microbial community responses to sulfate in temperate peatlands and is an important first step to understanding how SRB and methanogens compete to regulate carbon flow in these systems.

Microbiology↗