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DOE OSTI2024

The Liquid Jet Endstation for Hard X-ray Scattering and Spectroscopy at the Linac Coherent Light Source

The ability to study chemical dynamics on ultrafast timescales has greatly advanced with the introduction of X-ray free electron lasers (XFELs) providing short pulses of intense X-rays tailored to probe atomic structure and electronic configuration. Fully exploiting the full potential of XFELs requires specialized experimental endstations along with the development of techniques and methods to successfully carry out experiments. The liquid jet endstation (LJE) at the Linac Coherent Light Source (LCLS) has been developed to study photochemistry and biochemistry in solution systems using a combination of X-ray solution scattering (XSS), X-ray absorption spectroscopy (XAS), and X-ray emission spectroscopy (XES). The pump–probe setup utilizes an optical laser to excite the sample, which is subsequently probed by a hard X-ray pulse to resolve structural and electronic dynamics at their intrinsic femtosecond timescales. The LJE ensures reliable sample delivery to the X-ray interaction point via various liquid jets, enabling rapid replenishment of thin samples with millimolar concentrations and low sample volumes at the 120 Hz repetition rate of the LCLS beam. This paper provides a detailed description of the LJE design and of the techniques it enables, with an emphasis on the diagnostics required for real-time monitoring of the liquid jet and on the spatiotemporal overlap methods used to optimize the signal. Additionally, various scientific examples are discussed, highlighting the versatility of the LJE.

EXAFS↗

DOE OSTI2023

Mesoscopic two-point collective dynamics of glass-forming liquids

The collective density–density and hydrostatic pressure–pressure correlations of glass-forming liquids are spatiotemporally mapped out using molecular dynamics simulations. It is shown that the sharp rise of structural relaxation time below the Arrhenius temperature coincides with the emergence of slow, nonhydrodynamic collective dynamics on mesoscopic scales. The observed long-range, nonhydrodynamic mode is independent of wave numbers and closely coupled to the local structural dynamics. Below the Arrhenius temperature, it dominates the slow collective dynamics on length scales immediately beyond the first structural peak in contrast to the well-known behavior at high temperatures. Furthermore, these results highlight a key connection between the qualitative change in mesoscopic two-point collective dynamics and the dynamic crossover phenomenon.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2026

Visualizing Crystallization Dynamics and Transformation Pathways of Disordered Rocksalt Oxides During Thermally Activated Sol–Gel Synthesis

Sol–gel synthesis is a wet-chemical processing route for fabricating functional materials with control over composition and microstructure at relatively low temperatures compared to conventional solid-state synthesis. While sol–gel process initiates with intermixed molecular precursors, the early-stage nucleation pathways are insufficiently understood. Here, in this study, the chemical and structural transformation of ion disordered rocksalt (DRX) Li 1.2 Mn 0.4 Ti 0.4 O 2 (LMTO), a promising cathode material for lithium batteries, is studied by multiscale characterizations. In situ heating transmission electron microscopy (TEM) using a liquid cell visualizes and identifies crystallization pathways at the nanoscale. While some regions follow a classical multi-step transition through thermodynamically stable intermediates, others exhibit a kinetic shortcut via a localized amorphous matrix to directly form the DRX structure. Macroscale Fourier transform infrared spectroscopy corroborates the findings and reveals that transition metal ions are more strongly incorporated into the acetate-coordinated network than lithium. Although in situ heating TEM captures diverse local transformation pathways, in situ synchrotron X-ray diffraction indicates that the macroscopic transformation proceeds predominantly through spinel LMTO and lithium titanates toward DRX-LMTO. The findings uncover the spatiotemporal chemical and structural transformations in sol–gel derived DRX-LMTO materials, and call for fine-tuning of such sol–gel chemistries to manipulate the crystallization pathways and achieve target material homogeneity more efficiently.

cathode material↗

NASA NTRSDate not supplied

Correlated Spatiotemporal Evolution of Extreme-Ultraviolet Ribbons and Hard X-rays in a Solar Flare

We study the structure and evolution of solar flare ribbons in the chromosphere to infer properties of magnetic reconnection that occurs in the corona. We analyze the imaging observations of the M7.3 SOL2014-04-18T13 flare obtained by IRIS in both the near and far ultraviolet passbands and by SDO/AIA in the 1600A passband. Two flare ribbons are observed to spread away from the magnetic polarity inversion line as the flare progresses. Using the high-resolution IRIS observations, we measure the width of the newly brightened ribbon front along the extension of the ribbon, which maps the feet of magnetic field lines reconnecting in the current sheet in the corona. We find that the width of the ribbon front is highly structured, possibly reflecting corresponding structure in the coronal current layer. Further the ribbon grows most rapidly with time in regions where non-thermal hard X-ray (HXR) emission is concentrated (Brosius, et al. 2015). The light curve of the ultraviolet emissions in this region, as measured by IRIS and AIA, also well matches the HXR light curve at photon energies above 25 keV. In contrast, the ribbon-width evolution and light curves in other regions along the ribbons do not correlate well with the HXR emission. These results suggest that there is a strong connection between the production of non-thermal electrons and locally enhanced perpendicular extent of flare ribbon fronts, which reflect the inhomogeneous structure and/or reconnection dynamics of the flare current sheet in the corona.

Stephen Naus↗

DOE OSTI2023

Robotic pendant drop: containerless liquid for μs-resolved, AI-executable XPCS

Abstract The dynamics and structure of mixed phases in a complex fluid can significantly impact its material properties, such as viscoelasticity. Small-angle X-ray Photon Correlation Spectroscopy (SA-XPCS) can probe the spontaneous spatial fluctuations of the mixed phases under various in situ environments over wide spatiotemporal ranges (10 −6 –10 3 s /10 −10 –10 −6 m). Tailored material design, however, requires searching through a massive number of sample compositions and experimental parameters, which is beyond the bandwidth of the current coherent X-ray beamline. Using 3.7-μs-resolved XPCS synchronized with the clock frequency at the Advanced Photon Source, we demonstrated the consistency between the Brownian dynamics of ~100 nm diameter colloidal silica nanoparticles measured from an enclosed pendant drop and a sealed capillary. The electronic pipette can also be mounted on a robotic arm to access different stock solutions and create complex fluids with highly-repeatable and precisely controlled composition profiles. This closed-loop, AI-executable protocol is applicable to light scattering techniques regardless of the light wavelength and optical coherence, and is a first step towards high-throughput, autonomous material discovery.

36 MATERIALS SCIENCE↗

DOE OSTI2022

Ultrafast electron diffraction: Visualizing dynamic states of matter

Since the discovery of electron-wave duality, electron scattering instrumentation has developed into a powerful array of techniques for revealing the atomic structure of matter. Beyond detecting local lattice variations in equilibrium structures with the highest possible spatial resolution, recent research efforts have been directed toward the long-sought-after dream of visualizing the dynamic evolution of matter in real time. The atomic behavior at ultrafast timescales carries critical information on phase transition and chemical reaction dynamics, the coupling of electronic and nuclear degrees of freedom in materials and molecules, and the correlation among structure, function, and previously hidden metastable or nonequilibrium states of matter. Ultrafast electron pulses play an essential role in this scientific endeavor, and their generation has been facilitated by rapid technical advances in both ultrafast laser and particle accelerator technologies. Here this review presents a summary of the noteworthy developments in this field in the last few decades. The physics and technology of ultrafast electron beams is presented with an emphasis on the figures of merit most relevant for ultrafast electron diffraction experiments. Recent developments in the generation, manipulation, and characterization of ultrashort electron beams aimed at improving the combined spatiotemporal resolution of these measurements are discussed. The fundamentals of electron scattering from atomic matter and the theoretical frameworks for retrieving dynamic structural information from solid-state and gas-phase samples is described. Essential experimental techniques and several landmark works that have applied these approaches are also highlighted to demonstrate the widening applicability of these methods. Ultrafast electron probes with ever-improving capabilities, combined with other complementary photon-based or spectroscopic approaches, hold tremendous potential for revolutionizing our ability to observe and understand energy and matter at atomic scales.

43 PARTICLE ACCELERATORS↗

DOE OSTI2024

Spatiotemporal control of high-intensity laser pulses with a plasma lens

Spatiotemporal control encompasses a variety of techniques for producing laser pulses with dynamic intensity peaks that move independently of the group velocity. This controlled motion of the intensity peak offers a new approach to optimizing laser-based applications and enhancing signatures of fundamental phenomena. Here, we demonstrate spatiotemporal control with a plasma optic. A chirped laser pulse focused by a plasma lens exhibits a moving focal point, or “flying focus,” that can travel at an arbitrary, predetermined velocity. Unlike currently used conventional or adaptive optics, a plasma lens can be located close to the interaction region and can operate at an orders of magnitude higher, near-relativistic intensity. Published by the American Physical Society 2024

70 PLASMA PHYSICS AND FUSION TECHNOLOGY↗

DOE OSTI2025

Probing Surface Plasmon Dynamics in Periodic Nanostructures through Ultrafast Electron Microscopy

Surface plasmon polaritons (SPPs) can be manipulated to localize and guide light in subwavelength distances, enabling them to find applications in a wide range of areas, from sensing to quantum computing. Among several methods of SPP excitation, periodic arrays of nano- and microstructures are of particular interest, as they enable engineering SPP properties through structural parameters. Here, in this study, using the photon-induced near-field electron microscopy (PINEM) technique, we investigated the mode formation, coupling, interference, and decay of SPPs in square and hexagonal arrays of circular nanoholes under both visible and near-infrared excitation. Polarization-resolved analysis revealed the key factors governing SPP localization and interference patterns, showing that the periodicity and symmetry of the array primarily determine the SPP interference patterns and their orientation, while pump polarization mainly modulates their intensity. Time-resolved PINEM measurements demonstrated the spatial dependence of the SPP temporal characteristics. In addition, cathodoluminescence (CL) spectroscopy was employed to examine the intrinsic plasmonic characteristics of the structure. Finite difference time domain (FDTD) simulations showed strong agreement with both PINEM and CL measurements on the spatial and spectral behavior of SPPs. Understanding the spatiotemporal dynamics of SPPs on nanostructures beyond the diffraction limit is crucial for optimizing plasmonic structures for advanced photonic and quantum technologies.

Plasmonics↗

DOE OSTI2021

Optics-on-a-chip for ultrafast manipulation of 350-MHz hard x-ray pulses

Microelectromechanical systems (MEMS) are miniature devices integrated into a vast range of industrial and consumer applications. Optical MEMS are developed for dynamic spatiotemporal control in lightwave manipulation and communication as modulators, switches, multiplexers, spectrometer, etc. However, they have not been shown to function similarly in sub-nm wavelength regimes, namely, with hard x-rays, as high-brilliance pulsed x-rays have proven powerful for addressing challenges in time-domain science, from energy conversion to neurobiological control. While desirable temporal properties of x-ray pulses can be enhanced by optics, conventional x-ray optics are inherently massive in size, hence, never dynamic. We demonstrate highly ultrafast x-ray optics-on-a-chip based on MEMS capable of modulating hard x-ray pulses exceeding 350 MHz, 10 3 × higher than any other mechanical modulator, with a pulse purity >10 6 without compromising the spectral brilliance. Moreover, the timing characteristics of the devices can be tuned on-the-fly to deliver optimal pulse properties to create a host of dynamic x-ray instruments and applications, impossible with traditional optics of 10 9 × bulkier and more massive. The advent of the ultrafast optics-on-a-chip heralds a new paradigm of x-ray photonics, time-domain science, and accelerator diagnostics, especially at not only the future-generation light sources that offer coherent and high-frequency pulses but also lab-based facilities that normally do not offer timing structures.

42 ENGINEERING↗

NASA NTRS2022

Remote Sensing of Coronal Forces During a Solar Prominence Eruption

We present a new methodology—the Keplerian Optical Dynamics Analysis (KODA)—for quantifying the dynamics of erupting magnetic structures in the solar corona. The technique involves adaptive spatiotemporal tracking of propagating intensity gradients and their characterization in terms of time-evolving Keplerian areas swept out by the position vectors of moving plasma blobs. Whereas gravity induces purely ballistic motions consistent with Kepler's second law, noncentral forces such as the Lorentz force introduce nonzero torques resulting in more complex motions. KODA algorithms enable direct evaluation of the line-of-sight component of the net torque density from the image-plane projection of the areal acceleration. The method is applied to the prominence eruption of 2011 June 7, observed by the Solar Dynamics Observatory's Atmospheric Imaging Assembly. Results obtained include quantitative estimates of the magnetic forces, field intensities, and blob masses and energies across a vast region impacted by the postreconnection redistribution of the prominence material. The magnetic pressure and energy are strongly dominant during the early, rising phase of the eruption, while the dynamic pressure and kinetic energy become significant contributors during the subsequent falling phases. Measured intensive properties of the prominence blobs are consistent with those of typical active-region prominences; measured extensive properties are compared with those of the whole pre-eruption prominence and the post-eruption coronal mass ejection of 2011 June 7, all derived by other investigators and techniques. We show that KODA provides valuable information on spatially and temporally dependent characteristics of coronal eruptions that is not readily available via alternative means, thereby shedding new light on the environment and evolution of these solar events.

V M Uritskiy↗

DOE OSTI2026

Flying focus with arbitrary directionality for spatiotemporal control of laser intensity

Flying focus techniques produce laser pulses whose focal points travel at arbitrary, controllable velocities. While this flexibility can enhance a broad range of laser-based applications, existing techniques constrain the motion of the focal point to the propagation direction of the pulse. Here, we introduce a flying focus configuration that decouples the motion of the focus from the propagation direction. Here, a chirped laser pulse focused and diffracted by a diffractive lens and grating creates a focal point that can move both along and transverse to the propagation direction. The focal length of the lens, grating period, and chirp can be tuned to control the direction and velocity of the focus. Simulations demonstrate this control for a holographic configuration suited to high-power pulses, in which two off-axis pump beams with different focal lengths encode the equivalent phase of a chromatic lens and grating in a gas or plasma. For low-power pulses, conventional solid-state or adaptive optics can be used instead. Multi-dimensional control over the focal trajectory enables new configurations for applications, including laser wakefield acceleration of ions, nonlinear Thomson scattering, and surface-plasmon emission of THz radiation.

Classical optics↗