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DOE OSTI2020

The ePix10k 2-megapixel hard X-ray detector at LCLS

The ePix10ka2M (ePix10k) is a new large area detector specifically developed for X-ray free-electron laser (XFEL) applications. The hybrid pixel detector was developed at SLAC to provide a hard X-ray area detector with a high dynamic range, running at the 120 Hz repetition rate of the Linac Coherent Light Source (LCLS). The ePix10k consists of 16 modules, each with 352 × 384 pixels of 100 µm × 100 µm distributed on four ASICs, resulting in a 2.16 megapixel detector, with a 16.5 cm × 16.5 cm active area and ∼80% coverage. The high dynamic range is achieved with three distinct gain settings (low, medium, high) as well as two auto-ranging modes (high-to-low and medium-to-low). Here the three fixed gain modes are evaluated. The resulting dynamic range (from single photon counting to 10000 photons pixel −1 pulse −1 at 8 keV) makes it suitable for a large number of different XFEL experiments. The ePix10k replaces the large CSPAD in operation since 2011. The dimensions of the two detectors are similar, making the upgrade from CSPAD to ePix10k straightforward for most setups, with the ePix10k improving on experimental performance. The SLAC-developed ePix cameras all utilize a similar platform, are tailored to target different experimental conditions and are designed to provide an upgrade path for future high-repetition-rate XFELs. Here the first measurements on this new ePix10k detector are presented and the performance under typical XFEL conditions evaluated during an LCLS X-ray diffuse scattering experiment measuring the 9.5 keV X-ray photons scattered from a thin liquid jet.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗

DOE OSTI2017

Elucidating structural order and disorder phenomena in mullite-type Al{sub 4}B{sub 2}O{sub 9} by automated electron diffraction tomography

The crystal structure and disorder phenomena of Al{sub 4}B{sub 2}O{sub 9}, an aluminum borate from the mullite-type family, were studied using automated diffraction tomography (ADT), a recently established method for collection and analysis of electron diffraction data. Al{sub 4}B{sub 2}O{sub 9}, prepared by sol-gel approach, crystallizes in the monoclinic space group C2/m. The ab initio structure determination based on three-dimensional electron diffraction data from single ordered crystals reveals that edge-connected AlO{sub 6} octahedra expanding along the b axis constitute the backbone. The ordered structure (A) was confirmed by TEM and HAADF-STEM images. Furthermore, disordered crystals with diffuse scattering along the b axis are observed. Analysis of the modulation pattern implies a mean superstructure (AAB) with a threefold b axis, where B corresponds to an A layer shifted by ½a and ½c. Diffraction patterns simulated for the AAB sequence including additional stacking disorder are in good agreement with experimental electron diffraction patterns. - Graphical abstract: Crystal structure and disorder phenomena of B-rich Al{sub 4}B{sub 2}O{sub 9} studied by automated electron diffraction tomography (ADT) and described by diffraction simulation using DISCUS. - Highlights: • Ab-initio structure solution by electron diffraction from single nanocrystals. • Detected modulation corresponding mainly to three-fold superstructure. • Diffuse diffraction streaks caused by stacking faults in disordered crystals. • Observed streaks explained by simulated electron diffraction patterns.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2014

Enhancing optical power of GaN-based light-emitting diodes by nanopatterning on indium tin oxide with tunable fill factor using multiple-exposure nanosphere-lens lithography

In this study, the multiple-exposure nanosphere-lens lithography method utilizing the polystyrene nanospheres with focusing behavior is investigated and introduced to fabricate diverse photonic crystals (PCs) on indium tin oxide to enhance the optical output power of GaN-based light-emitting diode (LED). Simulated results indicate that the focused light intensity decreases with increasing tilted angle due to the shadow effect introduced by adjacent nanospheres. The fill factor of nanopattern is tunable by controlling tilted angles and exposure times. To attain quadruple PC without overlapping patterns, mathematical calculation model is used to define the optimum range of tilted angles. Angular emission patterns and three-dimensional finite-difference time domain simulated results indicate that the enhanced light extraction of PC LEDs results mainly from diffused scattering effects, and the diffraction effects of PC on light extracted efficiency increase with the increase of fill factor. Furthermore, it is confirmed that the multiple PC can extract more light from GaN into air than common PC with same period and fill factor.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗

DOE OSTI2013

Local lattice strains in the system of cubic Zn{sub 0.999}Fe{sub 0.001}S{sub x}Se{sub 1-x} (0 {<=} x {<=} 1) crystals

The structure of cubic Zn{sub 0.999}Fe{sub 0.001}S{sub x}Se{sub 1-x} (0 {<=} x {<=} 1) crystals obtained by vapor-phase chemical transport has been investigated by thermal-neutron diffraction. The diffraction patterns of these crystals are found to exhibit previously unknown diffuse-scattering effects related to local static atomic displacements in the metastable fcc lattice. It is substantiated that the tendency to form polytypes, which is characteristic to a greater extent of zinc sulfide, can be a key factor of instability in the lattice of compounds belonging to the series of anion-substituted solid solutions under study.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

DOE OSTI2015

Ordered domain lateral location, symmetry, and thermal stability in Ge:Si islands

Compositional atomic ordering is a crucial issue in the epitaxial growth of nanoparticles and thin films. Here, we report on a method based on x-ray diffuse scattering close to basis forbidden Bragg reflections to infer the lateral location, the symmetry, and the thermal stability of ordered domains in GeSi dome-shaped islands on Si(001) after growth and during annealing. We observe that atomic ordering does not disappear after annealing, demonstrating that it is a resilient metastable phenomenon.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

DOE OSTI2018

X-Ray Diffraction Analysis of Features of the Crystal Structure of GaN/Al{sub 0.32}Ga{sub 0.68}N HEMT-Heterostructures by the Williamson–Hall Method

The fitting of θ/2θ and ω peaks in X-ray diffraction curves is shown to be most accurate in the case of using an inverse fourth-degree polynomial or probability density function with Student’s distribution (Pearson type VII function). These functions describe well both the highest-intensity central part of the experimental peak and its low-intensity broadened base caused by X-ray diffuse scattering. The mean microdeformation ε and mean vertical domain size D are determined by the Williamson–Hall method for layers of GaN (ε ≈ 0.00006, D ≈ 200 nm) and Al{sub 0.32}Ga{sub 0.68}N (ε = 0.0032 ± 0.0005, D = 24 ± 7 nm). The D value obtained for the Al{sub 0.32}Ga{sub 0.68}N layer is most likely to result from the nominal thickness of this layer, which is 11 nm.

36 MATERIALS SCIENCE↗

DOE OSTI2015

X-ray diffraction study of BaTiO{sub 3} single crystals before and after fast-neutron irradiation

The neutron irradiation of ferroelectrics is efficiently used to form structural states that cannot be obtained by conventional technologies. To date, the effect of neutron irradiation on the structure and properties of BaTiO{sub 3} has been studied for only ceramic materials. We have considered the influence of fast-neutron irradiation (F = 1 × 10{sup 17} cm{sup −2}) on the structure and properties of BaTiO{sub 3} single crystals for the first time. The structural changes occurring in irradiated BaTiO{sub 3} and their correlation with the behavior of dielectric and nonlinear optical characteristics are analyzed with the aid of a specially developed method for taking into account the experimental correction to diffuse scattering. Neutron irradiation to the aforementioned dose retains the polar structure of the material and only slightly changes atomic displacements. The radiationinduced structural changes occur according to the high-temperature type to form a structure similar to the cubic modification of unirradiated BaTiO{sub 3} crystal.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

DOE OSTI2013

The material dependence of temperature measurement resolution in thermal scanning electron microscopy

Thermal scanning electron microscopy is a recently developed temperature mapping technique based on thermal diffuse scattering in electron backscatter diffraction in a scanning electron microscope. It provides nano-scale and non-contact temperature mapping capabilities. Due to the specific temperature sensitive mechanism inherent to this technique, the temperature resolution is highly material dependent. A thorough investigation of what material properties affect the temperature resolution is important for realizing the inherent temperature resolution limit for each material. In this paper, three material dependent parameters-the Debye-Waller B-factor temperature sensitivity, backscatter yield, and lattice constant-are shown to control the temperature resolution.

36 MATERIALS SCIENCE↗

DOE OSTI2017

Features of the structural states of KNbO{sub 3} single crystals before and after fast-neutron irradiation

Neutron irradiation is a unique tool for forming new structural states of ferroelectrics, which cannot be obtained by conventional methods. The inf luence of the irradiation by two doses of fast neutrons (F = 1 × 10{sup 17} and 3 × 10{sup 17} cm{sup –2}) on the structure and properties of KNbO{sub 3} single crystals has been considered for the first time. The developed method for taking into account the experimental correction to the diffuse scattering has been used to analyze the structural changes occurring in KNbO{sub 3} samples at T = 295 K and their correlations with the behavior of dielectric and nonlinear optical characteristics. The irradiation to the aforementioned doses retains the KNbO{sub 3} polar structure, shifting Ð¢{sub Ð}¡ to lower temperatures and significantly affecting only the thermal parameters and microstructure of single crystals. Neutron irradiation with small atomic displacements provides a structure similar to the high-temperature modification of an unirradiated KNbO{sub 3} crystal.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

DOE OSTI2024

Neutron diffraction: a primer

Because of the neutron’s special properties, neutron diffraction may be considered one of the most powerful techniques for structure determination of crystalline and related matter. Neutrons can be released from nuclear fission, from spallation processes, and also from low-energy nuclear reactions, and they can then be used in powder, time-of-flight, texture, single crystal, and other techniques, all of which are perfectly suited to clarify crystal and magnetic structures. With high neutron flux and sufficient brilliance, neutron diffraction also excels for diffuse scattering, for in situ and operando studies as well as for high-pressure experiments of today’s materials. For these, the wave-like neutron’s infinite advantage (isotope specific, magnetic) is crucial to answering important scientific questions, for example, on the structure and dynamics of light atoms in energy conversion and storage materials, magnetic matter, or protein structures. In this primer, we summarize the current state of neutron diffraction (and how it came to be), but also look at recent advances and new ideas, e.g., the design of new instruments, and what follows from that.

36 MATERIALS SCIENCE↗

DOE OSTI2014

Dynamic grazing incidence fast atom diffraction during molecular beam epitaxial growth of GaAs

A Grazing Incidence Fast Atom Diffraction (GIFAD) system has been mounted on a commercial molecular beam epitaxy chamber and used to monitor GaAs growth in real-time. In contrast to the conventionally used Reflection High Energy Electron Diffraction, all the GIFAD diffraction orders oscillate in phase, with the change in intensity related to diffuse scattering at step edges. We show that the scattered intensity integrated over the Laue circle is a robust method to monitor the periodic change in surface roughness during layer-by-layer growth, with oscillation phase and amplitude independent of incidence angle and crystal orientation. When there is a change in surface reconstruction at the start of growth, GIFAD intensity oscillations show that there is a corresponding delay in the onset of layer-by-layer growth. In addition, changes in the relative intensity of different diffraction orders have been observed during growth showing that GIFAD has the potential to provide insight into the preferential adatom attachment sites on the surface reconstruction during growth.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

DOE OSTI2023

Sub‐Nanosecond Reconfiguration of Ferroelectric Domains in Bismuth Ferrite

Abstract Domain switching is crucial for achieving desired functions in ferroic materials that are used in various applications. Fast control of domains at sub‐nanosecond timescales remains a challenge despite its potential for high‐speed operation in random‐access memories, photonic, and nanoelectronic devices. Here, ultrafast laser excitation is shown to transiently melt and reconfigure ferroelectric stripe domains in multiferroic bismuth ferrite on a timescale faster than 100 picoseconds. This dynamic behavior is visualized by picosecond‐ and nanometer‐resolved X‐ray diffraction and time‐resolved X‐ray diffuse scattering. The disordering of stripe domains is attributed to the screening of depolarization fields by photogenerated carriers resulting in the formation of charged domain walls, as supported by phase‐field simulations. Furthermore, the recovery of disordered domains exhibits subdiffusive growth on nanosecond timescales, with a non‐equilibrium domain velocity reaching up to 10 m s −1 . These findings present a new approach to image and manipulate ferroelectric domains on sub‐nanosecond timescales, which can be further extended into other complex photoferroic systems to modulate their electronic, optical, and magnetic properties beyond gigahertz frequencies. This approach could pave the way for high‐speed ferroelectric data storage and computing, and, more broadly, defines new approaches for visualizing the non‐equilibrium dynamics of heterogeneous and disordered materials.

36 MATERIALS SCIENCE↗

DOE OSTI2024

Nanometer-Scale Acoustic Wave Packets Generated by Stochastic Core-Level Photoionization Events

We demonstrate that the absorption of femtosecond hard x-ray pulses excites quasispherical, high-amplitude, and high-wave-vector coherent acoustic phonon wave packets using an all hard-x-ray pump-probe scattering experiment. The time- and momentum-resolved diffuse scattering signal is consistent with an ensemble of 3D strain wave packets induced by the rapid electron cascade dynamics following photoionization at uncorrelated excitation centers. We quantify key parameters of this process, including the localization size of the stress field and the photon energy conversion efficiency into elastic energy. The parameters are determined by the photoelectron and Auger electron cascade dynamics, as well as the electron-phonon interaction. In particular, we obtain the localization size of the observed strain wave packet to be 1.5 and 2.5 nm for bulk SrTiO 3 and KTaO 3 single crystals, respectively. The results provide crucial information on the mechanism of x-ray energy deposition into matter and shed light on the shortest collective length scales accessible to coherent acoustic phonon generation using x-ray excitation. Published by the American Physical Society 2024

36 MATERIALS SCIENCE↗

NASA NTRS1992

Physics of pitch angle scattering and velocity diffusion. I - Theory

A general theory for the pitch angle scattering and velocity diffusion of particles in the field of a spectrum of waves in a magnetized plasma is presented. The test particle theory is used to analyze the particle motion. The form of diffusion surfaces is examined, and analytical expressions are given for the resonance width and bounce frequency. The resonance widths are found to vary strongly as a function of harmonic number. The resulting diffusion can be quite asymmetric with respect to pitch angle of 90 deg. The conditions for the onset of pitch angle scattering and energy diffusion are explained in detail. Some of the known shortcomings of the standard quasi-linear theory are also addressed, and ways to overcome them are shown. In particular, the often stated quasi-linear gap at 90 deg is found to exist only under very special cases. For instance, oblique wave propagation can easily remove the gap. The conditions for the existence of the gap are described in great detail. A new diffusion equation which takes into account the finite resonance widths is also discussed. The differences between this new theory and the standard resonance broadening theory is explained.

Karimabadi, H.↗

NASA NTRS1991

Instabilities of line-driven stellar winds. V - Effect of an optically thick continuum

Earlier analyses of the linear instability of line-driven stellar winds are extended to the case, relevant to Wolf-Rayet stars, in which the continuum remains optically thick well above the sonic point. It is found that an optically thick flow driven by pure scattering lines is stabilized by the drag effect of the diffuse, scattered radiation. However, even a relatively small photon destruction probability can cause a flow with continuum optical thickness much greater than 1 to remain unstable, with a given growth rate. The implications of these results for the variability characteristics of winds from Wolf-Rayet stars are briefly discussed.

Owocki, Stanley P.↗

DOE OSTI2017

LUNUS, Version 0.1a

LUNUS software for generating 3D maps of diffuse scattering from macromolecular X-ray crystallography diffraction images. A set of tools needed for advanced refinement of crystal structures and crystallographic charge density models. Includes tools for processing X--ray diffraction images, charge density maps, and structure factors for analysis of diffuse X-ray scattering and charge density variations in crystallography. Specific methods include: elementary algebraic operations on images and 3D lattices; fourier transform of images and 3D lattices; image processing to measure diffuse intensity; crystallographic refinement; and 3D integration of diffuse intensity.

Wall, Michael↗

DOE OSTI2017

LUNUS, Version 0.1a

Wall, Michael↗

NASA NTRS1995

Terrain classification using circular polarimetric features

Conventional representations of polarization response are referred to a horizontally and vertically polarized basis. Recent studies by Freeman and Durden, van Zyl, and others suggest that alternative polarimetric features which more easily resolve the contributions of simple scattering mechanisms such as odd-bounce, even-bounce, and diffuse scattering could offer several advantages in terrain classification. The circular polarization covariance matrix is a potential source of such features. In this paper, we derive its relationship to the Stokes matrix, describe some of its properties, and compare the utility of linear and circular polarimetric features in classifying an AIRSAR scene containing urban, park, and ocean terrain.

Michelson, David G.↗