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At least 1,747 records · Page 97

Probing lattice defects in crystalline battery cathode using hard X-ray nanoprobe with data-driven modeling

Lattice defects, e.g., dislocations and grain boundaries, critically impact the properties of crystalline battery cathode materials. A longstanding challenge is to probe the meso–scale heterogeneity and evolution of lattice defects with sensitivity to atomic-scale details. Herein, we tackle this issue with a unique combination of X-ray nanoprobe diffractive imaging and advanced machine learning techniques. The domains with different lattice defect configuration within a single-crystalline LiCoO2 cathode particle are faithfully revealed using our approach. We further visualize the rearrangement of grain boundaries and local crystallinity upon mild thermal annealing. Furthermore, these results pave a direct way to the understanding of crystalline battery materials’ response under external stimuli with high fidelity, which provides valuable empirical guidance to defect-engineering strategies for improving the cathode materials against aggressive battery operation.

36 MATERIALS SCIENCE↗

Chemical partitioning for the Co--Pr system: First-principles, experiments and energetic calculations to investigate the hard magnetic phase

Co 5 Pr-D2 d is promising permanent magnet. Due to its peritectic formation feature, there is a synthetic challenge to produce single Co 5 Pr-D2 d phase. The object of our study is to assess thermodynamic pathways for crystalline phases under far-from-equilibrium conditions by combining first-principles calculations and experimental measurements into a robust description of the thermodynamic behavior. The energetic calculations, temperature and time dependent phase selections are predicted under varying degrees of chemical partitioning. Our calculation to assess the chemical partitioning-temperatures indicates that the major magnetic compounds: Co 17 Pr 2 -α, Co 5 Pr-D2 d , Co 19 Pr 5 -β, and Co 7 Pr 2 -χ form from a congruent manner to eutectic reactions with decreasing cooling rate. The compositions of the compounds from these highly driven liquids can be far from equilibrium.

36 MATERIALS SCIENCE↗

Correlation of precipitate evolution with Vickers hardness in Haynes® 282® superalloy: In-situ high-energy SAXS/WAXS investigation

Here, the aim of this work is to characterise precipitation kinetics in Haynes® 282® superalloy using high-energy Small Angle X-ray Scattering (SAXS) together with Wide Angle X-ray Scattering (WAXS). The phases identified by WAXS include: γ (matrix), γ' (hardening precipitates), MC (metallic carbides), and M 23 C 6 /M 6 C (secondary metallic carbides). The γ'-precipitates are spheroids with a diameter of several nanometres, depending on temperature and aging time. From the SAXS data quantitative parameters such as volume fraction, number density and inter-particle distance were determined and correlated with Vickers microhardness measurements performed ex situ . The strengthening components associated with precipitates and solid solutions were separated using the measured Vickers microhardness and SAXS model parameters. A power law dependence between strengthening attributable to the precipitates and the product of volume fraction and mean precipitate radius was found. The solid solution strengthening component was found to be correlated with the repulsion/diffusion zone width around the precipitates.

36 MATERIALS SCIENCE↗

Radiation hardness and precision timing study of silicon detectors for the CMS High Granularity Calorimeter (HGC)

The high luminosity upgraded LHC or Phase-II is expected to increase the instantaneous luminosity by a factor of 10 beyond the LHC's design value, expecting to deliver 250 fb –1 per year for a further 10 years of operation. Under these conditions the performance degradation due to integrated radiation dose will need to be addressed. The CMS collaboration is planning to upgrade the forward calorimeters. The replacement is called the High Granularity Calorimeter (HGC) and it will be realized as a sampling calorimeter with layers of silicon detectors interleaved. The sensors will be realized as pad detectors with sizes of less that ~1.0 cm 2 and an active thickness between 100 and 300 μm depending on the position, respectively, the expected radiation levels. For an integrated luminosity of 3000 fb –1 , the electromagnetic calorimetry will sustain integrated doses of 1.5 MGy (150 Mrads) and neutron fluences up to 10 16 neq/cm 2 . A radiation tolerance study after neutron irradiation of 300, 200, and 100 μm n-on-p and p-on-n silicon pads irradiated to fluences up to 1.6×10 16 neq/cm 2 is presented. In this work, the properties of these diodes studied before and after irradiation were leakage current, capacitance, charge collection efficiency, annealing effects and timing capability. The results of these measurements validate these sensors as candidates for the HGC system.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗

Zone Plates for Hard X-Ray FEL Radiation

We investigated theoretically the use of zone plates for the focusing of the European X-ray Free Electron Laser (XFEL). In a finite-element simulation the heat load on zone plates placed in the high intensity x-ray beam was simulated for four different zone plate materials: gold, iridium, tungsten, and CVD diamond. The main result of the calculations is that all zone plates remain below the melting temperature throughout a full XFEL pulse train of 3000 pulses. However, if the zone plate is placed in the direct beam it will experience large and rapid temperature fluctuations on the order of 300 K. The situation is relaxed if the optic is placed behind a monochromator and the fluctuations are reduced to around 20 K. Besides heat load, the maximization of the total efficiency of the complete optical system is an important issue. We calculated the efficiency of different zone plates and monochromator systems and found that the final beam size of the XFEL in combination with its monochromaticity will be important parameters.

43 PARTICLE ACCELERATORS↗

Hard X-ray Phase-Contrast Tomographic Nanoimaging

Synchrotron-based full-field tomographic microscopy established itself as a tool for noninvasive investigations. Many beamlines worldwide routinely achieve micrometer spatial resolution while the isotropic 100-nm barrier is reached and trespassed only by few instruments, mainly in the soft x-ray regime. We present an x-ray, full-field microscope with tomographic capabilities operating at 10 keV and with a 3D isotropic resolution of 144 nm recently installed at the TOMCAT beamline of the Swiss Light Source. Custom optical components, including a beam-shaping condenser and phase-shifting dot arrays, were used to obtain an ideal, aperture-matched sample illumination and very sensitive phase-contrast imaging. The instrument has been successfully used for the nondestructive, volumetric investigation of single, unstained cells.

43 PARTICLE ACCELERATORS↗

New Nanoscale Imaging with a Simple Hard X-Ray Nanoslit

A simple and new procedure to measure the optimal intensity distribution of an x-ray wavefield in nanoscale resolution is proposed. A heavy-metal wire can work as a ''nanoslit'' with a nanoscale aperture size. Its basic function can be described simply with geometrical optics using total reflection. The further function is investigated with numerical calculation of a diffraction edge. In the experiment, Fresnel fringes generated by a rectangular aperture were measured by using a 300-{mu}m platinum wire as the nanoslit. Its high potential use in imaging applications is discussed.

07 ISOTOPE AND RADIATION SOURCES↗

Hard x-ray or gamma ray laser by a dense electron beam

A dense electron beam propagating through a laser undulator can radiate a coherent x-ray or gamma ray. This lasing scheme is studied with the Landau damping theory. The analysis suggests that, with currently available physical parameters, coherent gamma rays of up to 50 keV can be generated. The electron quantum diffraction suppresses the free electron laser action, which limits the maximum radiation.

43 PARTICLE ACCELERATORS↗

Quantitative measurement of hard x-ray spectra for high intensity laser produced plasma

X-ray line spectra ranging from 17 to 77 keV were quantitatively measured with a Laue spectrometer, composed of a cylindrically curved crystal and a detector. Either a visible CCD detector coupled with a CsI phosphor screen or an imaging plate can be chosen, depending on the signal intensities and exposure times. The absolute sensitivity of the spectrometer system was calibrated using pre-characterized laser-produced x-ray sources and radioisotopes. The integrated reflectivity for the crystal is in good agreement with predictions by an open code for x-ray diffraction. The energy transfer efficiency from incident laser beams to hot electrons, as the energy transfer agency for specific x-ray line emissions, is derived as a consequence of this work.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗

Towards nanometer period gratings for hard x-ray phase-contrast imaging

Transmission grating-based x-ray interferometers have been developed into wide-field imaging devices that are sensitive to x-ray refraction and diffraction in the sample. While current grating designs rely on UV and x-ray lithography processes to produce periodic vertical structures, it becomes prohibitively difficult to make the grating periods below 1 - 2 microns due to the high aspect ratios of the structures. Since the phase-contrast sensitivity is inversely related to the grating period, we describe a new grating design for sub-micron to nanometer grating periods. In this design, multiple bi-layers of two alternating materials are deposited on a stair like substrate, and mostly on the floor surfaces of the steps only. The incident x-ray beam is parallel to the planes of the layers (side illumination). Thus, the multilayer structure on each step serves as a micro grating whose grating period is the thickness of a bi-layer. The array of micro gratings over the whole length of the stair can act as a single continuous grating, when certain continuity conditions between neighboring steps are met. Since the layer thickness can be as small as tens of nanometers, as has been demonstrated in multilayer x-ray zone plates, this design allows nanometer grating periods over large grating areas. Here we describe a prototype intensity grating of 440 nm period. We show x-ray projection images of the grating which were obtained by contact lithography.

36 MATERIALS SCIENCE↗

High-resolution and high-sensitivity phase-contrast imaging by focused hard x-ray ptychography with a spatial filter

We demonstrate high-resolution and high-sensitivity x-ray phase-contrast imaging of a weakly scattering extended object by scanning coherent diffractive imaging, i.e., ptychography, using a focused x-ray beam with a spatial filter. We develop the x-ray illumination optics installed with the spatial filter to collect coherent diffraction patterns with a high signal-to-noise ratio. We quantitatively visualize the object with a slight phase shift ({approx}{lambda}/320) at spatial resolution better than 17 nm in a field of view larger than {approx}2 Multiplication-Sign 2{mu}m{sup 2}. The present coherent method has a marked potential for high-resolution and wide-field-of-view observation of weakly scattering objects such as biological soft tissues.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗

High-resolution chemical imaging of gold nanoparticles using hard x-ray ptychography

We combine resonant scattering with (ptychographic) scanning coherent diffraction microscopy to determine the chemical state of gold nanoparticles with high spatial resolution. Ptychographic images of the sample are recorded for a series of energies around the gold L{sub 3} absorption edge. From these data, chemical information in the form of absorption and resonant scattering spectra is reconstructed at each location in the sample. For gold nanoparticles of about 100 nm diameter, a spatial resolution of about 20-30 nm is obtained. In the future, this microscopy approach will open the way to operando studies of heterogeneous catalysts on the nanometer scale.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

Effects of electron recirculation on a hard x-ray source observed during the interaction of a high intensity laser pulse with thin Au targets

The interaction of a high intensity laser pulse on the preplasma of a high-Z solid target produced by the pulse's pedestal generates high-energy electrons. These electrons subsequently penetrate inside the solid target and produce bremsstrahlung photons, generating an x-ray source which can be used for photonuclear studies or to radiograph high area density objects. The source characteristics are compared for targets with thin (20 μm) and thick (100 μm) Au foils on the Omega EP laser at Laboratory for Laser Energetics. Simulations using the particle-in-cell code CALDER show that for a 20 μm thickness Au target, electrons perform multiple round-trips in the target under the effect of the laser ponderomotive potential and the target electrostatic potential. These relativistic electrons have random transverse displacements, with respect to the target normal, attributed to electrostatic fluctuation fields. As a result, the x-ray spot size is increased by a factor 2 for thin target compared to thick targets, in agreement with experimental results. In addition, the computed doses agree with the measured ones provided that electron recirculation in the thin target is taken into account. A dose increase by a factor 1.7 is then computed by allowing for recirculation. In the 100 μm target case, on the other hand, this effect is found to be negligible.

07 ISOTOPE AND RADIATION SOURCES↗

Compact focusing spectrometer: Visible (1 eV) to hard x-rays (200 keV)

A low-cost spectrometer that covers a wide range of photon energies can be useful to teach spectroscopy, and for simple, rapid measurements of the photon spectrum produced by small plasma devices. The spectrometer here achieves its wide range, nominally from 1 eV to 200 keV, with a series of spherically and cylindrically bent gratings or crystals that all have the same shape and the same radius of curvature; they are complemented by matching apertures and diagnostics on the Rowland circle that serves as the circular part of the spectrometer's vacuum vessel. Spectral lines are easily identified with software that finds their positions from the dispersion of each diffractive element and the known energies of the lines.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗

Experimental study for the feasibility of using hard x-rays for micro-XRF analysis of multilayered metals

Application of polycapillary optical systems to improve a spatial resolution for the μ-XRF analysis by focusing a primary x-ray beam and/or by collecting fluorescence emission is well known. The challenge is to optimize them in combination with x-ray source for exciting K-lines above 20 keV that could allow characterization of many materials composed by heavy elements. To pursue this goal, preliminary studies on possible polycapillary lens employment in thickness determination for multilayer metal materials will be presented in this work. In this paper, the results of first attempts of integrating PyMCA with Monte Carlo simulation code (XMI-MSIM) that takes into account the secondary fluorescence effects on quantitative analysis of homogeneous matrices, in particular, metal alloys, are presented.

36 MATERIALS SCIENCE↗

Hard x-ray nanofocusing by refractive lenses of constant thickness

In order to focus light or x rays, the thickness of a refractive lens is typically varied over its aperture. Here, we present a refractive x-ray lens made of lamellae of constant thickness, the refractive lamellar lens. Refractive power is created by a specific bending of the lamellae rather than by a concave lens profile. This very special design has the technological advantage that materials like sapphire or diamond can be used to make lenses by coating techniques. A first lens prototype focused x rays with a photon energy E = 15.25 keV to a lateral beam size of 164 nm × 296 nm full width at half maximum.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

Hard X-ray nanofocusing using adaptive focusing optics based on piezoelectric deformable mirrors

An adaptive Kirkpatrick–Baez mirror focusing optics based on piezoelectric deformable mirrors was constructed at SPring-8 and its focusing performance characteristics were demonstrated. By adjusting the voltages applied to the deformable mirrors, the shape errors (compared to a target elliptical shape) were finely corrected on the basis of the mirror shape determined using the pencil-beam method, which is a type of at-wavelength figure metrology in the X-ray region. The mirror shapes were controlled with a peak-to-valley height accuracy of 2.5 nm. A focused beam with an intensity profile having a full width at half maximum of 110 × 65 nm (V × H) was achieved at an X-ray energy of 10 keV.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗