Increased spatial coherence length from an asymmetric crystal reflection at grazing exit.

Coherent X-ray imaging is an active field at synchrotron sources. The images rely on the available coherent flux over a limited field of view. At many synchrotron beamlines a double-crystal monochromator (DCM) is employed in a standard nondispersive arrangement. For coherent diffraction imaging it is advantageous to increase the available field of view by increasing the spatial coherence length (SCL) of a beam exiting such a DCM. Here, Talbot interferometry data together with ray-tracing simulations for a (+ - - +) four-reflection experimental arrangement are presented, wherein the first two reflections are in the DCM and the final fourth reflection is asymmetric at grazing exit. Analyses of the interferometry data combined with the simulations show that compared with the beam exiting the DCM a gain of 76% in the SCL was achieved, albeit with a factor of 20 reduction in flux density, which may not be a severe penalty at a synchrotron beamline. Previous efforts reported in the literature to increase the SCL that employed asymmetric crystal diffraction at grazing incidence are also discussed. A much reduced SCL is found presently in simulations wherein the same asymmetric crystal is set for grazing incidence instead of grazing exit. In addition, the present study is compared and contrasted with two other means of increasing the SCL. These are (i) focusing the beam onto an aperture to act as a secondary source, and (ii) allowing the beam to propagate in vacuum an additional distance along the beamline.

Multislice forward modeling of coherent surface scattering imaging on surface and interfacial structures.

To study nanostructures on substrates, surface-sensitive reflection-geometry scattering techniques such as grazing incident small angle X-ray scattering are commonly used to yield an averaged statistical structural information of the surface sample. Grazing incidence geometry can probe the absolute three-dimensional structural morphology of the sample if a highly coherent beam is used. Coherent surface scattering imaging (CSSI) is a powerful yet non-invasive technique similar to coherent X-ray diffractive imaging (CDI) but performed at small angles and grazing-incidence reflection geometry. A challenge with CSSI is that conventional CDI reconstruction techniques cannot be directly applied to CSSI because the Fourier-transform-based forward models cannot reproduce the dynamical scattering phenomenon near the critical angle of total external reflection of the substrate-supported samples. To overcome this challenge, we have developed a multislice forward model which can successfully simulate the dynamical or multi-beam scattering generated from surface structures and the underlying substrate. The forward model is also demonstrated to be able to reconstruct an elongated 3D pattern from a single shot scattering image in the CSSI geometry through fast-performing CUDA-assisted PyTorch optimization with automatic differentiation.

High-energy micrometre-scale pixel direct conversion X-ray detector.

The objective of this work was to fabricate and characterize a new X-ray imaging detector with micrometre-scale pixel dimensions (7.8 µm) and high detection efficiency for hard X-ray energies above 20 keV. A key technology component consists of a monolithic hybrid detector built by direct deposition of an amorphous selenium film on a custom designed CMOS readout integrated circuit. Characterization was carried out at the synchrotron beamline 1-BM-B at the Advanced Photon Source of Argonne National Laboratory. The direct conversion detector demonstrated micrometre-scale spatial resolution with a 63 keV modulation transfer function of 10% at Nyquist frequency. In addition, spatial resolving power down to 8 µm was determined by imaging a transmission bar target at 21 keV. X-ray signal linearity, responsivity and lag were also characterized in the same energy range. Finally, phase contrast edge enhancement was observed in a phase object placed in the beam path. This amorphous selenium/CMOS detector technology can address gaps in commercially available X-ray detectors which limit their usefulness for existing synchrotron applications at energies greater than 50 keV; for example, phase contrast tomography and high-resolution imaging of nanoscale lattice distortions in bulk crystalline materials using Bragg coherent diffraction imaging. The technology will also facilitate the creation of novel synchrotron imaging applications for X-ray energies at or above 20 keV.

Broadband X-ray ptychography using multi-wavelength algorithm.

Ptychography is a rapidly developing scanning microscopy which is able to view the internal structures of samples at a high resolution beyond the illumination size. The achieved spatial resolution is theoretically dose-limited. A broadband source can provide much higher flux compared with a monochromatic source; however, it conflicts with the necessary coherence requirements of this coherent diffraction imaging technique. In this paper, a multi-wavelength reconstruction algorithm has been developed to deal with the broad bandwidth in ptychography. Compared with the latest development of mixed-state reconstruction approach, this multi-wavelength approach is more accurate in the physical model, and also considers the spot size variation as a function of energy due to the chromatic focusing optics. Therefore, this method has been proved in both simulation and experiment to significantly improve the reconstruction when the source bandwidth, illumination size and scan step size increase. It is worth mentioning that the accurate and detailed information of the energy spectrum for the incident beam is not required in advance for the proposed method. Further, we combine multi-wavelength and mixed-state approaches to jointly solve temporal and spatial partial coherence in ptychography so that it can handle various disadvantageous experimental effects. The significant relaxation in coherence requirements by our approaches allows the use of high-flux broadband X-ray sources for high-efficient and high-resolution ptychographic imaging.

Small Bragg-plane slope errors revealed in synthetic diamond crystals.

Wavefront-preserving X-ray diamond crystal optics are essential for numerous applications in X-ray science. Perfect crystals with flat Bragg planes are a prerequisite for wavefront preservation in Bragg diffraction. However, this condition is difficult to realize in practice because of inevitable crystal imperfections. Here, X-ray rocking curve imaging is used to study the smallest achievable Bragg-plane slope errors in the best presently available synthetic diamond crystals and how they compare with those of perfect silicon crystals. It is shown that the smallest specific slope errors in the best diamond crystals are about 0.08 (3) µrad mm-2. These errors are only 50% larger than the 0.05 (2) µrad mm-2 specific slope errors measured in perfect silicon crystals. High-temperature annealing at 1450°C of almost flawless diamond crystals reduces the slope errors very close to those of silicon. Further investigations are in progress to establish the wavefront-preservation properties of these crystals.

Multislice does it all-calculating the performance of nanofocusing X-ray optics.

We describe an approach to calculating the optical performance of a wide range of nanofocusing X-ray optics using multislice scalar wave propagation with a complex X-ray refractive index. This approach produces results indistinguishable from methods such as coupled wave theory, and it allows one to reproduce other X-ray optical phenomena such as grazing incidence reflectivity where the direction of energy flow is changed significantly. Just as finite element analysis methods allow engineers to compute the thermal and mechanical responses of arbitrary structures too complex to model by analytical approaches, multislice propagation can be used to understand the properties of the real-world optics of finite extent and with local imperfections, allowing one to better understand the limits to nanoscale X-ray imaging.

Near infrared overtone (vOH = 2 ← 0) spectroscopy of Ne-H2O clusters.

Vibrationally state selective overtone spectroscopy and dynamics of weakly bound Ne-H2O complexes (D0(para) = 31.67 cm-1, D0(ortho) = 34.66 cm-1) are reported for the first time, based on near infrared excitation of van der Waals cluster bands correlating with vOH = 2 ← 0 overtone transitions (|02-⟩←|00+⟩ and |02+⟩←|00+⟩) out of the ortho (101) and para (000) internal rotor states of the H2O moiety. Quantum theoretical calculations for nuclear motion on a high level ab initio potential energy surface (CCSD(T)/VnZ-f12 (n = 3,4), corrected for basis set superposition error and extrapolated to the complete basis set limit) are employed for assignment of Σ←Σ,Π←Σ, and Σâ†Π infrared bands in the overtone spectra, where Σ(K = 0) and Π (K = 1) represent approximate projections (K) of the body angular momentum along the Ne-H2O internuclear axis. End-over-end tumbling of the ortho Ne-H2O cluster is evident via rotational band contours observed, with band origins and rotational progressions in excellent agreement with ab initio frequency and intensity predictions. A clear Q branch in the corresponding |02+⟩fΠ(111)←eΣ(000) para Ne-H2O spectrum provides evidence for a novel e/f parity-dependent metastability in these weakly bound clusters, in agreement with ab initio bound state calculations and attributable to the symmetry blocking of an energetically allowed channel for internal rotor predissociation. Finally, Boltzmann analysis of the rotational spectra reveals anomalously low jet temperatures (Trot ≈ 4(1) K), which are attributed to "evaporative cooling" of weakly bound Ne-H2O clusters and provide support for similar cooling dynamics in rare gas-tagging studies.

Hard x-ray spectroscopy and imaging by a reflection zone plate in the presence of astigmatism.

The feasibility of an off-axis x-ray reflection zone plate to perform wavelength-dispersive spectroscopy, on-axis point focusing, and two-dimensional imaging is demonstrated by means of one and the same diffractive optical element (DOE) at a synchrotron radiation facility. The resolving power varies between 3×101 and 4×102 in the range of 7.6 keV to 9.0 keV, with its maximum at the design energy of 8.3 keV. This result is verified using an adjustable entrance slit, by which horizontal (H) and vertical (V) focusing to 0.85 µm(H) and 1.29 µm(V) is obtained near the sagittal focal plane of the astigmatic configuration. An angular and axial scan proves an accessible field of view of at least 0.6 arcmin × 0.8 arcmin and a focal depth of ±0.86 mm. Supported by the grating efficiency of around 17.5% and a very short pulse elongation, future precision x-ray fluorescence and absorption studies of transition metals at their K-edge on an ultrashort timescale could benefit from our findings.

Fresnel zone plate stacking in the intermediate field for high efficiency focusing in the hard X-ray regime.

Focusing efficiency of Fresnel zone plates (FZPs) for X-rays depends on zone height, while the achievable spatial resolution depends on the width of the finest zones. FZPs with optimal efficiency and sub-100-nm spatial resolution require high aspect ratio structures which are difficult to fabricate with current technology especially for the hard X-ray regime. A possible solution is to stack several zone plates. To increase the number of FZPs within one stack, we first demonstrate intermediate-field stacking and apply this method by stacks of up to five FZPs with adjusted diameters. Approaching the respective optimum zone height, we maximized efficiencies for high resolution focusing at three different energies, 10, 11.8, and 25 keV.

Probing transverse coherence of x-ray beam with 2-D phase grating interferometer.

Transverse coherence of the x-ray beam from a bending magnet source was studied along multiple directions using a 2-D π/2 phase grating by measuring interferogram visibilities at different distances behind the grating. These measurements suggest that the preferred measuring orientation of a 2-D checkerboard grating is along the diagonal directions of the square blocks, where the interferograms have higher visibility and are not sensitive to the deviation of the duty cycle of the grating period. These observations are verified by thorough wavefront propagation simulations. The accuracy of the measured coherence values was also validated by the simulation and analytical results obtained from the source parameters. In addition, capability of the technique in probing spatially resolved local transverse coherence is demonstrated.

Angular spectrum simulation of X-ray focusing by Fresnel zone plates.

A computing simulation routine to model any type of circularly symmetric diffractive X-ray element has been implemented. The wavefield transmitted beyond the diffractive structures is numerically computed by the angular spectrum propagation method to an arbitrary propagation distance. Cylindrical symmetry is exploited to reduce the computation and memory requirements while preserving the accuracy of the numerical calculation through a quasi-discrete Hankel transform algorithm, an approach described by Guizar-Sicairos & Gutierrez-Vega [J. Opt. Soc. Am. A, (2004), 21, 53-58]. In particular, the code has been used to investigate the requirements for the stacking of two high-resolution Fresnel zone plates with an outermost zone width of 20 nm.

Particulate emissions calculations from fall tillage operations using point and remote sensors.

Soil preparation for agricultural crops produces aerosols that may significantly contribute to seasonal atmospheric particulate matter (PM). Efforts to reduce PM emissions from tillage through a variety of conservation management practices (CMPs) have been made, but the reductions from many of these practices have not been measured in the field. A study was conducted in California's San Joaquin Valley to quantify emissions reductions from fall tillage CMP. Emissions were measured from conventional tillage methods and from a "combined operations" CMP, which combines several implements to reduce tractor passes. Measurements were made of soil moisture, bulk density, meteorological profiles, filter-based total suspended PM (TSP), concentrations of PM with an equivalent aerodynamic diameter ≤10 µm (PM) and PM with an equivalent aerodynamic diameter ≤2.5 µm (PM), and aerosol size distribution. A mass-calibrated, scanning, three-wavelength light detection and ranging (LIDAR) procedure estimated PM through a series of algorithms. Emissions were calculated via inverse modeling with mass concentration measurements and applying a mass balance to LIDAR data. Inverse modeling emission estimates were higher, often with statistically significant differences. Derived PM emissions for conventional operations generally agree with literature values. Sampling irregularities with a few filter-based samples prevented calculation of a complete set of emissions through inverse modeling; however, the LIDAR-based emissions dataset was complete. The CMP control effectiveness was calculated based on LIDAR-derived emissions to be 29 ± 2%, 60 ± 1%, and 25 ± 1% for PM, PM, and TSP size fractions, respectively. Implementation of this CMP provides an effective method for the reduction of PM emissions.

Digital autofocusing of a coded-aperture Laue diffraction microscope.

To provide optimal depth resolution with a coded-aperture Laue diffraction microscope, an accurate position of the coded-aperture and its scanning geometry need to be known. However, finding the geometry by trial and error is a time-consuming and often challenging process because of the large number of parameters involved. In this paper, we propose an optimization approach to automate the focusing process after data is collected. We demonstrate the robustness and efficiency of the proposed approach with experimental data taken at a synchrotron facility.

Probing three-dimensional mesoscopic interfacial structures in a single view using multibeam X-ray coherent surface scattering and holography imaging.

Visualizing surface-supported and buried planar mesoscale structures, such as nanoelectronics, ultrathin-film quantum dots, photovoltaics, and heterogeneous catalysts, often requires high-resolution X-ray imaging and scattering. Here, we discovered that multibeam scattering in grazing-incident reflection geometry is sensitive to three-dimensional (3D) structures in a single view, which is difficult in conventional scattering or imaging approaches. We developed a 3D finite-element-based multibeam-scattering analysis to decode the heterogeneous electric-field distribution and to faithfully reproduce the complex scattering and surface features. This approach further leads to the demonstration of hard-X-ray Lloyd's mirror interference of scattering waves, resembling dark-field, high-contrast surface holography under the grazing-angle scattering conditions. A first-principles calculation of the single-view holographic images resolves the surface patterns' 3D morphology with nanometer resolutions, which is critical for ultrafine nanocircuit metrology. The holographic method and simulations pave the way for single-shot structural characterization for visualizing irreversible and morphology-transforming physical and chemical processes in situ or operando.

Quantitative X-ray wavefront measurements of Fresnel zone plate and K-B mirrors using phase retrieval.

A scanning coherent diffraction imaging method was used to reconstruct the X-ray wavefronts produced by a Fresnel zone plate (FZP) and by Kirkpatrick-Baez (KB) focusing mirrors. The ptychographical measurement was conducted repeatedly by placing a lithographed test sample at different defocused planes. The wavefronts, recovered by phase-retrieval at well-separated planes, show good consistency with numerical propagation results, which provides a self-verification. The validity of the obtained FZP wavefront was further confirmed with theoretical predictions.

High-Resolution Scanning Coded-Mask-Based X-ray Multi-Contrast Imaging and Tomography.

Near-field X-ray speckle tracking has been used in phase-contrast imaging and tomography as an emerging technique, providing higher contrast images than traditional absorption radiography. Most reported methods use sandpaper or membrane filters as speckle generators and digital image cross-correlation for phase reconstruction, which has either limited resolution or requires a large number of position scanning steps. Recently, we have proposed a novel coded-mask-based multi-contrast imaging (CMMI) technique for single-shot measurement with superior performance in efficiency and resolution compared with other single-shot methods. We present here a scanning CMMI method for the ultimate imaging resolution and phase sensitivity by using a coded mask as a high-contrast speckle generator, the flexible scanning mode, the adaption of advanced maximum-likelihood optimization to scanning data, and the multi-resolution analysis. Scanning CMMI can outperform other speckle-based imaging methods, such as X-ray speckle vector tracking, providing higher quality absorption, phase, and dark-field images with fewer scanning steps. Scanning CMMI is also successfully demonstrated in multi-contrast tomography, showing great potentials in high-resolution full-field imaging applications, such as in vivo biomedical imaging.

Management of a Periodontal Patient With Dermatomyositis: A Case Report.

INTRODUCTION: Dermatomyositis is an uncommon inflammatory disease marked by muscle and joint weakness with skin rash. Dermatomyositis affects adults and children, with higher prevalence for females aged 40 to 60 years. Most common oral lesions include mucosal edema, erythema, and telangiectasia. CASE PRESENTATION: A 51-year-old white female with an unremarkable medical history presented for periodontal evaluation in 2010. She reported a 6-month history of gingival inflammation and skin irritation on her hands and a rash on the center of her chest and forehead. Other complaints included fatigue, hot flashes, decreased appetite, and weight loss. Periodontal examination revealed generalized acute marginal erythema, with localized slight incipient bone loss. Oral hygiene was deemed good to fair. Oral hygiene instructions were reviewed and a prescription for chlorhexidine gluconate was given. The patient was then referred to an allergist and dermatologist where a diagnosis of dermatomyositis was made. After the initial diagnosis, localized scaling and root planing was performed using local anesthetic. The patient was managed medically using prednisone, mycophenolate mofetil, and methotrexate and a 3-month periodontal maintenance recall interval. The patient remained stable over an 8-year period. CONCLUSIONS: Dermatomyositis is an uncommon inflammatory disease that requires medical and dental teams for proper diagnosis and management. Although the condition is chronic in nature with no definitive cure, signs, and symptoms can be managed with steroids and immunosuppressants to delay progression of the disease and improve quality of life for the patient.

Fast X-ray Nanotomography with Sub-10 nm Resolution as a Powerful Imaging Tool for Nanotechnology and Energy Storage Applications.

In the last decade, transmission X-ray microscopes (TXMs) have come into operation in most of the synchrotrons worldwide. They have proven to be outstanding tools for non-invasive ex and in situ 3D characterization of materials at the nanoscale across varying range of scientific applications. However, their spatial resolution has not improved in many years, while newly developed functional materials and microdevices with enhanced performances exhibit nanostructures always finer. Here, optomechanical breakthroughs leading to fast 3D tomographic acquisitions (85 min) with sub-10 nm spatial resolution, narrowing the gap between X-ray and electron microscopy, are reported. These new achievements are first validated with 3D characterizations of nanolithography objects corresponding to ultrahigh-aspect-ratio hard X-ray zone plates. Then, this powerful technique is used to investigate the morphology and conformality of nanometer-thick film electrodes synthesized by atomic layer deposition and magnetron sputtering deposition methods on 3D silicon scaffolds for electrochemical energy storage applications.

Effects of surface undulations on asymmetric X-ray diffraction: a rocking-curve topography study.

The results are reported of an X-ray diffraction study of an Si crystal designed and fabricated for very asymmetric diffraction from the 333 reflection for X-ray energies of 8.100 and 8.200 keV. A crystal with an asymmetry angle of 46 ±â€…0.1° between the surface and the (111) planes was studied. The grazing angles of incidence were near 1.08 and 0.33° for these two energies, respectively. Features arising from surface undulations were not observed at 8.100 keV, but were observed at 8.200 keV. The results at 8.100 keV allow an alternative explanation based on strain near the surface to be ruled out. Topographic images were obtained as a function of rocking angle, and in the case of 8.200 keV the surface morphology is evident. The results are found to be in agreement with dynamical X-ray diffraction calculations made with the Takagi-Taupin equations specialized to a surface having convex or concave features, as reported in the accompanying paper [Macrander (2020). J. Appl. Cryst. 53, 793-799].

Multi-beam X-ray ptychography for high-throughput coherent diffraction imaging.

X-ray ptychography is a rapidly developing coherent diffraction imaging technique that provides nanoscale resolution on extended field-of-view. However, the requirement of coherence and the scanning mechanism limit the throughput of ptychographic imaging. In this paper, we propose X-ray ptychography using multiple illuminations instead of single illumination in conventional ptychography. Multiple locations of the sample are simultaneously imaged by spatially separated X-ray beams, therefore, the obtained field-of-view in one scan can be enlarged by a factor equal to the number of illuminations. We have demonstrated this technique experimentally using two X-ray beams focused by a house-made Fresnel zone plate array. Two areas of the object and corresponding double illuminations were successfully reconstructed from diffraction patterns acquired in one scan, with image quality similar with those obtained by conventional single-beam ptychography in sequence. Multi-beam ptychography approach increases the imaging speed, providing an efficient way for high-resolution imaging of large extended specimens.