Journal of Synchrotron Radiation最新文献

γ-Irradiation and synchrotron-radiation-based X-ray absorption fine-structure (XAFS) spectroscopy have been used to induce structure disorder through the interaction of γ-rays (200 kGy) with fabricated Mn-doped ZnO nanoparticles (NPs) and then to examine thoroughly the resultant structural change. The extracted electronic/fine XAFS structural parameters reflect a compositional and γ-irradiation co-dependence. The average crystal structure of samples prepared by the sol-gel method was investigated by X-ray diffraction (XRD). A detailed structural XRD data analysis was carried out by applying a Rietveld refinement using the MAUD program. XAFS spectra were collected at the Zn K-edge (9659 eV) in transmission mode and at the Mn K-edge (6539 eV) in fluorescence mode. Direct evidence of the solubility of Mn ions in the ZnO structure was demonstrated by fitting the extended-XAFS (EXAFS) signal. Near-edge XAFS (XANES) analysis provided the oxidation states of Zn and Mn ions through fingerprint XANES spectra of the sample along with those of standard compounds. Linear combination fitting showed that the most fit chemical forms of Zn and Mn in the samples are ZnO and MnO, respectively. The oxidation states of both Zn and Mn XAFS absorbers were confirmed from pre-edge fitting. The results of the magnetic measurements were explained in light of the average and electronic/local structural information obtained from XRD, XANES and EXAFS techniques. The magnetic properties of the samples translate into an induced change in the average crystal and electronic/local structures upon Mn concentration change and γ-irradiation. XRD confirmed the successful preparation of hexagonal Mn-doped ZnO NPs with a crystallite size in the range 33-41 nm. Both XRD and EXAFS analysis detected a minor amount of Mn₃O₄ as a secondary phase. XANES and EXAFS provided information exploring the outstanding potential of the utilized protocol for detecting precisely the presence of the secondary phase of Mn₃O₄, which changes with Mn content (x). Mean-square relative displacement (σ²) values extracted from the EXAFS fitting were found to grow for Zn-Zn/Mn paths demonstrating the substitution of Mn/Zn into Zn crystal sites. The EXAFS analysis explains the reasons behind the enhancement in the magnetic properties and shows that the Mn doping content at x = 0.05 produces the most local atomic disorder in ZnO NPs. There is a strong harmony among the XRD, XANES, EXAFS and magnetization behavior of the Mn-doped ZnO NPs. Maximum magnetization was acquired at an Mn content of 0.05. γ-Ray-irradiated Zn_1-xMn_xO NPs are recommended as optimized candidates for showing the diversity of the applications.

X-ray topography exerting the super-Borrmann effect has been performed using synchrotron radiation to display dislocation images with a high-speed and high-resolution CMOS camera. Forward-transmitted X-rays are positively employed instead of reflected X-rays to reveal dislocations in relatively thick crystals by simultaneously exciting a pair of adjacent {111} planes owing to the super-Borrmann effect. Before the experiment, minimum values of the attenuation coefficients A_min^P for σ and π polarizations of the incident X-rays in the three-beam case are calculated. Results demonstrate that A_min^P for both polarizations are almost 20 times larger than those in the two-beam (usual Borrmann effect) case. The transmitted X-rays can be used to confirm the efficacy of taking topographs under the super-Borrmann conditions, as well as under multiple-diffraction conditions. Furthermore, super-Borrmann topographs can be considered for relatively thick crystals, where a conventional Lang X-ray topography technique is difficult to apply.

Bragg coherent X-ray diffractive imaging is a cutting-edge method for recovering three-dimensional crystal structure with nanoscale resolution. Phase retrieval provides an atomic displacement parallel to the Bragg peak reciprocal lattice vector. The derivative of the displacement along the same vector provides the normal strain field, which typically serves as a proxy for any structural changes. In this communication it is found that the other component of the displacement gradient, perpendicular to the reciprocal lattice vector, provides additional information from the experimental data collected from nanocrystals with mobile dislocations. Demonstration on published experimental data show how the perpendicular component of the displacement gradient adds to existing analysis, enabling an estimate for the external stresses, pinpointing the location of surface dislocations, and predicting the dislocation motion in in situ experiments.

To cater for the diverse experiment requirements at the High Energy Photon Source (HEPS) with often limited human resources, Bluesky was chosen as the basis for our software framework, Mamba. In our attempt to address Bluesky's lack of integrated graphical user interfaces (GUIs), command injection with feedback was chosen as the main way for the GUIs to cooperate with the command line interface; a remote-procedure-call service is also provided, which covers functionalities unsuitable for command injection, as well as pushing of status updates. In order to fully support high-frequency applications like fly scans, Bluesky's support for asynchronous control is being improved; furthermore, to support high-throughput experiments, Mamba Data Worker is being developed to cover the complexity in asynchronous online data processing for these experiments. To systematically simplify the specification of metadata, scan parameters and data-processing graphs for each type of experiment, an experiment parameter generator will be developed; experiment-specific modules to automate preparation steps will also be made. The integration of off-the-shelf code in Mamba for domain-specific needs is under investigation, and Mamba GUI Studio is being developed to simplify the implementation and integration of GUIs.

X-ray micro-tomography systems often suffer from high levels of noise. In particular, severe ring artifacts are common in reconstructed images, caused by defects in the detector, calibration errors, and fluctuations producing streak noise in the raw sinogram data. Furthermore, the projections commonly contain high levels of Poissonian noise arising from the photon-counting detector. This work presents a 3-D multiscale framework for streak attenuation through a purposely designed collaborative filtering of correlated noise in volumetric data. A distinct multiscale denoising step for attenuation of the Poissonian noise is further proposed. By utilizing the volumetric structure of the projection data, the proposed fully automatic procedure offers improved feature preservation compared with 2-D denoising and avoids artifacts which arise from individual filtering of sinograms.

The advent of hard X-ray free-electron lasers enables nanoscopic X-ray imaging with sub-picosecond temporal resolution. X-ray grating interferometry offers a phase-sensitive full-field imaging technique where the phase retrieval can be carried out from a single exposure alone. Thus, the method is attractive for imaging applications at X-ray free-electron lasers where intrinsic pulse-to-pulse fluctuations pose a major challenge. In this work, the single-exposure phase imaging capabilities of grating interferometry are characterized by an implementation at the I13-1 beamline of Diamond Light Source (Oxfordshire, UK). For comparison purposes, propagation-based phase contrast imaging was also performed at the same instrument. The characterization is carried out in terms of the quantitativeness and the contrast-to-noise ratio of the phase reconstructions as well as via the achievable spatial resolution. By using a statistical image reconstruction scheme, previous limitations of grating interferometry regarding the spatial resolution can be mitigated as well as the experimental applicability of the technique.

Bayesian-inference-based approaches, in particular the random-walk Markov Chain Monte Carlo (MCMC) method, have received much attention recently for X-ray scattering analysis. Hamiltonian MCMC, a state-of-the-art development in the field of MCMC, has become popular in recent years. It utilizes Hamiltonian dynamics for indirect but much more efficient drawings of the model parameters. We described the principle of the Hamiltonian MCMC for inversion problems in X-ray scattering analysis by estimating high-dimensional models for several motivating scenarios in small-angle X-ray scattering, reflectivity, and X-ray fluorescence holography. Hamiltonian MCMC with appropriate preconditioning can deliver superior performance over the random-walk MCMC, and thus can be used as an efficient tool for the statistical analysis of the parameter distributions, as well as model predictions and confidence analysis.

Scientific tasks aimed at decoding and characterizing complex systems and processes at high pressures set new challenges for modern X-ray diffraction instrumentation in terms of X-ray flux, focal spot size and sample positioning. Presented here are new developments at the Extreme Conditions beamline (P02.2, PETRA III, DESY, Germany) that enable considerable improvements in data collection at very high pressures and small scattering volumes. In particular, the focusing of the X-ray beam to the sub-micrometer level is described, and control of the aberrations of the focusing compound refractive lenses is made possible with the implementation of a correcting phase plate. This device provides a significant enhancement of the signal-to-noise ratio by conditioning the beam shape profile at the focal spot. A new sample alignment system with a small sphere of confusion enables single-crystal data collection from grains of micrometer to sub-micrometer dimensions subjected to pressures as high as 200 GPa. The combination of the technical development of the optical path and the sample alignment system contributes to research and gives benefits on various levels, including rapid and accurate diffraction mapping of samples with sub-micrometer resolution at multimegabar pressures.

X-ray fluorescence microscopy performed at nanofocusing synchrotron beamlines produces quantitative elemental distribution maps at unprecedented resolution (down to a few tens of nanometres), at the expense of relatively long measuring times and high absorbed doses. In this work, a method was implemented in which fast low-dose in-line holography was used to produce quantitative electron density maps at the mesoscale prior to nanoscale X-ray fluorescence acquisition. These maps ensure more efficient fluorescence scans and the reduction of the total absorbed dose, often relevant for radiation-sensitive (e.g. biological) samples. This multimodal microscopy approach was demonstrated on human sural nerve tissue. The two imaging modes provide complementary information at a comparable resolution, ultimately limited by the focal spot size. The experimental setup presented allows the user to swap between them in a flexible and reproducible fashion, as well as to easily adapt the scanning parameters during an experiment to fine-tune resolution and field of view.

A revised version of Table 2 of Nanao et al. [J. Synchrotron Rad. (2022). 29, 581-590] is provided.