Nanoscale determination of interatomic distance by ptychography-EXAFS method using advanced Kirkpatrick-Baez mirror focusing optics.

This work demonstrates a combination technique of X-ray ptychography and the extended X-ray absorption fine structure (ptychography-EXAFS) method, which can determine the interatomic distances of bulk materials at the nanoscale. In the high-resolution ptychography-EXAFS method, it is necessary to use high-intense coherent X-rays with a uniform wavefront in a wide energy range, hence a ptychographic measurement system installed with advanced Kirkpatrick-Baez mirror focusing optics is developed and its performance is evaluated. Ptychographic diffraction patterns of micrometre-size MnO particles are collected by using this system at 139 energies between 6.504 keV and 7.114 keV including the Mn K absorption edge, and then the EXAFS of MnO is derived from the reconstructed images. By analyzing the EXAFS spectra obtained from a 48 nm × 48 nm region, the nanoscale bond lengths of the first and second coordination shells of MnO are determined. The present approach has great potential to elucidate the unclarified relationship among the morphology, electronic state and atomic arrangement of inhomogeneous bulk materials with high spatial resolution.

Multislice imaging of integrated circuits by precession X-ray ptychography.

A method for nondestructively visualizing multisection nanostructures of integrated circuits by X-ray ptychography with a multislice approach is proposed. In this study, tilt-series ptychographic diffraction data sets of a two-layered circuit with a ∼1.4 µm gap at nine incident angles are collected in a wide Q range and then artifact-reduced phase images of each layer are successfully reconstructed at ∼10 nm resolution. The present method has great potential for the three-dimensional observation of flat specimens with thickness on the order of 100 µm, such as three-dimensional stacked integrated circuits based on through-silicon vias, without laborious sample preparation.

Visualization of Heterogeneous Oxygen Storage Behavior in Platinum-Supported Cerium-Zirconium Oxide Three-Way Catalyst Particles by Hard X-ray Spectro-Ptychography.

The cerium density and valence in micrometer-size platinum-supported cerium-zirconium oxide Pt/Ce2 Zr2 Ox (x=7-8) three-way catalyst particles were successfully mapped by hard X-ray spectro-ptychography (ptychographic-X-ray absorption fine structure, XAFS). The analysis of correlation between the Ce density and valence in ptychographic-XAFS images suggested the existence of several oxidation behaviors in the oxygen storage process in the Ce2 Zr2 Ox particles. Ptychographic-XAFS will open up the nanoscale chemical imaging and structural analysis of heterogeneous catalysts.

Three-dimensional iterative multislice reconstruction for ptychographic X-ray computed tomography.

Ptychographic X-ray computed tomography (PXCT) is a potential tool for visualizing three-dimensional (3D) structures of large-volume samples at high spatial resolution. Currently, both the requirement of a large number of views and the narrow depth of field limit the range of applications of PXCT. Here, we propose an improved 3D reconstruction algorithm for PXCT that is based on 3D iterative reconstruction and multislice phase retrieval calculation. Computer simulations showed that the proposed algorithm can reduce the number of required views without degrading the spatial resolution. In a synchrotron experiment, ptychographic diffraction data sets of a flat and thick processor specimen were collected under a limited-angle condition, and then high-resolution multislice images of the Cu multilevel interconnects were clearly reconstructed using the proposed algorithm. The proposed algorithm is expected to open up a new frontier of large-volume 3D nanoimaging in various fields.

Use of Kramers-Kronig relation in phase retrieval calculation in X-ray spectro-ptychography.

Coherent diffraction imaging (CDI) is a method for reconstructing the complex-valued image of an object from diffraction intensities by using iterative phasing methods. X-ray ptychography is a scanning type of CDI using X-rays, allowing us to visualize the complex transmission function of an extended specimen. We here propose the use of the Kramers-Kronig relation (KKR) as an additional constraint in phase retrieval algorithms for multiple-energy X-ray ptychography using the absorption edge of a specific element. A numerical simulation showed that the speed of convergence was increased by using the improved algorithm with the KKR. We successfully demonstrated its usefulness in a proof-of-principle experiment at SPring-8. The present algorithm is particularly useful for imaging X-ray absorption fine structures of a specific element buried within thick samples by hard X-ray spectro-ptychography.

Dark-field X-ray ptychography: Towards high-resolution imaging of thick and unstained biological specimens.

The phase shift of light or electrons in objects is now necessary for probing weak-phase objects such as unstained biological specimens. Optical microscopy (OM) and transmission electron microscopy (TEM) have been used to observe weak-phase objects. However, conventional OM has low spatial resolution and TEM is limited to thin specimens. Here, we report on the development of dark-field X-ray ptychography, which combines X-ray ptychography and X-ray in-line holography, to observe weak-phase objects with a phase resolution better than 0.01 rad, a spatial resolution better than 15 nm, and a field of view larger than 5 µm. We apply this method to the observation of both the outline and magnetosomes of the magnetotactic bacteria MO-1. Observation of thick samples with high resolution is expected to find broad applications in not only biology but also materials science.

Multiple defocused coherent diffraction imaging: method for simultaneously reconstructing objects and probe using X-ray free-electron lasers.

The sample size must be less than the diffraction-limited focal spot size of the incident beam in single-shot coherent X-ray diffraction imaging (CXDI) based on a diffract-before-destruction scheme using X-ray free electron lasers (XFELs). This is currently a major limitation preventing its wider applications. We here propose multiple defocused CXDI, in which isolated objects are sequentially illuminated with a divergent beam larger than the objects and the coherent diffraction pattern of each object is recorded. This method can simultaneously reconstruct both objects and a probe from the coherent X-ray diffraction patterns without any a priori knowledge. We performed a computer simulation of the prposed method and then successfully demonstrated it in a proof-of-principle experiment at SPring-8. The prposed method allows us to not only observe broad samples but also characterize focused XFEL beams.

High-resolution multislice x-ray ptychography of extended thick objects.

We report the first demonstration of hard x-ray ptychography using a multislice approach, which can solve the problem of the limited spatial resolution under the projection approximation. We measured ptychographic diffraction patterns of a two-layered object with a 105 µm gap using 7 keV focused coherent x rays. We successfully reconstructed the phase map of each layer at ∼50 nm resolution using a multislice approach, while the resolution was worse than ∼192 nm under the projection approximation. The present method has the potential to enable the three-dimensional high-resolution observation of extended thick specimens in materials science and biology.

Genetic characterization of multidrug resistance in Shigella spp. from Japan.

This study characterized the genetic basis of antimicrobial resistance of a number of Shigella spp. isolated from humans from 2000 to 2004 in Hiroshima prefecture, Japan. A total of 26 isolates of Shigella spp. were included in this study. Antimicrobial susceptibility tests revealed high levels of resistance, especially to ampicillin, streptomycin, trimethoprim, tetracycline, nalidixic acid and ciprofloxacin. PCR and DNA sequencing were used for screening and characterization of antibiotic-resistance determinants. PCR sequencing analysis revealed the presence of only one type of class 1 integron in one isolate of Shigella sonnei. This class 1 integron was 1904 bp and contained two gene cassettes: a probable esterase/lipase (estX) and aadA1, which confers resistance to streptomycin and spectinomycin. Two types of class 2 integron were identified in this study. One was the classic type (2158 bp) and carried the three conserved resistance gene cassettes of the class 2 integron, dfrA1, sat1 and aadA1, which confer resistance to trimethoprim, streptothricin and streptomycin/spectinomycin, respectively. This type was detected in both Shigella sonnei (14 isolates) and Shigella flexneri (five isolates). The other type was shorter (1313 bp) and carried only two gene cassettes, dfrA1 and sat1. This integron was detected in a single isolate of Shigella sonnei. PFGE patterns showed limited diversity within clusters of the same species. Furthermore, an extended-spectrum beta-lactamase gene, bla(OXA-30), which confers resistance to ampicillin, was characterized in all isolates of Shigella flexneri except the oldest strain, which was isolated in 2000. Southern blot hybridization and conjugation experiments showed that bla(OXA-30) was located in the chromosome.