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Intense x-ray pulses can cause the non-thermal structural transformation of diamond. At the SACLA XFEL facility, pump x-ray pulses triggered this phase transition, and probe x-ray pulses produced diffraction patterns. Time delays were observed from 0 to 250 fs, and the x-ray dose varied from 0.9 to 8.0 eV/atom. The intensity of the (111), (220), and (311) diffraction peaks decreased with time, indicating a disordering of the crystal lattice. From a Debye-Waller analysis, the rms atomic displacements perpendicular to the (111) planes were observed to be significantly larger than those perpendicular to the (220) or (311) planes. At a long time delay of 33 ms, graphite (002) diffraction indicates that graphitization did occur above a threshold dose of 1.2 eV/atom. These experimental results are in qualitative agreement with XTANT+ simulations using a hybrid model based on density-functional tight-binding molecular dynamics., Competing Interests: The authors have no conflicts to disclose., (© 2023 Author(s).)

X-ray diffraction of silicon irradiated with tightly focused femtosecond x-ray pulses (photon energy, 11.5 keV; pulse duration, 6 fs) was measured at various x-ray intensities up to 4.6×10^{19}  W/cm^{2}. The measurement reveals that the diffraction intensity is highly suppressed when the x-ray intensity reaches of the order of 10^{19}  W/cm^{2}. With a dedicated simulation, we confirm that the observed reduction of the diffraction intensity can be attributed to the femtosecond change in individual atomic scattering factors due to the ultrafast creation of highly ionized atoms through photoionization, Auger decay, and subsequent collisional ionization. We anticipate that this ultrafast reduction of atomic scattering factor will be a basis for new x-ray nonlinear techniques, such as pulse shortening and contrast variation x-ray scattering.

In this study, the growth behavior of Indium gallium nitride (InGaN)-based nanocolumn arrays was investigated, and red emission nanocolumn micro-light emitting diodes ( μ -LEDs) were fabricated. The internal structure of the InGaN/GaN superlattice (SL) layer under the multiple-quantum-well (MQW) active layers was evaluated using scanning transmission electron microscopy (STEM) analysis. It was revealed that the InGaN crystal plane at the top of the nanocolumn changed from the c-plane, (1-102) plane, to the (10-11) plane as the number of SL pairs increased. A semipolar (10-11) plane was completely formed on top of the nanocolumn by growing InGaN/GaN SLs over 15-20 pairs, where the InGaN/GaN SL layers were uniformly piled up, maintaining the (10-11) plane. Therefore, when InGaN/AlGaN MQWs were grown on the (10-11) plane InGaN/GaN SL layer, the growth of the (10-11) plane semipolar InGaN active layers was observed in the high-angle annular dark field (HAADF)-STEM image. Moreover, the acute nanocolumn top of the (10-11) plane of the InGaN/GaN SL underlayer did not contribute to the formation of the c-plane InGaN core region. Red nanocolumn μ -LEDs with an φ 12 μ m emission window were fabricated using the (10-11) plane MQWs to obtain the external quantum efficiency of 1.01% at 51 A cm -2 . The process of nanocolumn μ -LEDs suitable for the smaller emission windows was provided, where the flat p-GaN contact layer contributed to forming a fine emission window of φ 5 μ m., (© 2023 IOP Publishing Ltd.)

We demonstrate a propagation-based phase-contrast imaging method for full-field X-ray microscopy based on advanced Kirkpatrick-Baez (AKB) mirrors to achieve high-contrast observations of weak phase objects and correct field curvature aberrations. Through a demonstration performed at SPring-8, the phase contrast of weak phase objects such as polystyrene spheres and chemically fixed cells was successfully observed with high sensitivity (∼0.03 rad). Furthermore, the field of view of the AKB mirrors was expanded to the full area of the obtained images (25 × 30 µm) by correcting the field curvature aberration using reconstructed complex wavefields.

X-ray free-electron lasers (XFELs) provide intense pulses that can generate stimulated X-ray emission, a phenomenon that has been observed and studied in materials ranging from neon to copper. Two schemes have been employed: amplified spontaneous emission (ASE) and seeded stimulated emission (SSE), where a second color XFEL pulse provides the seed. Both phenomena are currently explored for coherent X-ray laser sources and spectroscopy. Here, we report measurements of ASE and SSE of the 5.9 keV Mn K α 1 fluorescence line from a 3.9 molar NaMnO 4 solution, pumped with 7 femtosecond FWHM XFEL pulses at 6.6 keV. We observed ASE at a pump pulse intensity of 1.7 × 10 19 W/cm 2 , consistent with earlier findings. We observed SSE at dramatically reduced pump pulse intensities down to 1.1 × 10 17 W/cm 2 . These intensities are well within the range of many existing XFEL instruments, which supports the experimental feasibility of SSE as a tool to generate coherent X-ray pulses, spectroscopic studies of transition metal complexes, and other applications., Competing Interests: Disclosures. The authors declare no conflicts of interest.

In this study, double-multilayer monochromators that generate intense, high-energy, pink X-ray beams are designed, installed and evaluated at the SPring-8 medium-length (215 m) bending-magnet beamline BL20B2 for imaging applications. Two pairs of W/B 4 C multilayer mirrors are designed to utilize photon energies of 110 keV and 40 keV with bandwidths of 0.8% and 4.8%, respectively, which are more than 100 times larger when compared with the Si double-crystal monochromator (DCM) with a bandwidth of less than 0.01%. At an experimental hutch located 210 m away from the source, a large and uniform beam of size 14 mm (V) × 300 mm (H) [21 mm (V) × 300 mm (H)] was generated with a high flux density of 1.6 × 10 9 photons s -1 mm -2 (6.9 × 10 10 photons s -1 mm -2 ) at 110 keV (40 keV), which marked a 300 (190) times increase in the photon flux when compared with a DCM with Si 511 (111) diffraction. The intense pink beams facilitate advanced X-ray imaging for large-sized objects such as fossils, rocks, organs and electronic devices with high speed and high spatial resolution., (open access.)

Microscopy by Achromatic X-rays With Emission of Laminar Light (MAXWELL) is a new X-ray/visible technique with attractive characteristics including isotropic resolution in all directions, large-volume imaging and high throughput. An ultrathin, laminar X-ray beam produced by a Wolter type I mirror irradiates the sample stimulating the emission of visible light by scintillating nanoparticles, captured by an optical system. Three-dimensional (3D) images are obtained by scanning the specimen with respect to the laminar beam. We implemented and tested the technique with a high-brightness undulator at SPring-8, demonstrating its validity for a variety of specimens. This work was performed under the Synchrotrons for Neuroscience-an Asia-Pacific Strategic Enterprise (SYNAPSE) collaboration., (© 2022. The Author(s).)

Bimodal behavior in the translational order of silicon's second shell in SiO 2 liquid at high temperatures and high pressures has been recognized in theoretical studies, and the fraction of the S state with high tetrahedrality is considered as structural origin of the anomalous properties. However, it has not been well identified in experiment. Here we show experimental evidence of a bimodal behavior in the translational order of silicon's second shell in SiO 2 glass under pressure. SiO 2 glass shows tetrahedral symmetry structure with separation between the first and second shells of silicon at low pressures, which corresponds to the S state structure reported in SiO 2 liquid. On the other hand, at high pressures, the silicon's second shell collapses onto the first shell, and more silicon atoms locate in the first shell. These observations indicate breaking of local tetrahedral symmetry in SiO 2 glass under pressure, as well as SiO 2 liquid., (© 2022. The Author(s).)

Coherent nonlinear spectroscopies and imaging in the X-ray domain provide direct insight into the coupled motions of electrons and nuclei with resolution on the electronic length scale and timescale. The experimental realization of such techniques will strongly benefit from access to intense, coherent pairs of femtosecond X-ray pulses. We have observed phase-stable X-ray pulse pairs containing more than 3 × 107 photons at 5.9 keV (2.1 Å) with ∼1 fs duration and 2 to 5 fs separation. The highly directional pulse pairs are manifested by interference fringes in the superfluorescent and seeded stimulated manganese Kα emission induced by an X-ray free-electron laser. The fringes constitute the time-frequency X-ray analog of Young’s double-slit interference, allowing for frequency domain X-ray measurements with attosecond time resolution.

To shorten the duration of x-ray pulses, we present a nonlinear optical technique using atoms with core-hole vacancies (core-hole atoms) generated by inner-shell photoionization. The weak Coulomb screening in the core-hole atoms results in decreased absorption at photon energies immediately above the absorption edge. By employing this phenomenon, referred to as saturable absorption, we successfully reduce the duration of x-ray free-electron laser pulses (photon energy: 9.000 keV, duration: 6-7 fs, fluence: 2.0-3.5×10^{5}  J/cm^{2}) by ∼35%. This finding that core-hole atoms are applicable to nonlinear x-ray optics is an essential stepping stone for extending nonlinear technologies commonplace at optical wavelengths to the hard x-ray region.

To identify factors that influence post-exercise muscle glycogen repletion, we compared the glycogen recovery after level running with downhill running, an experimental model of impaired post-exercise glycogen recovery. Male Institute of Cancer Research (ICR) mice performed endurance level running (no inclination) or downhill running (-5° inclination) on a treadmill. In Experiment 1, to determine whether these two types of exercise resulted in different post-exercise glycogen repletion patterns, tissues were harvested immediately post-exercise or 2 days post-exercise. Compared to the control (sedentary) group, level running induced significant glycogen supercompensation in the soleus muscle at 2 days post-exercise (p = 0.002). Downhill running did not induce glycogen supercompensation. In Experiment 2, mice were orally administered glucose 1 day post-exercise; this induced glycogen supercompensation in soleus and plantaris muscle only in the level running group (soleus: p = 0.005, plantaris: p = 0.003). There were significant positive main effects of level running compared to downhill running on the plasma insulin (p = 0.017) and C-peptide concentration (p = 0.011). There was no difference in the glucose transporter 4 level or the phosphorylated states of proteins related to insulin signaling and metabolism in skeletal muscle. The level running group showed significantly higher hexokinase 2 (HK2) protein content in both soleus (p = 0.046) and plantaris muscles (p =0.044) at 1 day after exercise compared to the downhill running group. Our findings suggest that post-exercise skeletal muscle glycogen repletion might be partly influenced by plasma insulin and skeletal muscle HK2 protein levels., (© 2021. University of Navarra.)

X-ray scientists are continually striving to improve the quality of X-ray microscopy, due to the fact that the information obtained from X-ray microscopy of materials can be complementary to that obtained from optical and electron microscopes. In contrast to the ease with which one can deflect electron beams, the relative difficulty to deflect X-ray has constrained the development of scanning X-ray microscopes (SXMs) based on a scan of an X-ray small probe. This restriction has caused severe complications that hinder progress toward achieving ultimate resolution. Here, a simple and innovative method for constructing an SXM equipped with a nanoprobe scanner is proposed. The nanoprobe scanner combines X-ray prisms and advanced Kirkpatrick-Baez focusing mirrors. By rotating the prisms on the order of degrees, X-ray probe scanning with single-nanometre accuracy can be easily achieved. The validity of the concept was verified by acquiring an SXM image of a test pattern at a photon energy of 10 keV, where 50 nm line-and-space structures were resolved. This method is readily applicable to an SXM with a single-nanometre resolution and will assist effective utilization of increasing brightness of fourth-generation synchrotron radiation sources., (© Jumpei Yamada et al. 2021.)

Background: Margin convergence has been shown to restore muscle tension in a cadaveric model of a rotator cuff tear. However, the clinical utility of this technique remains uncertain for patients with pseudoparalysis caused by an irreparable rotator cuff tear., Questions/purposes: (1) For patients with massive irreparable rotator cuff tears, in what proportion of patients does margin convergence reverse pseudoparalysis? (2) In patients with massive irreparable rotator cuff tears, does margin convergence improve American Shoulder and Elbow Surgeons (ASES) scores? (3) What is the survivorship free from MRI evidence of retear after margin convergence?, Methods: Between 2000 and 2015, we treated 203 patients for pseudoparalysis with a rotator cuff tear. Pseudoparalysis was defined as active elevation less than 90° with no stiffness, which a physical therapist evaluated in the sitting position using a goniometer after subacromial injection of 10 cc lidocaine to eliminate pain. Of those, we considered patients who underwent at least 3 weeks of unsuccessful nonoperative treatment in our hospital as potentially eligible. Twenty-one percent (43 of 203) who either improved or were lost to follow-up within 3 weeks of nonoperative treatment were excluded. A further 12% (25 of 203) were excluded because of cervical palsy, axillary nerve palsy after dislocation or subluxation, and development of severe shoulder stiffness (passive shoulder elevation < 90°). Repair was the first-line treatment, but if tears were considered irreparable with the torn tendon unable to reach the original footprint after mobilizing the cuff during surgery, margin convergence was used. When margin convergence failed, the procedure was converted to hemiarthroplasty using a small humeral head to help complete the repair. Therefore, 21% (42 of 203) of patients treated with regular repair (18% [36 of 203]) or hemiarthroplasty (3% [6 of 203]) were excluded. That left 93 patients eligible for consideration. Of those, 13 patients were lost before the minimum study follow-up of 2 years or had incomplete datasets, and 86% (80 of 93) were analyzed (49 men and 31 women; mean age 68 ± 9 years; mean follow-up 26 ± 4 months). Seventy-six percent (61 of 80) were not evaluated in the last 5 years. We considered reversal of pseudoparalysis as our primary study outcome of interest; we defined this as greater than 90° active forward elevation; physical therapists in care measured this in the sitting position by using goniometers. Clinical outcomes were evaluated based on the ASES score from chart review, active ROM in the shoulder measured by the physical therapists, and the 8-month Kaplan-Meier survivorship free from MRI evidence of retear graded by the first author., Results: Pseudoparalysis was reversed in 93% (74 of 80) patients, and improvement in ASES scores was observed at the final follow-up (preoperative 22 ± 10 to postoperative 62 ± 21, mean difference 40 [95% CI 35 to 45]; p < 0.01). The 8-month Kaplan-Meier survivorship free from MRI evidence of retear after surgery was 72% (95% CI 63% to 81%). There were no differences in clinical scores between patients with and without retears (intact ASES 64 ± 24, re-tear ASES 59 ± 10, mean difference 6 [95% CI -5 to 16]; p = 0.27)., Conclusion: Margin convergence can be a good option for treating patients with pseudoparalysis and irreparable rotator cuff tears despite the relatively high retear rates. The proportion of pseudoparalysis reversal was lower in patients with three-tendon involvement. Further studies will be needed to define the appropriate procedure in this group., Level of Evidence: Level IV, therapeutic study., Competing Interests: Each author certifies that neither he nor she, nor any member of his or her immediate family, has funding or commercial associations (consultancies, stock ownership, equity interest, patent/licensing arrangements, etc.) that might pose a conflict of interest in connection with the submitted article. All ICMJE Conflict of Interest Forms for authors and Clinical Orthopaedics and Related Research® editors and board members are on file with the publication and can be viewed on request., (Copyright © 2020 by the Association of Bone and Joint Surgeons.)

We propose an extended X-ray adaptive zoom condenser that can form an intermediate virtual focus. The system comprises two deformable mirrors for focusing within a single dimension and can vary its numerical aperture (NA) without changing the positions of the light source, mirrors, or final focus. The desired system NA is achieved simply by controlling the mirror surfaces, which enables conversion between convex and concave forms, by varying the position of the intermediate virtual focus. A feasibility test at SPring-8 under a photon energy of 10 keV demonstrated that the beam size can be varied between 134 and 1010 nm.

This paper proposes and demonstrates a simple method using the intensity correlation of X-ray fluorescence to evaluate the focused beam size of an X-ray free-electron laser (XFEL). This method was applied to the sub-micrometre focused XFEL beam at the SPring-8 Angstrom Compact Free Electron Laser, and the beam size evaluated using the proposed method was consistent with that measured using the knife-edge scan method. The proposed method is readily applicable to extremely small X-ray spots and can be applied for the precise diagnostics of sub-10 nm focused X-ray beams which have recently emerged., (open access.)

Ultimate focusing of an X-ray free-electron laser (XFEL) enables the generation of ultrahigh-intensity X-ray pulses. Although sub-10 nm focusing has already been achieved using synchrotron light sources, the sub-10 nm focusing of XFEL beams remains difficult mainly because the insufficient stability of the light source hinders the evaluation of a focused beam profile. This problem is specifically disadvantageous for the Kirkpatrick-Baez (KB) mirror focusing system, in which a slight misalignment of ∼300 nrad can degrade the focused beam. In this work, an X-ray nanobeam of a free-electron laser was generated using reflective KB focusing optics combined with speckle interferometry. The speckle profiles generated by 2 nm platinum particles were systematically investigated on a single-shot basis by changing the alignment of the multilayer KB mirror system installed at the SPring-8 Angstrom Compact Free-Electron Laser, in combination with computer simulations. It was verified that the KB mirror alignments were optimized with the required accuracy, and a focused vertical beam of 5.8 nm (±1.2 nm) was achieved after optimization. The speckle interferometry reported in this study is expected to be an effective tool for optimizing the alignment of nano-focusing systems and for generating an unprecedented intensity of up to 10 22  W cm -2 using XFEL sources., (open access.)

A novel full-field X-ray fluorescence microscope based on total-reflection advanced Kirkpatrick-Baez mirror optics was developed. The total-reflection imaging mirror optics arrangement, with four reflections, has the advantage of being able to function both as a powerful low-pass energy filter, completely rejecting incident excitation X-rays, and as an achromatic optical imaging system. Isolated X-ray fluorescence signals can be imaged, avoiding imaging-detector saturation, with low background noise. A prototype fluorescence microscope constructed at SPring-8 demonstrated the capability to simultaneously image elemental distributions using various X-ray fluorescence signals (Ni, Cu, Zn, Ge, and Bi). A half-period spatial resolution of ~0.5-1 µm (1000-500 LP/mm) was achieved, owing to the achromaticity of the imaging mirrors and the photon-counting scheme of the CCD camera used for fluorescence detection.

We demonstrated that the combination of a hyperbolic convex and elliptical concave mirrors works as a compact reflective X-ray imaging system with a short optical focal length and large magnification factor. We performed an experiment to form a one-dimensional demagnified image with a demagnification factor of 321 within an approximately 2-m-long optical setup at an X-ray energy of 10 keV. The results showed that this imaging optics system is capable of providing a resolution of ~40 nm. From wavefront analysis, it was confirmed that the optics possessed a wide field-of-view with a significant reduction of comatic aberration.

X-ray spectromicroscopy with a full-field imaging technique is a powerful method for chemical analysis of heterogeneous complex materials with a nano-scale spatial resolution. For imaging optics, an X-ray reflective optical system has excellent capabilities with highly efficient, achromatic, and long-working-distance properties. An advanced Kirkpatrick-Baez geometry that combines four independent mirrors with elliptic and hyperbolic shapes in both horizontal and vertical directions was developed for this purpose, although the complexity of the system has a limited applicable range. Here, we present an optical system consisting of two monolithic imaging mirrors. Elliptic and hyperbolic shapes were formed on a single substrate to achieve both high resolution and sufficient stability. The mirrors were finished with a ~1-nm shape accuracy using elastic emission machining. The performance was tested at SPring-8 with a photon energy of approximately 10 keV. We could clearly resolve 50-nm features in a Siemens star without chromatic aberration and with high stability over 20 h. We applied this system to X-ray absorption fine structure spectromicroscopy and identified elements and chemical states in specimens of zinc and tungsten micron-size particles.

We propose the use of two pairs of concave-convex mirrors as imaging optics for the compact full-field x-ray microscope with high resolution and magnification factors. The optics consists of two pairs of hyperbolic convex and elliptical concave mirrors with the principal surface near the object, consequently enabling the focal length to be 10 times shorter than conventional advanced Kirkpatrick-Baez mirror optics. This paper describes characteristics of the optics calculated by ray-tracing and wave-optical simulators. The expected spatial resolution is approximately 40 nm with a wide field of view of more than 10 μm and a total length of about 2 m, which may lead to the possibility of laboratory-sized, achromatic, and high-resolution full-field x-ray microscopes.

We developed an ion beam figuring system that utilizes electrostatic deflection. The system can produce an arbitrary shape by deterministically scanning the ion beam. The scan of the ion beam, which can be precisely controlled using only an electrical signal, enables us to avoid degradation of the mirror shape caused by imperfect acceleration or deceleration of a mechanically scanning stage. Additionally, this surface figuring method can easily be combined with X-ray metrology because the workpiece remains fixed during the figuring. We evaluated the figuring accuracy of the system by fabricating a plano-elliptical mirror for X-ray focusing. A mirror with a shape error of 1.4 nm root mean square (RMS) with a maximum removal depth of 992 nm, which corresponds to figuring accuracy of 0.14% RMS, was achieved. After the second shape corrections, an elliptical shape with a shape error of approximately 1 nm peak-to-valley, 0.48 nm RMS could be fabricated. Then, the mirror surface was smoothed by a low-energy ion beam. Consequently, a micro-roughness of 0.117 nm RMS, measured by atomic force microscopy, was achieved over an area of 1 × 1 μm(2).