Optimization of the Guide Design of MIRACLES, the Neutron Time-of-Flight Backscattering Spectrometer at the European Spallation Source

To boost the science case of MIRACLES, the time-of-flight backscattering spectrometer at the European Spallation Source (ESS), an optimized neutron guide system, is proposed. This systematic study resulted in an enhancement in the transport of cold neutrons, compared with the previous conceptual design, with wavelengths ranging from λ = 2 Å to 20 Å along the 162.5-m distance from source to sample. This maintained the undisturbed main focus of the instrument, viz, to carry out quasielastic and inelastic neutron scattering (QENS and INS) experiments on a large dynamic range and for both energy-gain and energy-loss sides. To improve the collection of cold neutrons from the source and direct them to the sample position, the vertical geometry was adjusted to an adapted version of a ballistic elliptical profile. Its horizontal geometry was conceived to: (i) keep the high-resolution performance of the instrument, and (ii) minimize the background originating from fast and thermal neutrons. To comply with the first requirement, a narrow guide section at the pulse shaping chopper position has been implemented. To fulfil the second, a curved guide segment has been chosen to suppress neutrons with wavelengths λ < 2 Å. Subsequent tailoring of the phase space provided an efficient transport of cold neutrons along the beamline to reach a 3 × 3 cm2 sample. Finally, additional calculations were performed to present a potential upgrade, with the exchange of the final segment, to focus on samples of approximately 1 × 1 cm2; the proposal anticipates a flux increase of 70% in this 1 cm2 sample area.

Scanning ion-conductance microscope with modulation of the sample position along the Z-coordinate and separate Z-axial and lateral (X, Y) scanning

Scanning ion-conductance microscope with independent piezoscanners in the lateral scanning plane XY and Z axis was designed and tested. For precise, fast and safe approach of the nanopipette to the sample surface, a coarse approach system based on a piezoinertial mover was used. Measurements of test periodic polymer structures were carried out using nanopipettes with an inner pipette diameter of about 100-150 nm. The optimal geometric parameters of the nanopipette were found and the resolution of the method was estimated. To increase the stability and reproducibility of SICM images, the Z-modulation of the position of the substrate with the sample was realized using a bimorph piezomembrane.

Robust autofocusing for scanning electron microscopy based on a dual deep learning network

Scanning electron microscopy (SEM) is a high-resolution imaging technique with subnanometer spatial resolution that is widely used in materials science, basic science, and nanofabrication. However, conducting SEM is rather complex due to the nature of using an electron beam and the many parameters that must be adjusted to acquire high-quality images. Only trained operators can use SEM equipment properly, meaning that the use of SEM is restricted. To broaden the usability of SEM, we propose an autofocus method for a SEM system based on a dual deep learning network, which consists of an autofocusing-evaluation network (AENet) and an autofocusing-control network (ACNet). The AENet was designed to evaluate the quality of given images, with scores ranging from 0 to 9 regardless of the magnification. The ACNet can delicately control the focus of SEM online based on the AENet’s outputs for any lateral sample position and magnification. The results of these dual networks showed successful autofocus performance on three trained samples. Moreover, the robustness of the proposed method was demonstrated by autofocusing on unseen samples. We expect that our autofocusing system will not only contribute to expanding the versatility of SEM but will also be applicable to various microscopes.

Measurement of the coherent beam properties at the CoSAXS beamline

The CoSAXS beamline at the MAX IV Laboratory is a modern multi-purpose (coherent) small-angle X-ray scattering (CoSAXS) instrument, designed to provide intense and optionally coherent illumination at the sample position, enabling coherent imaging and speckle contrast techniques. X-ray tracing simulations used to design the beamline optics have predicted a total photon flux of 1012–1013 photons s−1 and a degree of coherence of up to 10% at 7.1 keV. The normalized degree of coherence and the coherent flux of this instrument were experimentally determined using the separability of a ptychographic reconstruction into multiple mutually incoherent modes and thus the Coherence in the name CoSAXS was verified. How the beamline can be used both for coherent imaging and XPCS measurements, which both heavily rely on the degree of coherence of the beam, was demonstrated. These results are the first experimental quantification of coherence properties in a SAXS instrument at a fourth-generation synchrotron light source.

Development and application of a tender X-ray ptychographic coherent diffraction imaging system on BL27SU at SPring-8

Ptychographic coherent diffraction imaging (CDI) allows the visualization of both the structure and chemical state of materials on the nanoscale, and has been developed for use in the soft and hard X-ray regions. In this study, a ptychographic CDI system with pinhole or Fresnel zone-plate optics for use in the tender X-ray region (2–5 keV) was developed on beamline BL27SU at SPring-8, in which high-precision pinholes optimized for the tender energy range were used to obtain diffraction intensity patterns with a low background, and a temperature stabilization system was developed to reduce the drift of the sample position. A ptychography measurement of a 200 nm thick tantalum test chart was performed at an incident X-ray energy of 2.500 keV, and the phase image of the test chart was successfully reconstructed with approximately 50 nm resolution. As an application to practical materials, a sulfur polymer material was measured in the range of 2.465 to 2.500 keV including the sulfur K absorption edge, and the phase and absorption images were successfully reconstructed and the nanoscale absorption/phase spectra were derived from images at multiple energies. In 3 GeV synchrotron radiation facilities with a low-emittance storage ring, the use of the present system will allow the visualization on the nanoscale of the chemical states of various light elements that play important roles in materials science, biology and environmental science.

Adaptation of the Standard Off-Axis Digital Holographic Microscope to Achieve Variable Magnification

Traditional microscopy provides only for a small set of magnifications using a finite set of microscope objectives. Here, a novel architecture is proposed for quantitative phase microscopy that requires only a simple adaptation of the traditional off-axis digital holographic microscope. The architecture has the key advantage of continuously variable magnification, resolution, and Field-of-View, by simply moving the sample. The method is based on combining the principles of traditional off-axis digital holographic microscopy and Gabor microscopy, which uses a diverging spherical wavefield for magnification. We present a proof-of-concept implementation and ray-tracing is used to model the magnification, Numerical Aperture, and Field-of-View as a function of sample position. Experimental results are presented using a micro-lens array and shortcomings of the method are highlighted for future work; in particular, the problem of aberration is highlighted, which results from imaging far from the focal plane of the infinity corrected microscope objective.

BL-11C Micro-MX: a high-flux microfocus macromolecular-crystallography beamline for micrometre-sized protein crystals at Pohang Light Source II

BL-11C, a new protein crystallography beamline, is an in-vacuum undulator-based microfocus beamline used for macromolecular crystallography at the Pohang Accelerator Laboratory and it was made available to users in June 2017. The beamline is energy tunable in the range 5.0–20 keV to support conventional single- and multi-wavelength anomalous-dispersion experiments against a wide range of heavy metals. At the standard working energy of 12.659 keV, the monochromated beam is focused to 4.1 µm (V) × 8.5 µm (H) full width at half-maximum at the sample position and the measured photon flux is 1.3 × 1012 photons s−1. The experimental station is equipped with a Pilatus3 6M detector, a micro-diffractometer (MD2S) incorporating a multi-axis goniometer, and a robotic sample exchanger (CATS) with a dewar capacity of 90 samples. This beamline is suitable for structural determination of weakly diffracting crystalline substances, such as biomaterials, including protein, nucleic acids and their complexes. In addition, serial crystallography experiments for determining crystal structures at room temperature are possible. Herein, the current beamline characteristics, technical information for users and some recent scientific highlights are described.

Labmade Metallizer: Deposition of Aluminum Film on Glass Substrate and Subsequent Anodization to obtain Aluminum Oxide

In this work, the assembly of a low-cost metallizer is presented, based on physical vapor deposition, to obtain metallic aluminum film deposited over a glass substrate. Later, the Al film is anodized and converted into a porous nanostructured oxide film. The metallic film thickness was measured by profilometry, and the sample position inside the chamber was evaluated. Samples positioned at the center of the sample holder showed considerable thickness and best homogeneity compared to those samples positioned at the edges of the sample holder. A thick metallic film of Al (6 to 7 µm) was deposited over the glass substrate for subsequent anodizing treatment. Mild anodization allowed the total conversion of metallic Al after 7000 s, producing a transparent anodic aluminum oxide (AAO) film adhered to the glass substrate. The AAO morphology was investigated by SEM. Some factors have been listed to describe the low regularity and homogeneity of nanopores in the outer layer of AAO, such as internal defects, compaction of deposited Al film layers and the glass substrate roughness.

The lower energy diffraction and scattering side-bounce beamline for materials science at the Canadian Light Source

A new diffraction beamline for materials science has been built at the Canadian Light Source synchrotron. The X-ray source is an in-vacuum wiggler with a 2.5 T peak magnetic field at 5.2 mm gap. The optical configuration includes a toroidal mirror, a single side-bounce Bragg monochromator, and a cylindrical mirror, producing a sub-150 µm vertical × 500 µm horizontal focused beam with a photon energy range of 7–22 keV and a flux of 1012 photons per second at the sample position. Three endstations are currently open to general users, and the techniques available include high-resolution powder diffraction, small molecule crystallography, X-ray reflectivity, in situ rapid thermal annealing, and SAXS/WAXS. The beamline design parameters, calculated and measured performance, and initial experimental results are presented to demonstrate the capabilities for materials science.

Crystal orientation and detector distance effects on resolving pseudosymmetry by electron backscatter diffraction

Accurately indexing pseudosymmetric materials has long proven challenging for electron backscatter diffraction. The recent emergence of intensity-based indexing approaches promises an enhanced ability to resolve pseudosymmetry compared with traditional Hough-based indexing approaches. However, little work has been done to understand the effects of sample position and orientation on the ability to resolve pseudosymmetry, especially for intensity-based indexing approaches. Thus, in this work the effects of crystal orientation and detector distance in a model tetragonal ZrO2 (c/a = 1.0185) material are quantitatively investigated. The orientations that are easiest and most difficult to correctly index are identified, the effect of detector distance on indexing confidence is characterized, and these trends are analyzed on the basis of the appearance of specific zone axes in the diffraction patterns. The findings also point to the clear benefit of shorter detector distances for resolving pseudosymmetry using intensity-based indexing approaches.