High-resolution X-ray Microscopy Research Articles

Generation of pore-space images using improved pyramid Wasserstein generative adversarial networks

High-resolution three-dimensional X-ray microscopy can be used to image the pore space of materials. Machine learning algorithms can generate a statistical ensemble of representative images of arbitrary sizes for rock characterization, modeling, and analysis. However, current methods struggle to capture features at different spatial scales observed in many complex rocks which have a wide range of pore size. We use the Improved Pyramid Wasserstein Generative Adversarial Network (IPWGAN) to automatically reproduce multi-scale features in segmented three-dimensional images of porous materials, enabling the reliable generation of large-scale representations of complex porous media. A Laplacian pyramid generator is introduced, which creates pore-space features across a hierarchy of spatial scales. Feature statistics mixing regularization enhances the discriminator’s ability to distinguish between real and generated images by mixing their feature statistics, thereby indirectly enhancing the generator’s ability to capture and reproduce multi-scale pore-space features, leading to increased diversity and realism in the generated images. The method has been tested on five sandstone and carbonate samples. The generated images, which can be of any size – including cm-scale ten-billion-cell images – demonstrate the power of the approach. These images have two-point correlation functions, porosity, permeability, Euler characteristic, curvature, and specific surface area closer to those of the training datasets than existing machine learning techniques. The generated images accurately capture geometric and flow properties, demonstrating a considerable improvement over previously published studies using generative adversarial networks. For instance, the mean relative error in the calculated absolute permeability between the Berea sandstone images generated by IPWGAN and the corresponding real rock images can be reduced by 79%. The work allows representative models of a wide range of porous media to be generated, offering potential benefits in carbon dioxide sequestration, underground hydrogen storage, and enhanced oil recovery.

Direct Observation of Room-Temperature Magnetic Skyrmion Motion Driven by Ultra-Low Current Density in Van Der Waals Ferromagnets.

The recent discovery of room-temperature ferromagnetism in 2D van der Waals (vdW) materials, such as Fe3GaTe2 (FGaT), has garnered significant interest in offering a robust platform for 2D spintronic applications. Various fundamental operations essential for the realization of 2D spintronics devices are experimentally confirmed using these materials at room temperature, such as current-induced magnetization switching or tunneling magnetoresistance. Nevertheless, the potential applications of magnetic skyrmions in FGaT systems at room temperature remain unexplored. In this work, the current-induced generation of magnetic skyrmions in FGaT flakes employing high-resolution magnetic transmission soft X-ray microscopy is introduced, supported by a feasible mechanism based on thermal effects. Furthermore, direct observation of the current-induced magnetic skyrmion motion at room temperature in FGaT flakes is presented with ultra-low threshold current density. This work highlights the potential of FGaT as a foundation for room-temperature-operating 2D skyrmion device applications.

Free light-shape focusing in extreme-ultraviolet radiation with self-evolutionary photon sieves

Extreme-ultraviolet (EUV) radiation is a promising tool, not only for probing microscopic activities but also for processing nanoscale structures and performing high-resolution imaging. In this study, we demonstrate an innovative method to generate free light-shape focusing with self-evolutionary photon sieves under a single-shot coherent EUV laser; this includes vortex focus shaping, array focusing, and structured-light shaping. The results demonstrate that self-evolutionary photon sieves, consisting of a large number of specific pinholes fabricated on a piece of Si3N4 membrane, are capable of freely regulating an EUV light field, for which high-performance focusing elements are extremely lacking, let alone free light-shape focusing. Our proposed versatile photon sieves are a key breakthrough in focusing technology in the EUV region and pave the way for high-resolution soft X-ray microscopy, spectroscopy in materials science, shorter lithography, and attosecond metrology in next-generation synchrotron radiation and free-electron lasers.

Unveiling the Inner Structure of Micrometric Hollow Polymeric Fibers Using Synchrotron X-Ray Nanotomography.

In this study, a novel application of synchrotron X-ray nanotomography based on high-resolution full-field transmission X-ray microscopy for characterizing the structure and morphology of micrometric hollow polymeric fibers is presented. By employing postimage analysis using an open-source software such as Tomviz and ImageJ, various key parameters in fiber morphology, including diameter, wall thickness, wall thickness distribution, pore size, porosity, and surface roughness, were assessed. Electrospun polycaprolactone fibers with micrometric diameters and submicrometric features with induced porosity via gas dissolution foaming were used to this aim. The acquired synchrotron X-ray nanotomography data were analyzed using two approaches: 3D tomographic reconstruction and 2D radiographic projection-based analysis. The results of the combination of both approaches demonstrate unique capabilities of this technique, not achievable by other available techniques, allowing for a full characterization of the internal and external morphology and structure of the fibers as well as to obtain valuable qualitative insights into the overall fiber structure.

Exploring the infiltrative and degradative ability of Fusarium oxysporum on polyethylene terephthalate (PET) using correlative microscopy and deep learning

Managing the worldwide steady increase in the production of plastic while mitigating the Earth’s global pollution is one of the greatest challenges nowadays. Fungi are often involved in biodegradation processes thanks to their ability to penetrate into substrates and release powerful catabolic exoenzymes. However, studying the interaction between fungi and plastic substrates is challenging due to the deep hyphal penetration, which hinders visualisation and evaluation of fungal activity. In this study, a multiscale and multimodal correlative microscopy workflow was employed to investigate the infiltrative and degradative ability of Fusarium oxysporum fungal strain on polyethylene terephthalate (PET) fragments. The use of non-destructive high-resolution 3D X-ray microscopy (XRM) coupled with a state-of-art Deep Learning (DL) reconstruction algorithm allowed optimal visualisation of the distribution of the fungus on the PET fragment. The fungus preferentially developed on the edges and corners of the fragment, where it was able to penetrate into the material through fractures. Additional analyses with scanning electron microscopy (SEM), Raman and energy dispersive X-ray spectroscopy (EDX) allowed the identification of the different phases detected by XRM. The correlative microscopy approach unlocked a more comprehensive understanding of the fungus-plastic interaction, including elemental information and polymeric composition.

Simultaneous bright- and dark-field X-ray microscopy at X-ray free electron lasers

The structures, strain fields, and defect distributions in solid materials underlie the mechanical and physical properties across numerous applications. Many modern microstructural microscopy tools characterize crystal grains, domains and defects required to map lattice distortions or deformation, but are limited to studies of the (near) surface. Generally speaking, such tools cannot probe the structural dynamics in a way that is representative of bulk behavior. Synchrotron X-ray diffraction based imaging has long mapped the deeply embedded structural elements, and with enhanced resolution, dark field X-ray microscopy (DFXM) can now map those features with the requisite nm-resolution. However, these techniques still suffer from the required integration times due to limitations from the source and optics. This work extends DFXM to X-ray free electron lasers, showing how the 10^{12} photons per pulse available at these sources offer structural characterization down to 100 fs resolution (orders of magnitude faster than current synchrotron images). We introduce the XFEL DFXM setup with simultaneous bright field microscopy to probe density changes within the same volume. This work presents a comprehensive guide to the multi-modal ultrafast high-resolution X-ray microscope that we constructed and tested at two XFELs, and shows initial data demonstrating two timing strategies to study associated reversible or irreversible lattice dynamics.

Alterations promoted by acid straightening and/or bleaching in hair microstructures.

Human hair is a biopolymer constituted mainly of keratin intermediate filaments, lipids, pigments and water. Cosmetic treatments usually interact with the hair at the molecular level, inducing changes in its components and modifying the physicochemical and mechanical properties of the fibers. Here, the effect of acid straightening on the morphology and ultrastructure of Caucasian hair was investigated by a group of complementary experimental methods: wide-, small- and ultra-small-angle X-ray scattering; high-resolution 3D X-ray microscopy; quasi-elastic neutron scattering and inelastic neutron scattering; thermogravimetry-mass spectrometry; and differential scanning calorimetry (DSC). X-ray diffraction patterns showed that acid straightening associated with a flat iron (∼180°C) changed the cortex of the fiber, shown by denaturation of the intermediate filaments (measured by DSC). The increase in the spacing of the lipid layers and the observation of the dehydration behavior of the fiber provided indications that water may be confined between these layers, while neutron spectroscopy showed alterations in the vibration mode of the CH2 groups of the lipids and an increase of the proton (H+) mobility in the hair structure. The latter may be associated with the extremely low pH of the formulation (pH ≃ 1). Additionally, this investigation showed that bleached hair (one-time bleached) is more damaged by the action of acid straightening than virgin hair, which was shown by a threefold increase in the percentage of total porosity of the tresses. The obtained results demonstrate that the investigation approach proposed here can provide very important thermodynamic and structural information on induced changes of hair structure, and certainly can be applied for the evaluation of the action mode and efficiency of cosmetic treatments.

A Correlative Approach Combining Non-destructive High Resolution X-Ray Microscopy with Femtosecond Laser Preparation and FIB/SEM to Access Deeply Buried Features in Parts and Components of New Energy Vehicles.

A Correlative Approach Combining Non-destructive High Resolution X-Ray Microscopy with Femtosecond Laser Preparation and FIB/SEM to Access Deeply Buried Features in Parts and Components of New Energy Vehicles.

Silicon and calcium controls on iron and aluminum mobility in Arctic soils

Arctic permafrost soils store large amounts of organic carbon and nutrients. With deepening of the perennial thawing upper active layer due to rising temperatures in the Arctic, not only the mobility of organic matter (OM), but also those of elements like silicon (Si) or calcium (Ca) may increase. It is known that major elements like Si and Ca can affect mineralization rates of OM, consequently influencing the carbon cycle. But only little is known about the interactions of Si and Ca with inorganic nutrients like iron (Fe) or potentially toxic elements like aluminum (Al) in Artic soils. In this study, we analyzed the effect of Si and Ca fertilization in laboratory incubation experiments with soil samples from several Arctic regions. Our results show a significant increase in Fe and Al mobility (Mehlich-3 extractable) after increasing Si. Using high resolution X-ray microscopy (STXM/NEXAFS), we show that Si promotes Fe(II) phases and by this increases Fe mobility. Al mobility was increased for acidic and neutral pH soils but decreased for alkaline soils after increasing Si. Furthermore, we show a decreased Al mobility after increasing Ca, independent on the original pH values and the OM content of the soils. These results demonstrate the importance of interactions between Si and Ca on one hand and Fe and Al mobility on the other hand for Arctic soils.

Semiconductors (LEDs) quality control based in high-resolution 3D X-ray microscope

Electronic devices are getting smaller each time and the technology, increasingly complex. Commonly found problems such as reflow soldering and open solder connections, which are mostly difficult to detect by conventional means like X-ray images or physical cut on the transverse section. Along with the challenge of finding these flaws, there are also some problems that may arise on the exposure of them using destructive analysis techniques, such as the fiscal transversal cut and chemical decapsulation. Both techniques may induce damage not relevant to where that flaw is located or remove evidence of a flaw or a damaged place. The high-resolution 3D x-ray computerized microtomography provides a powerful alternative solution and non-invasive to issues that involve the analysis of semiconductor devices. This research contemplates the study of semiconductor’s integrity (LED’s) based of X-ray computerized microtomography. The SkyScan 1272 Bruker commercial equipment was used for analysis of the P-N junction in a set with 10 LEDs, under non polarized conditions and upon electrical overstress effects on its contact terminals. The P-N junction had their dimensions analyzed on the three spatial directions (x, y and z) and studied on the effects that occur when a LED is damaged. The study methodology of integrity regarding computerized microtomography have shown consist outcomes that allowed the understanding of what occurs on the LED's structure and investigates matters that allows decisions to be made regarding its quality, and so, accomplishing the goals designated on this research.

High spatial resolution analysis using automated indentation mapping differentiates biomechanical properties of normal vs. degenerated articular cartilage in mice.

Characterizing the biomechanical properties of articular cartilage is crucial to understanding processes of tissue homeostasis vs. degeneration. In mouse models, however, limitations are imposed by their small joint size and thin cartilage surfaces. Here we present a three-dimensional (3D) automated surface mapping system and methodology that allows for mechanical characterization of mouse cartilage with high spatial resolution. We performed repeated indentation mappings, followed by cartilage thickness measurement via needle probing, at 31 predefined positions distributed over the medial and lateral femoral condyles of healthy mice. High-resolution 3D x-ray microscopy (XRM) imaging was used to validate tissue thickness measurements. The automated indentation mapping was reproducible, and needle probing yielded cartilage thicknesses comparable to XRM imaging. When comparing healthy vs. degenerated cartilage, topographical variations in biomechanics were identified, with altered thickness and stiffness (instantaneous modulus) across condyles and within anteroposterior sub-regions. This quantitative technique comprehensively characterized cartilage function in mice femoral condyle cartilage. Hence, it has the potential to improve our understanding of tissue structure-function interplay in mouse models of repair and disease.

Achieving High-Resolution Hard X-ray Microscopy using Monolithic 2D Multilayer Laue Lenses

Abstract: This article introduces the 2D multilayer Laue lens (MLL) nanofocusing optics recently developed for high-resolution hard X-ray microscopy. The new optics utilized a micro-electro-mechanical-system (MEMS)-based template to accommodate two linear MLL optics in a pre-aligned configuration. Angular misalignment between the two lenses was controlled in tens of millidegrees, and the lateral position error was on a micrometer scale. Using the developed 2D MLLs, an astigmatism-free point focus of approximately 14 nm by 13 nm in horizontal and vertical directions, respectively, at 13.6 keV photon energy was obtained. The success of 2D MLL optics with an approaching 10 nm resolution is a significant step forward for the development of high-resolution hard X-ray microscopy and applications of MLL optics in the hard X-ray community.

Machine-learning-based automatic small-angle measurement between planar surfaces in interferometer images: A 2D multilayer Laue lenses case

We report a new machine-learning-based approach to automatically measure the small angle between multiple planar surfaces characterized by white light interferometers. By applying an unsupervised clustering algorithm, DBSCAN (Density-Based Spatial Clustering of Applications with Noise), the multiple surfaces in an interferometer image are automatically identified as distinct surfaces. The angles between every two surfaces are then calculated through the surface fitting. This method can be applied to multiple surfaces regardless of their shapes and locations and significantly simplifies the angle measurement procedure. Using the developed method, we have demonstrated a quick and precise angle measurement for the alignment of 2D Multilayer Laue Lenses (MLLs) for the development of high-resolution x-ray microscopy. This automatic, accurate, and robust small-angle measurement method is compatible with widely used white light interferometers and can be further applied to other metrology applications of interferometer results.

Cover Feature: Elucidating the Sectioning Fragmentation Mechanism in Silica‐Supported Olefin Polymerization Catalysts with Laboratory‐Based X‐Ray and Electron Microscopy (ChemCatChem 21/2022)

The Cover Feature shows an artistic interpretation of a supported polymerization catalyst particle that is fragmenting during ethylene polymerization. In their Research Article, F. Meirer, B. M. Weckhuysen and co-workers used high resolution X-ray and electron microscopy to elucidate the origins of the sectioning fragmentation mechanism in two different silica-supported olefin polymerization catalysts at the single particle level. The occurrence of the sectioning fragmentation mechanism was shown to be favoured by a low degree of macroporosity in the silica granulates constituting the catalyst support, a high accessibility of the particle interior at reaction onset, as well as fast catalyst kinetics. More information can be found in the Research Article by F. Meirer, B. M. Weckhuysen and co-workers.

Comparative Analysis of Robotics-Assisted and Manual Insertions of Cochlear Implant Electrode Arrays.

Robotics-assisted cochlear implant (CI) insertions will result in reduced intracochlear trauma when compared with manual, across multiple users. Whether intracochlear trauma and translocations are two factors that may contribute to significant variability in CI outcomes remains to be seen. To address this issue, we have developed a robotics-assisted insertion system designed to aid the surgeon in inserting electrode arrays with consistent speeds and reduced variability. This study evaluated the effect of robotics-assisted insertions on the intracochlear trauma as compared with manual insertions in cadaveric cochleae in a simulated operative environment. Twelve neurotologists performed bilateral electrode insertions into cochleae of full cadaveric heads using both the robotics-assisted system and manual hand insertion. Lateral wall electrodes from three different manufacturers (n = 24) were used and randomized between surgeons. Insertion angle of the electrode and trauma scoring were evaluated using high-resolution three-dimensional x-ray microscopy and compared between robotics-assisted and manual insertions. Three-dimensional x-ray microscopy provided excellent resolution to characterize the in situ trauma and insertion angle. Robotics-assisted insertions significantly decreased insertional intracochlear trauma as measured by reduced trauma scores compared with manual insertions (average: 1.3 versus 2.2, device versus manual, respectively; p < 0.05). There was no significant difference between insertion angles observed for manual and robotics-assisted techniques (311 ± 131° versus 307 ± 96°, device versus manual, respectively). Robotics-assisted insertion systems enable standardized electrode insertions across individual surgeons and experience levels. Clinical trials are necessary to investigate whether insertion techniques that reduce insertional variability and the likelihood of intracochlear trauma also improve CI auditory outcomes.

A high-resolution X-ray microscope system for performance evaluation of scintillator plates

In the development of new scintillators for X-ray imaging, a high-resolution and highly efficient system is required to evaluate the performance of the scintillator plates. For this purpose, we developed a high-resolution X-ray microscope system. The developed compact X-ray microscope system is based on a magnifying unit and a cooled charge-coupled device (CCD) camera, combined with a small industrial X-ray irradiation system. Using this system, we carried out imaging of three scintillator plates and evaluated their spatial resolution. Each scintillator plates was set in front of the lens of the objective, X-rays were irradiated to the scintillator plates, and transmission images of masks were acquired. The measured spatial resolution of the scintillator plates varied from 16 μm to 30 μm, depending on the type of scintillator plate. The focus size of the X-ray tube had an almost negligible effect on the spatial resolution of the images for the evaluated scintillator plates.

Determination of as-built properties of fiber reinforced polymers in a wind turbine blade using scanning electron and high-resolution X-ray microscopy

The fiber volume fraction (FVF) and porosity in fiber reinforced polymers (FRPs) depends strongly on the manufacturing process. These parameters influence the mechanical properties and thus the performance of an FRP. For this research, an epoxy-pre-impregnated glass FRP was investigated to determine the FVF and matrix mass fraction taking into consideration all material constituents, including sizing, stitching thread, as well as the porosity, the area density and the fiber orientations of each lamina, the filament fiber diameter, and the inter-laminar void size and shape. Therefore, samples from a commercially manufactured wind turbine rotor blade were experimentally investigated using scanning electron (SEM) and high-resolution X-ray microscopy (micro-CT), as well as a standardized calcination method and geometric measurements. Post-processing techniques such as thresholding and edge detection were used to analyze the images. There was good FVF agreement between SEM and the method of calcination. Micro-void cross-sectional shapes were well captured by SEM while meso- and macro-voids were volumetrically resolved with a reproducible void size distribution for two sample volumes by micro-CT.

Calibration by differentiation - Self-supervised calibration for X-ray microscopy using a differentiable cone-beam reconstruction operator.

High-resolution X-ray microscopy (XRM) is gaining interest for biological investigations of extremely small-scale structures. XRM imaging of bones in living mice could provide new insights into the emergence and treatment of osteoporosis by observing osteocyte lacunae, which are holes in the bone of few micrometres in size. Imaging living animals at that resolution, however, is extremely challenging and requires very sophisticated data processing converting the raw XRM detector output into reconstructed images. This paper presents an open-source, differentiable reconstruction pipeline for XRM data which analytically computes the final image from the raw measurements. In contrast to most proprietary reconstruction software, it offers the user full control over each processing step and, additionally, makes the entire pipeline deep learning compatible by ensuring differentiability. This allows fitting trainable modules both before and after the actual reconstruction step in a purely data-driven way using the gradient-based optimizers of common deep learning frameworks. The value of such differentiability is demonstrated by calibrating the parameters of a simple cupping correction module operating on the raw projection images using only a self-supervisory quality metric based on the reconstructed volume and no further calibration measurements. The retrospective calibration directly improves image quality as it avoids cupping artefacts and decreases the difference in grey values between outer and inner bone by 68-94%. Furthermore, it makes the reconstruction process entirely independent of the XRM manufacturer and paves the way to explore modern deep learning reconstruction methods for arbitrary XRM and, potentially, other flat-panel computed tomography systems. This exemplifies how differentiable reconstruction can be leveraged in the context of XRM and, hence, is an important step towards the goal of reducing the resolution limit of in vivo bone imaging to the single micrometredomain.

Pore space of steatite ceramics triggered by the allowance of natural fibers: High-resolution X-ray microscopy analysis and related thermo-mechanical properties

A large number (greater than 150) of porous steatite ceramic rods were prepared using different types of renewable plant fiber products as pore-forming agent with mass contents ranging from 2 to 10%. In addition, dense steatite ceramics were synthesized for comparison within a gas furnace at sintering temperatures between 1300 and 1350 °C. High-resolution 3D X-ray microscopy facilitated a non-destructive, direct investigation of the three-dimensional pore space and microstructure. By using image-based pore space analysis, various pore space parameters, such as, e.g., pore volume, pore-size distribution, and pore connectivity were determined. In addition to the characterization of the pore space, phase analysis, structural and chemical investigations were carried out by X-ray powder diffraction, electron microscopy, Fourier-transform infrared, Raman and X-ray spectroscopy. Finally, to evaluate the influence of characteristics on the physical properties, elastic, strength and thermal properties were determined. With the increase of porosity, the flexural strength and thermal conductivity values decrease from σf = 123 ± 8 to 37 ± 5 MPa and λ = 3.22 ± 0.02 to 1.77 ± 0.02 W/(m·K), respectively. The obtained experimental results were discussed by means of micromechanical models, highlighting the effect of pore-space morphologies on the physical performance of porous steatite ceramics.

An achromatic X-ray lens

Diffractive and refractive optical elements have become an integral part of most high-resolution X-ray microscopes. However, they suffer from inherent chromatic aberration. This has to date restricted their use to narrow-bandwidth radiation, essentially limiting such high-resolution X-ray microscopes to high-brightness synchrotron sources. Similar to visible light optics, one way to tackle chromatic aberration is by combining a focusing and a defocusing optic with different dispersive powers. Here, we present the first successful experimental realisation of an X-ray achromat, consisting of a focusing diffractive Fresnel zone plate (FZP) and a defocusing refractive lens (RL). Using scanning transmission X-ray microscopy (STXM) and ptychography, we demonstrate sub-micrometre achromatic focusing over a wide energy range without any focal adjustment. This type of X-ray achromat will overcome previous limitations set by the chromatic aberration of diffractive and refractive optics and paves the way for new applications in spectroscopy and microscopy at broadband X-ray tube sources.