Scanning Transmission X-ray Microscopy Research Articles

Strongly-Interacted NiSe2/NiFe2O4 Architectures Built Through Selective Atomic Migration as Catalysts for the Oxygen Evolution Reaction.

The interactions between the catalyst and support are widely used in many important catalytic reactions but the construction of strong interaction with definite microenvironments to understand the structure-activity relationship is still challenging. Here, strongly-interacted composites are prepared via selective exsolution of active NiSe2 from the host matrix of NiFe2O4 (S-NiSe2/NiFe2O4) taking advantage of the differences of migration energy, in which the NiSe2 possessed both high dispersion and small size. The characteristics of spatially resolved scanning transmission X-ray microscopy (STXM) coupled with analytical Mössbauer spectra for the surface and bulk electronic structures unveiled that this strongly interacted composite triggered more charge transfers from the NiSe2 to the host of NiFe2O4 while stabilizing the inherent atomic coordination of NiFe2O4. The obtained S-NiSe2/NiFe2O4 exhibits overpotentials of 290mV at 10mAcm-2 for oxygen evolution reaction (OER). This strategy is general and can be extended to other supported catalysts, providing a powerful tool for modulating the catalytic performance of strongly-interacted composites.

Manifold projection image segmentation for nano-XANES imaging

As spectral imaging techniques are becoming more prominent in science, advanced image segmentation algorithms are required to identify appropriate domains in these images. We present a version of image segmentation called manifold projection image segmentation (MPIS) that is generally applicable to a broad range of systems without the need for training because MPIS uses unsupervised machine learning with a few physically motivated hyperparameters. We apply MPIS to nanoscale x-ray absorption near edge structure (XANES) imaging, where XANES spectra are collected with nanometer spatial resolution. We show the superiority of manifold projection over linear transformations, such as the commonly used principal component analysis (PCA). Moreover, MPIS maintains accuracy while reducing computation time and sensitivity to noise compared to the standard nano-XANES imaging analysis procedure. Finally, we demonstrate how multimodal information, such as x-ray fluorescence data and spatial location of pixels, can be incorporated into the MPIS framework. We propose that MPIS is adaptable for any spectral imaging technique, including scanning transmission x-ray microscopy, where the length scale of domains is larger than the resolution of the experiment.

Imaging the space-resolved chemical heterogeneity of degraded graphite anode through scanning transmission X-ray microscope

Deeply understanding the chemical heterogeneity of graphite anode is important because it can provide insights into the underlying mechanisms of electrode degradation and failure in battery systems. Herein, the chemical heterogeneity of graphite anode is imaged by X-ray fluorescence mode scanning transmission X-ray microscope (XRF-STXM) to space-resolve the chemical distribution and structure at C, O, F and Na sites. The synchrotron radiation X-ray photoelectron spectroscopy analysis suggests that the solid-electrolyte-interphase (SEI) layer on graphite anodes contains a complex mixture of both organic (-COOR, -C-OR, etc.) and inorganic species (CO32−, LiF, LixPOyFz, etc.), which can vary with depth. Furthermore, XRF-STXM imaging combined with X-ray absorption spectra is used to map out the heterogeneity in the chemical spatial distribution of SEI composition and its location dependence, as well as its strong correlation with the distribution of conductive additives/binders and binders decomposition. The distribution of SEI exhibits a distinctive feature, with the CO32− and LiF species being significantly thicker at edge plane than at basal plane and the distribution being highly non-uniform. The insights gained from the visualization of the spatial chemical distribution will deepen our understanding of SEI, which is crucial for delineating effective strategies for the development of Li-ion batteries.

Advances in sparse dynamic scanning in spectromicroscopy through compressive sensing.

Scanning microscopies and spectroscopies like X-ray Fluorescence (XRF), Scanning Transmission X-ray Microscopy (STXM), and Ptychography are of very high scientific importance as they can be employed in several research fields. Methodology and technology advances aim at analysing larger samples at better resolutions, improved sensitivities and higher acquisition speeds. The frontiers of those advances are in detectors, radiation sources, motors, but also in acquisition and analysis software together with general methodology improvements. We have recently introduced and fully implemented an intelligent scanning methodology based on compressive sensing, on a soft X-ray microscopy beamline. This demonstrated sparse low energy XRF scanning of dynamically chosen regions of interest in combination with STXM, yielding spectroimaging data in the megapixel-range and in shorter timeframes than were previously not feasible. This research has been further developed and has been applied to scientific applications in biology. The developments are mostly in the dynamic triggering decisional mechanism in order to incorporate modern Machine Learning (ML) but also in the suitable integration of the method in the control system, making it available for other beamlines and imaging techniques. On the applications front, the method was previously successfully used on different samples, from lung and ovarian human tissues to plant root sections. This manuscript introduces the latest methodology advances and demonstrates their applications in life and environmental sciences. Lastly, it highlights the auxiliary development of a mobile application, designed to assist the user in the selection of specific regions of interest in an easy way.

Organomineralization of dolomite in hypersaline microbial mats from Qatar sabkhas visualized by TEM & STXM

Deep insight into the low-temperature mineralization mechanism of dolomite in sediments has remained elusive. This issue is popularly termed “The Dolomite Problem” due to its multifactorial nature. Dolomite has been observed to mineralize in the exopolymeric substances produced by microbial mat communities (Bontognali et al. 2013), where productivity is high. One working hypothesis suggests that degrading organic matter in hypersaline environments releases the necessary component ions, increasing saturation with respect to dolomite (DiLoreto et al. 2019, Dupraz et al. 2009, Petrash et al. 2017). Other models suggest a dissolution-reprecipitation reaction of calcite to dolomite (Rivers 2023). High-resolution micro-spectroscopy techniques (such as transmission electron microscopy, TEM; and scanning transmission X-ray microscopy, STXM) can be used to determine chemical changes in crystals nucleating in a matrix, however to date very little studies have focused on observing dolomite mineralization at the nano-scale. The present study investigates microbial mats collected from hypersaline salt flats in the Persian gulf at micro- to nano-meter scales using high-spatial and -energy resolution TEM (Thermo Scientific Talos 200X at the Canadian Centre for Electron Microscopy) and STXM (PolLux Beamline at the Swiss Light Source at Paul Scherrer Institut), specifically to see changes in carbonate mineralization due to interactions with organic matter. C, Ca and O elemental maps of carbonate crystals were obtained with EDXS (energy-dispersive X-ray spectroscopy) in TEM. These crystals were also indexed by SAED (selected area electron diffraction in TEM). Fine spectral signatures (near-edge X-ray absorption fine structures, or NEXAFS) at the C K-edge (280-290 eV) and Ca L2,3-edge (344-356 eV) in STXM were used to determine the chemical identity of carbonate minerals and surrounding organic matter of the microbial mats. The results of the study show that dolomite nucleates in close association with the organic matter of the mats, where degradation is highest (defined in our adjacent study as the increase in C:N ratio). In TEM, polycrystalline dolomite is seen mineralizing in the matrix of the microbial mat organic material (Fig. 1). In STXM, the identity of the carbonate mineral changes from calcite on the outside to dolomite on the inside of the microbial mat particle (Fig. 2). In addition, our microsensor observations of elevated H2S concentrations, surface oxygenation from oxygenic phototrophy, high reduction potential, high organic carbon, high Mg:Ca ratio and high organic matter degradation (by C:N ratio) in each of the studied microbial mats confirms that the ideal dolomite mineralization conditions according to models of the dolomite problem are present in each case.

Learning heterogeneous reaction kinetics from X-ray videos pixel by pixel

Reaction rates at spatially heterogeneous, unstable interfaces are notoriously difficult to quantify, yet are essential in engineering many chemical systems, such as batteries1 and electrocatalysts2. Experimental characterizations of such materials by operando microscopy produce rich image datasets3–6, but data-driven methods to learn physics from these images are still lacking because of the complex coupling of reaction kinetics, surface chemistry and phase separation7. Here we show that heterogeneous reaction kinetics can be learned from in situ scanning transmission X-ray microscopy (STXM) images of carbon-coated lithium iron phosphate (LFP) nanoparticles. Combining a large dataset of STXM images with a thermodynamically consistent electrochemical phase-field model, partial differential equation (PDE)-constrained optimization and uncertainty quantification, we extract the free-energy landscape and reaction kinetics and verify their consistency with theoretical models. We also simultaneously learn the spatial heterogeneity of the reaction rate, which closely matches the carbon-coating thickness profiles obtained through Auger electron microscopy (AEM). Across 180,000 image pixels, the mean discrepancy with the learned model is remarkably small (<7%) and comparable with experimental noise. Our results open the possibility of learning nonequilibrium material properties beyond the reach of traditional experimental methods and offer a new non-destructive technique for characterizing and optimizing heterogeneous reactive surfaces.

Morphological and lipid metabolism alterations in macrophages exposed to model environmental nanoplastics traced by high-resolution synchrotron techniques.

The release of nanoplastics (NPs) in the environment is a significant health concern for long-term exposed humans. Although their usage has certainly revolutionized several application fields, at nanometer size, NPs can easily interact at the cellular level, resulting in potential harmful effects. Micro/Nanoplastics (M/NPs) have a demonstrated impact on mammalian endocrine components, such as the thyroid, adrenal gland, testes, and ovaries, while more investigations on prenatal and postnatal exposure are urgently required. The number of literature studies on the NPs' presence in biological samples is increasing. However, only a few offer a close study on the model environmental NP-immune system interaction exploited by advanced microscopy techniques. The present study highlights substantial morphological and lipid metabolism alterations in human M1 macrophages exposed to labeled polypropylene and polyvinyl chloride nanoparticles (PP and PVC NPs) (20 μg/ml). The results are interpreted by advanced microscopy techniques combined with standard laboratory tests and fluorescence microscopy. We report the accurate detection of polymeric nanoparticles doped with cadmium selenide quantum dots (CdSe-QDs NPs) by following the Se (L line) X-ray fluorescence emission peak at higher sub-cellular resolution, compared to the supportive light fluorescence microscopy. In addition, scanning transmission X-ray microscopy (STXM) imaging successfully revealed morphological changes in NP-exposed macrophages, providing input for Fourier transform infrared (FTIR) spectroscopy analyses, which underlined the chemical modifications in macromolecular components, specifically in lipid response. The present evidence was confirmed by quantifying the lipid droplet (LD) contents in PP and PVC NPs-exposed macrophages (0-100 μg/ml) by Oil Red O staining. Hence, even at experimental NPs' concentrations and incubation time, they do not significantly affect cell viability; they cause an evident lipid metabolism impairment, a hallmark of phagocytosis and oxidative stress.

Bifunctional Oxygen Electrocatalysis on Manganese Oxide

Limited supply of precious metals impedes the scale up of electrolyzer production. To enable 100s of GWs of PEM electrolyzer capacity by 2030, iridium supply must grow by more than 10x.[1] Alternatively, catalysts made of cheaper, more abundant manganese could relieve these constraints, if engineered to have comparable activity and stability. The unique bifunctional OER/ORR activity of Mn oxide could also enable electrolyzers that both produce and consume fuel with a single catalyst. Yet rational design of Mn oxide catalysts requires a better understanding of the structural and chemical motifs that lead to high bifunctional performance.In this talk, we will discuss our investigation of the bifunctional OER & ORR activity of Mn oxide and its unusual pH dependence. Our model system, 𝛼-KxMnO2, is among the best reported Mn oxide catalysts for both the OER and the ORR, with ORR activity matching that of Pt.[2] While the OER activity of Mn oxide has been shown to increase at higher pH,[3] we will show that its ORR activity improves as well. We will discuss our attempts to understand this phenomenon with operando scanning transmission x-ray microscopy (STXM), which enables spectroscopic investigation of single catalyst particles during reaction with spatial resolution down to 25 nm. Complementary surface DFT calculations provide further evidence for identification of the active crystal facets and insights into the pH-dependency of the OER & ORR mechanisms. We will discuss the implications of this work on the design of bidirectional electrolyzers with low-cost, non-precious metal catalysts.[1] IRENA. Green Hydrogen Cost Reduction. 2020 [2] Meng, Y. et al. J. Am. Chem. Soc. 2014, 136 (32), 11452–11464.[3] Takashima, T. et al. J. Am. Chem. Soc. 2012, 134 (3), 1519–1527.

Interfacial Challenge for Solid-State Lithium Batteries- Liquid Addition

All solid-state lithium batteries with garnet electrolytes (Li7La3Zr2O12, LLZO) are promising energy storage devices that have gained increasing attention due to their huge potential towards non-flammability and higher energy density. However, reported solid-state lithium batteries cannot achieve the projected energy density (> 500 Wh/kg at the cell level) mainly due to insufficient contact and poor compatibility between LLZO and electrodes. The use of liquid electrolytes in small quantities has been suggested as a component in the quasi-solid hybrid electrolytes to address these two issues. However, the working principle of liquid electrolytes added as the interface inside the batteries is not clear yet.This study added 10L carbonate-based liquid electrolyte between LLZO and LiNi0.6Mn0.6Co0.2O2 (NMC 622) cathode. The assembled Li|LLZO|NMC 622 cell exhibited an initial discharge capacity of 168 mAh g-1 with a capacity retention ratio of ~82 % after 28 cycles. Scanning Transmission X-ray Microscopy revealed the reaction of LE with garnet and NMC 622. More importantly, the LE decomposed and solidified during the cycling process. Decomposed LE participated in the formation of a newly-identified solid-liquid electrolyte interface (SLEI) just after the 1st cycle. Furthermore, the X-ray Absorption Spectroscopy results indicated that the SLEI consisted predominantly of LiF, LaF3, Li2O, and Li2CO3 species.Overall, this study proved the solidification of liquid electrolytes at the garnet/cathode interface. The formation of SLEI effectively suppressed the degradation of the garnet electrolyte and stabilized the battery cycling performance. More efforts are required to optimize the liquid and establish a more stable SLEI that could expand the cycling life of the batteries.

STXM – scanning transmission X-ray microscopy

STXM – scanning transmission X-ray microscopy

Direct observation of Néel-type skyrmions and domain walls in a ferrimagnetic DyCo3 thin film

Isolated magnetic skyrmions are stable, topologically protected spin textures that are at the forefront of research interests today due to their potential applications in information technology. A distinct class of skyrmion hosts are rare earth - transition metal (RE-TM) ferrimagnetic materials. To date, the nature and the control of basic traits of skyrmions in these materials are not fully understood. We show that for an archetypal ferrimagnetic material DyCo3 that exhibits a strong perpendicular anisotropy, the ferrimagnetic skyrmion size can be tuned by an external magnetic field. Moreover, by taking advantage of the high spatial resolution of scanning transmission X-ray microscopy (STXM) and utilizing a large x-ray magnetic linear dichroism (XMLD) contrast that occurs naturally at the RE resonant edges, we resolve the nature of the magnetic domain walls of ferrimagnetic skyrmions. We demonstrate that through this method one can easily discriminate between Bloch and Néel type domain walls for each individual skyrmion. For all isolated ferrimagnetic skyrmions, we observe that the domain walls are of Néel-type. This key information is corroborated with results of micromagnetic simulations and allows us to conclude on the nature of the Dzyaloshinskii-Moriya interaction (DMI) which concurs to the stabilisation of skyrmions in this ferrimagnetic system. Establishing that an intrinsic DMI occurs in RE-TM materials will also be beneficial towards a deeper understanding of chiral spin texture control in ferrimagnetic materials.

Nitrogen-Rich Organic Matter Formation and Stabilization in Iron Ore Tailings: A Submicrometer Investigation.

Organic matter (OM) formation and stabilization are critical processes in the eco-engineered pedogenesis of Fe ore tailings, but the underlying mechanisms are unclear. The present 12 month microcosm study has adopted nanoscale secondary ion mass spectrometry (NanoSIMS) and synchrotron-based scanning transmission X-ray microscopy (STXM) techniques to investigate OM formation, molecular signature, and stabilization in tailings at micro- and nanometer scales. In this system, microbial processing of exogenous isotopically labeled OM demonstrated that 13C labeled glucose and 13C/15N labeled plant biomass were decomposed, regenerated, and associated with Fe-rich minerals in a heterogeneous pattern in tailings. Particularly, when tailings were amended with plant biomass, the 15N-rich microbially derived OM was generated and bound to minerals to form an internal organo-mineral association, facilitating further OM stabilization. The organo-mineral associations were primarily underpinned by interactions of carboxyl, amide, aromatic, and/or aliphatic groups with weathered mineral products derived from biotite-like minerals in fresh tailings (i.e., with Fe2+ and Fe3+) or with Fe3+ oxyhydroxides in aged tailings. The study revealed microbial OM generation and subsequent organo-mineral association in Fe ore tailings at the submicrometer scale during early stages of eco-engineered pedogenesis, providing a basis for the development of microbial based technologies toward tailings' ecological rehabilitation.

Combined Electrochemical, XPS, and STXM Study of Lithium Nitride as a Protective Coating for Lithium Metal and Lithium-Sulfur Batteries.

Li3N is an excellent protective coating material for lithium electrodes with very high lithium-ion conductivity and low electronic conductivity, but the formation of stable and homogeneous coatings is technically very difficult. Here, we show that protective Li3N coatings can be simply formed by the direct reaction of electrodeposited lithium electrodes with N2 gas, whereas using battery-grade lithium foil is problematic due to the presence of a native passivation layer that hampers that reaction. The protective Li3N coating is effective at preventing lithium dendrite formation, as found from unidirectional plating and plating-stripping measurements in Li-Li cells. The Li3N coating also efficiently suppresses the parasitic reactions of polysulfides and other electrolyte species with the lithium electrode, as demonstrated by scanning transmission X-ray microscopy, X-ray photoelectron spectroscopy, and optical microscopy. The protection of the lithium electrode against corrosion by polysulfides and other electrolyte species, as well as the promotion of smooth deposits without dendrites, makes the Li3N coating highly promising for applications in lithium metal batteries, such as lithium-sulfur batteries. The present findings show that the formation of Li3N can be achieved with lithium electrodes covered by a secondary electrolyte interface layer, which proves that the in situ formation of Li3N coatings inside the batteries is attainable.

Physicochemical characterization of free troposphere and marine boundary layer ice-nucleating particles collected by aircraft in the eastern North Atlantic

Abstract. Atmospheric ice nucleation impacts the hydrological cycle and climate by modifying the radiative properties of clouds. To improve our predictive understanding of ice formation, ambient ice-nucleating particles (INPs) need to be collected and characterized. Measurements of INPs at lower latitudes in a remote marine region are scarce. The Aerosol and Cloud Experiments in the Eastern North Atlantic (ACE-ENA) campaign, in the region of the Azores islands, provided the opportunity to collect particles in the marine boundary layer (MBL) and free troposphere (FT) by aircraft during the campaign's summer and winter intensive operation period. The particle population in samples collected was examined by scanning transmission X-ray microscopy with near-edge X-ray absorption fine structure spectroscopy. The identified INPs were analyzed by scanning electron microscopy with energy-dispersive X-ray analysis. We observed differences in the particle population characteristics in terms of particle diversity, mixing state, and organic volume fraction between seasons, mostly due to dry intrusion events during winter, as well as between the sampling locations of the MBL and FT. These differences are also reflected in the temperature and humidity conditions under which water uptake, immersion freezing (IMF), and deposition ice nucleation (DIN) proceed. Identified INPs reflect typical particle types within the particle population on the samples and include sea salt, sea salt with sulfates, and mineral dust, all associated with organic matter, as well as carbonaceous particles. IMF and DIN kinetics are analyzed with respect to heterogeneous ice nucleation rate coefficients, Jhet, and ice nucleation active site density, ns, as a function of the water criterion Δaw. DIN is also analyzed in terms of contact angles following classical nucleation theory. Derived MBL IMF kinetics agree with previous ACE-ENA ground-site INP measurements. FT particle samples show greater ice nucleation propensity compared to MBL particle samples. This study emphasizes that the types of INPs can vary seasonally and with altitude depending on sampling location, thereby showing different ice nucleation propensities, which is crucial information when representing mixed-phase cloud and cirrus cloud microphysics in models.

Domain wall motion at low current density in a synthetic antiferromagnet nanowire

The current-driven motion of magnetic domain walls (DWs) is the working principle of magnetic racetrack memories. In this type of spintronic technology, high current densities are used to propel DW motion in magnetic nanowires, causing significant wire heating that corresponds to wasted energy. Synthetic antiferromagnets are known to show very fast DW motion at high current densities, but lower current densities around onset of motion have received less attention. Here we use scanning transmission x-ray microscopy to study the response of DWs in a SAF multilayer to short current pulses. We observe that the DWs depin at A m−2 and move more quickly in response to 5 ns duration current pulses than in comparable multilayers that lack antiferromagnetic coupling. The results suggest that DWs in SAF structures are superior to conventional Néel DWs for low energy consumption racetrack technologies.

Scanning transmission X-ray microscopy at the Advanced Light Source

Over 50 years of development, synchrotron based X-ray microscopy has become a routine and powerful tool for the analysis of nanoscale structure and chemistry in many areas of science. Scanning X-ray microscopy is particularly well suited to the study of chemical and magnetic states of matter and has become available at most synchrotron light sources using a variety of optical schemes, detectors and sample environments. The Advanced Light Source at Lawrence Berkeley National Laboratory has an extensive program of soft X-ray scanning microscopy which supports a broad range of scientific research using a suite of advanced tools for high spatio-temporal resolution and control of active materials. Instruments operating within an energy range between 200–2500 eV with spatial resolution down to 7 nm and sub 20 picosecond time resolution are available. These capabilities can be routinely used in combination with a variety of sample stimuli, including gas or fluid flow, temperature control from 100 to 1200 K, DC bias and pulsed or continuous microwave excitation. We present here a complete survey of our instruments, their most advanced capabilities and a perspective on how they complement each other to solve complex problems in energy, materials and environmental science.

Quantitative mapping of calcium cell reservoirs in cyanobacteria at the submicrometer scale

Calcium plays an important role in the physiology of bacterial cells and as a free soluble form inside the cells, it is tightly regulated at a low concentration. However, much higher amounts of stored calcium exist within cells and can be remobilized at diverse occasions. As a consequence, there has been a variety of techniques developed to quantitatively map the different forms of Ca in cells. Here we show how scanning transmission x-ray microscopy (STXM), a synchrotron-based microscopy technique, conducted in the soft x-ray range at the Ca L2,3 edges (340–360 eV) offers an original and informative quantitative view of different Ca reservoirs in bacterial cells at a spatial resolution better than 100 nm. To illustrate this, we analyzed mutants of the cyanobacterium Synechococcus elongatus PCC 7942, overexpressing different versions of a gene called ccyA from two phylogenetically distant cyanobacteria: Gloeomargarita lithophora and Synechococcus sp. PCC 6312. This gene is diagnostic of the capability of some cyanobacteria to form intracellular amorphous calcium carbonate (iACC) but its function remains unknown. Here we show that the overexpression of the ccyA gene in the iACC non-forming cyanobacterium S. elongatus PCC 7942 results in an increased Ca content, especially in some Ca-rich cells. Moreover, we show that STXM can discriminate four different reservoirs of Ca in cyanobacteria and provides quantitative assessment of their relative importance.

Waste biomass from hypersaline potash mining byproducts: Detection and visualization of Cu(II) and Cr(VI) on Croceicoccus sp. FTI14 biosorbent

Microorganisms in hypersaline potash mining byproducts and their potential environmental applications have not been extensively reported. This study reports the diverse waste-impacted microbial communities (archaea and bacteria) adapted to extreme salinity (>10–25%). Of these, halotolerant Croceicoccus sp. FTI14 was investigated as a biosorbent for removing dissolved Cu(II) and Cr(VI) from synthetic Cu(II) and Cr(VI)-contaminated DI, groundwater and saline groundwater (0.55 M ionic strength). FTI14 biomass was oven-dried, finely ground, and investigated in batch biosorption experiments. At initial metal concentrations of 40 mg/L, FTI14 removed 40 ± 0.7% (16.3 ± 0.5 mg/g) and 19 ± 0.1% (7.8 ± 0.1 mg/g) of the Cu(II) from deionized water and saline groundwater, respectively, while only 22.9 ± 0.7% (9.6 ± 0.2 mg/g) and 2.1 ± 0.6% (1.0 ± 0.3 mg/g) Cr(VI) removal was achieved. Cu(II) uptake (mg/g) exceeded Cr(VI) uptake by a factor of 1.7–7.8. Langmuir and Freundlich models were applied on FTI14 biosorption isotherm data. The Freundlich model showed a better fit for both Cu(II) and Cr(VI), as indicated by the AIC values compared with evidence ratios. Synchrotron-based scanning transmission X-ray microscopy (STXM) visualizations of the biosorbent showed a mixture of whole cells and indistinct biomass and a spatial association between metals and biomass. Metal exposure alters the amide functional groups peak in Fourier transform Infra-red (FTIR) spectra, suggesting its role in sorption process. Thus, this study indicates culturable halotolerant microorganisms from hypersaline potash mining byproducts and its potential as biosorbent applications for metal removal from impacted groundwater.

Atomically dispersed Ni-N-C electrocatalysts, studied by Ni L-edge spectro-ptychography

Soft X-ray spectro-ptychography of nickel-nitrogen-carbon electrocatalysts containing atomically dispersed Ni-based active sites were measured at the Ni L3 edge. Samples prepared with two different loadings of Ni precursors were investigated and compared to the results of an earlier study using scanning transmission X-ray microscopy (STXM) [Zhang et al., ACS Catalysis 12 (2022) 8746]. The ptychography data sets were measured using a defocused probe (1–3 µm). The spatial resolution was improved from ∼60 nm (STXM) to ∼20 nm (ptychography). Spectro-ptychography stacks were measured at 4 component-specific energies (4-E stack) and at many energies across the full Ni L3 edge (34-E stack). Maps of three key chemical components (Ni metal, Ni3S2, and atomically dispersed N-coordinated Ni catalyst sites) were derived by fits of suitable reference spectra to absorption signals derived from the amplitude images from ptychographic reconstruction. The spectro-ptychography 4-E and 34-E stacks gave chemical mapping similar to each other and to the earlier STXM results. The phase signals obtained from the same data set and reconstruction were also found to be analyzable using reference phase spectra extracted from the phase stack, which generated chemical maps similar to those based on ptychography amplitude data. By using a defocused probe, the radiation dose and acquisition times for spectro-ptychography are comparable to conventional STXM, but significantly improved spatial resolution was achieved. This study highlights the added value of spectro-ptychography relative to STXM for studies of electrocatalysts.

Scanning transmission soft X-ray spectromicroscopy of mouse kidney and liver

Scanning transmission X-ray microscopy (STXM) in the soft X-ray range is well-suited to study ultrastructural features of mammalian soft tissues. Especially at the carbon 1s edge, the imaging contrast varies drastically across the edge due to rapid changes in the X-ray absorption cross-section of functional groups present in the tissue samples enabling label-free soft X-ray spectromicroscopic studies. We present STXM spectromicroscopic imaging of mouse kidney and liver tissues. We especially concentrate on ultrastructural abnormalities in genetically modified Slc17a5 mice. STXM is a promising technique to study storage diseases without chemical alteration due to staining agents, but sample preparation poses a challenge.