{"title":"Developments in sample environment for a scanning transmission X-ray microscope at UVSOR-III synchrotron","authors":"Takuji Ohigashi , Nobuhiro Kosugi","doi":"10.1016/j.elspec.2023.147356","DOIUrl":"10.1016/j.elspec.2023.147356","url":null,"abstract":"<div><p><span>The beamline, BL4U, in UVSOR-III </span>Synchrotron<span> is dedicated to scanning transmission X-ray microscopy (STXM) based on 2-dimensional soft X-ray absorption and has been in operation since 2013, to enable both academic and industrial users to carry out advanced chemical analysis under various sample environments. In this paper, we have summarized our major developments for the last decade; especially, expansion of the photon energy range down to the Li K-edge (55 eV), sample cryo-cooling to reduce radiation damage, 3-dimensional computer tomography, and air-free sample transfer.</span></p></div>","PeriodicalId":15726,"journal":{"name":"Journal of Electron Spectroscopy and Related Phenomena","volume":"266 ","pages":"Article 147356"},"PeriodicalIF":1.9,"publicationDate":"2023-07-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"47774751","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"物理与天体物理","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Peter Guttmann , Carla Bittencourt , Stephan Werner , Stefan Rehbein , Christoph Pratsch , Gerd Schneider
{"title":"Nanoscale spectromicroscopy with the full-field X-ray microscope at the BESSY II electron storage ring in the soft and tender X-ray range","authors":"Peter Guttmann , Carla Bittencourt , Stephan Werner , Stefan Rehbein , Christoph Pratsch , Gerd Schneider","doi":"10.1016/j.elspec.2023.147344","DOIUrl":"10.1016/j.elspec.2023.147344","url":null,"abstract":"<div><p><span>In this paper, we give an overview of the nanoscale spectromicroscopy studies performed with the full-field X-ray microscope at the BESSY II electron storage ring. We do not consider spectromicroscopy studies performed with X-ray microscopes operated at other </span>synchrotron<span><span> sources. Such studies can be found in the literature. To our knowledge, the full-field X-ray microscope at the BESSY II storage ring is the first one operating with both a plane-grating-monochromator (PGM) beamline equipped with multi-layer </span>optics<span> for the tender X-ray range, as well as with standard optical elements for the soft X-ray range. We discuss how this instrument has been used in various published NEXAFS-TXM studies to probe low dimensional nanostructures. This research work paves the way for understanding electronic structures approaching the atomic scale, and will thereby help in the design of tailored functional systems.</span></span></p></div>","PeriodicalId":15726,"journal":{"name":"Journal of Electron Spectroscopy and Related Phenomena","volume":"266 ","pages":"Article 147344"},"PeriodicalIF":1.9,"publicationDate":"2023-07-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"42832309","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"物理与天体物理","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Haeyeon Jun , Chloé Dindault , Denis Tondelier , Bernard Geffroy , Ileana Florea , Jean-Eric Bouree , Philip Schulz , Yvan Bonnassieux , Sufal Swaraj
{"title":"On the use of soft X-ray STXM for organic-inorganic halide perovskite photovoltaic materials","authors":"Haeyeon Jun , Chloé Dindault , Denis Tondelier , Bernard Geffroy , Ileana Florea , Jean-Eric Bouree , Philip Schulz , Yvan Bonnassieux , Sufal Swaraj","doi":"10.1016/j.elspec.2023.147358","DOIUrl":"10.1016/j.elspec.2023.147358","url":null,"abstract":"<div><p><span><span>Metal-halide perovskites<span> are complex materials with outstanding optoelectronic properties. Thus it is of interest to analyze these materials by using every available research tool. </span></span>Synchrotron<span> tools have played an important role in fundamental and applied research for decades. Many synchrotron-based hard X-ray tools are already providing effective feedback to the perovskite solar cell (PSC) research community. With several fourth-generation light sources up and running or under development, this contribution will continue to impact every aspect of scientific advancement including PSC research. Arguably, the contribution of soft X-rays in PSC research is relatively limited. In view of the developments in the synchrotron world and the fact that a multimethod approach, combining laboratory-based techniques as well as synchrotron-based techniques, is necessary to provide constructive feedback to the PSC community we present here a collection of arguments and procedures with the aim of highlighting the use of soft X-ray scanning transmission X-ray microscopy (STXM). Some aspects of these arguments are elaborated with STXM investigation of perovskite material formamidinium-methylammonium lead iodide (FA</span></span><sub>1−x</sub>MA<sub>x</sub>PbI<sub>3</sub>).</p></div>","PeriodicalId":15726,"journal":{"name":"Journal of Electron Spectroscopy and Related Phenomena","volume":"266 ","pages":"Article 147358"},"PeriodicalIF":1.9,"publicationDate":"2023-07-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"45526239","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"物理与天体物理","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
{"title":"Soft X-ray scanning transmission microscopy as a selective probe of topical dermal drug delivery: The role of petrolatum and occlusion","authors":"Gregor Germer , Takuji Ohigashi , Hayato Yuzawa , Nobuhiro Kosugi , Roman Flesch , Fiorenza Rancan , Annika Vogt , Eckart Rühl","doi":"10.1016/j.elspec.2023.147343","DOIUrl":"10.1016/j.elspec.2023.147343","url":null,"abstract":"<div><p><span>Selective and label-free probing of drugs by scanning transmission X-ray microscopy (STXM) is applied along with hyperspectral imaging to probe topically applied drugs in human skin explants </span><em>ex vivo</em><span>. A comparison of data evaluation strategies is reported, which includes changes in optical density at selected photon energies in the O 1 s regime, linear combination modeling using reference spectra, as well as principal component and cluster analyses. It is shown that consistent results are obtained from linear combination modeling of reference spectra and changes in optical density. The dermal penetration of the anti-inflammatory drug rapamycin is investigated with high spatial resolution using a petrolatum-based formulation. For such well-known formulation the result of occlusion is investigated leading to drug uptake into corneocytes. Additional changes in drug penetration induced by weakening the skin barrier by the serine protease trypsin are also included. These results are discussed in comparison with the dermal penetration of other drug formulations. Finally, alternatives to present data acquisition strategies in STXM are discussed with respect to sub-sampling in combination with mathematical approaches, so that the full chemical and spatial information can be retrieved and radiation damage is minimized.</span></p></div>","PeriodicalId":15726,"journal":{"name":"Journal of Electron Spectroscopy and Related Phenomena","volume":"266 ","pages":"Article 147343"},"PeriodicalIF":1.9,"publicationDate":"2023-07-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"43902152","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"物理与天体物理","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Artem Mikhailov , Tatyana Asanova , Igor Asanov , Igor Píš , Elena Magnano , Gennadiy Kostin , Dominik Schaniel
{"title":"N, O and F K-edges XAS and DFT combination for the exploration of linkage isomers of coordinated nitric oxide in a ruthenium nitrosyl complex","authors":"Artem Mikhailov , Tatyana Asanova , Igor Asanov , Igor Píš , Elena Magnano , Gennadiy Kostin , Dominik Schaniel","doi":"10.1016/j.elspec.2023.147342","DOIUrl":"10.1016/j.elspec.2023.147342","url":null,"abstract":"<div><p><span>We report on the experimental investigation of single crystals of </span><em>trans</em>-[RuNOPy<sub>4</sub>F](ClO<sub>4</sub>)<sub>2</sub> (<strong>1</strong><span><span>) in its ground state (GS). The X-ray absorption spectroscopy<span> (XAS) spectra measured at the N, O and F K-edges were compared to TDDFT calculations to identify and assign the absorption peaks, and to elucidate the structures of coordinated </span></span>nitric oxide (NO). Based on a reasonable match of experimental and calculated spectra of GS, the N, O and F K-edges XAS spectra of Ru-ON (MS1) and Ru-η</span><sup>2</sup>-(NO) (MS2) isomers of <strong>1</strong><span> were calculated. According to the calculations, the energy or/and intensity of the 1 s→LUMO, LUMO+ 1 peaks of N, O or F K-edge changes significantly after GS isomerization to both MS1 and MS2. Current theoretical modeling of the NO linkage isomer in </span><strong>1</strong> is a background for the future investigation of isomerization process of NO by XAS methods. Since the investigated isomerization occurs in a variety of different nitrosyl complexes, obtained results can be extrapolated to a large family of transition metal nitrosyl compounds.</p></div>","PeriodicalId":15726,"journal":{"name":"Journal of Electron Spectroscopy and Related Phenomena","volume":"266 ","pages":"Article 147342"},"PeriodicalIF":1.9,"publicationDate":"2023-07-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"42374186","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"物理与天体物理","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
{"title":"Analysis of X-ray images and spectra (aXis2000): A toolkit for the analysis of X-ray spectromicroscopy data","authors":"Adam P. Hitchcock","doi":"10.1016/j.elspec.2023.147360","DOIUrl":"10.1016/j.elspec.2023.147360","url":null,"abstract":"<div><p>Spectromicroscopy refers to analytical methods that combine imaging and spectroscopy to provide detailed, spatially resolved analytical information about a sample, such as the type and quantitative spatial distributions of chemical components, geometric or magnetic alignment information, crystal structure, etc. The analysis of X-ray images and spectra (aXis2000) software described in this work provides a set of routines within a single, integrated, graphical-oriented package to read, display, manipulate and analyze spectromicroscopy data, with particular focus on soft X-ray spectromicroscopy methods such as scanning transmission X-ray microscopy (STXM), X-ray photoemission electron microscopy (XPEEM), scanning photoelectron X-ray microscopy (SPEM) and transmission X-ray microscopy (TXM). Here, this free software is described and compared to other software that can provide similar or complementary capabilities. Examples of spectromicroscopic analyses using advanced features of aXis2000 are provided.</p></div>","PeriodicalId":15726,"journal":{"name":"Journal of Electron Spectroscopy and Related Phenomena","volume":"266 ","pages":"Article 147360"},"PeriodicalIF":1.9,"publicationDate":"2023-07-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"49090380","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"物理与天体物理","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Vladimir I. Kelemen , Sándor Demes , Eugene Yu. Remeta
{"title":"Theoretical study of elastic electron scattering by zinc atoms in the framework of relativistic optical potential model","authors":"Vladimir I. Kelemen , Sándor Demes , Eugene Yu. Remeta","doi":"10.1016/j.elspec.2023.147365","DOIUrl":"10.1016/j.elspec.2023.147365","url":null,"abstract":"<div><p>A theoretical study of integral and differential cross sections as well as of spin-polarization effects is reported for elastic electron scattering by zinc atoms at collision energies up to 3 keV. It has been shown that a <em>P</em>-wave shape resonance appears in the low-energy range of the integral cross sections. Its energy is about 0.19 and 0.20 eV, while its width is about 0.309 and 0.356 eV for the <em>j</em> = 3/2 and <em>j</em> = 1/2 total angular momentum of the electron, respectively. The differential cross sections of scattering and the Sherman-functions <span><math><mrow><mi>S</mi><mo>(</mo><mi>E</mi><mo>,</mo><mi>θ</mi><mo>)</mo></mrow></math></span> are computed by the parameter-free complex optical potential method. The calculated data are in a good overall agreement with the available experimental and theoretical data in the literature. The energy and angular positions have been located for five critical minima in the differential cross sections. The low-energy minimum is located at [6.63 eV; 102.34°], while the high-energy minimum is at [347.53 eV; 124.11°]. Ten points for the scattered electrons' total spin-polarization (<span><math><mrow><mi>S</mi><mo>=</mo><mo>±</mo><mn>1</mn></mrow></math></span>) have been found in the vicinity of the critical minima along with the energy and the angular widths of the spin-polarization peaks (where <span><math><mrow><mo>|</mo><mi>S</mi><mo>|</mo></mrow><mo>≥</mo><mn>0.9</mn></math></span>).</p></div>","PeriodicalId":15726,"journal":{"name":"Journal of Electron Spectroscopy and Related Phenomena","volume":"266 ","pages":"Article 147365"},"PeriodicalIF":1.9,"publicationDate":"2023-07-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"44728785","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"物理与天体物理","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
{"title":"ANTARES: Space-resolved electronic structure","authors":"J. Avila, S. Lorcy, P. Dudin","doi":"10.1016/j.elspec.2023.147362","DOIUrl":"10.1016/j.elspec.2023.147362","url":null,"abstract":"<div><p><span><span>The spatially resolved ARPES<span> (nanoARPES) is a development of conventional ARPES technique achieved with the focusing of light on the sample into the spot with submicron sizes. This development is used in research of essentially small samples, for example, heterostructures build of flakes of 2D materials<span>, micro-crystals or polycrystalline samples, different crystal termination, domains in electronic structure. ANTARES is delivering the nanoARPES technique to user community since 2010, up to now the instrument was used with samples of various types, and that was useful to accumulate the specific experience. In this paper we report the current layout and actual performance of the ANTARES instrument at </span></span></span>Synchrotron<span> SOLEIL, as well as the most typical application areas. The most important and recent upgrades include focusing optics and in-operando setup. The new optical units deliver the increased flux on sample as well as the option to vary the photon energy. The in-operando setup offers the option of electrical connection to the sample being studied with nanoARPES, that promises various applications, where the most demanded now is the control of charge carrier density with applied voltage. This “gate-doping” is often applied to the heterostructures of 2D materials, that could be designed and build on purpose. The 2D heterostructures is probably the most typical field of application of the instrument, with or without </span></span><em>in-operando</em> option. At the same time the use case of the ANTARES instrument is still in the development by the realisation of new kinds of samples and of the new types of the experiments.</p></div>","PeriodicalId":15726,"journal":{"name":"Journal of Electron Spectroscopy and Related Phenomena","volume":"266 ","pages":"Article 147362"},"PeriodicalIF":1.9,"publicationDate":"2023-07-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"45313515","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"物理与天体物理","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Juwon Kim , Danwon Lee , Chihyun Nam , Jinkyu Chung , Bonho Koo , Namdong Kim , Jongwoo Lim
{"title":"Energy material analysis via in-situ/operando scanning transmission x-ray microscopy: A review","authors":"Juwon Kim , Danwon Lee , Chihyun Nam , Jinkyu Chung , Bonho Koo , Namdong Kim , Jongwoo Lim","doi":"10.1016/j.elspec.2023.147337","DOIUrl":"10.1016/j.elspec.2023.147337","url":null,"abstract":"<div><p><span>The development of advanced energy systems is essential for replacing fossil fuel-based societies, and progress in the fundamental understanding of solid-state energy materials has revolutionized this field. In particular, investigating the inhomogeneity of reactions in energy systems requires analysis at the level of individual particles, which are the smallest units in the system. Synchrotron-based scanning transmission X-ray microscopy (STXM) is a valuable tool for exploring reaction and degradation mechanisms, and providing nanoscale site-specific information on chemical and structural changes within single particles. In-situ/operando </span>STXM is particularly useful for observing reactions under well-controlled conditions in real time, thus providing insights into local phenomena obscured by the ensemble effect. This review highlights the research achievements of in-situ/operando STXM in the field of energy materials and provides perspectives for advanced X-ray imaging techniques that can further enhance STXM capabilities.</p></div>","PeriodicalId":15726,"journal":{"name":"Journal of Electron Spectroscopy and Related Phenomena","volume":"266 ","pages":"Article 147337"},"PeriodicalIF":1.9,"publicationDate":"2023-07-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"48063124","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"物理与天体物理","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Andrei Kolmakov , J. Trey Diulus , Kurt D. Benkstein , Steve Semancik , Majid Kazemian , Matteo Amati , Maya Kiskinova , Luca Gregoratti
{"title":"Operando photoelectron spectromicroscopy of nanodevices: Correlating the surface chemistry and transport in SnO2 nanowire chemiresistors","authors":"Andrei Kolmakov , J. Trey Diulus , Kurt D. Benkstein , Steve Semancik , Majid Kazemian , Matteo Amati , Maya Kiskinova , Luca Gregoratti","doi":"10.1016/j.elspec.2023.147366","DOIUrl":"10.1016/j.elspec.2023.147366","url":null,"abstract":"<div><p><span><span>With size reduction of active elements in microelectronics to tens of nanometers and below, the effect of surface and interface properties on overall device performance becomes crucial. High resolution spectroscopic and imaging techniques provide a metrological route for characterization of these properties relevant to </span>device diagnostics<span> and failure analysis. With its roughly 100 nm spatial resolution, superior surface sensitivity, and approximately 200 meV spectral resolution, scanning photoelectron<span> microscopy (SPEM) stands out as a comprehensive tool to access the surface/interface composition of nanodevices, as well to provide chemical state designations and materials property evolutions upon treatment by thermal, electrical, chemical, radiative and other stimuli. Here we present a SPEM-on-device setup that combines X-ray spectromicroscopy with advanced NIST microhotplate technology to demonstrate new combined analytical and electrical measurements capabilities of this metrology platform for </span></span></span><em>operando</em> nanodevice characterization. Using model integrated SnO<sub>2</sub><span> nanowire (NW) chemiresistor devices, the chemically induced alterations in the chemical state of the nanowire surface are correlated to the observed conductance changes, thus directly testing the receptor and transduction mechanisms for SnO</span><sub>2</sub> NW conductometric chemical sensors.</p></div>","PeriodicalId":15726,"journal":{"name":"Journal of Electron Spectroscopy and Related Phenomena","volume":"266 ","pages":"Article 147366"},"PeriodicalIF":1.9,"publicationDate":"2023-07-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"42556502","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"物理与天体物理","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}