Christoph J Sahle, Marta Majkut, Kari O Ruotsalainen, Florent Gerbon, Noora Suomalainen, Marie Claire Lagier, Blanka Detlefs, Laurent Claustre, Alessandro Mirone, Alessandro Longo
{"title":"A miniature X-ray diffraction setup on ID20 at the European Synchrotron Radiation Facility.","authors":"Christoph J Sahle, Marta Majkut, Kari O Ruotsalainen, Florent Gerbon, Noora Suomalainen, Marie Claire Lagier, Blanka Detlefs, Laurent Claustre, Alessandro Mirone, Alessandro Longo","doi":"10.1107/S1600577524009147","DOIUrl":"10.1107/S1600577524009147","url":null,"abstract":"<p><p>We describe an ultra-compact setup for in situ X-ray diffraction on the inelastic X-ray scattering beamline ID20 at the European Synchrotron Radiation Facility. The main motivation for the design and construction of this setup is the increasing demand for on-the-fly sample characterization, as well as ease of navigation through a sample's phase diagram, for example subjected to high-pressure and/or high-temperature conditions. We provide technical details and demonstrate the performance of the setup.</p>","PeriodicalId":48729,"journal":{"name":"Journal of Synchrotron Radiation","volume":" ","pages":"1622-1626"},"PeriodicalIF":2.5,"publicationDate":"2024-11-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC11542657/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142511018","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"物理与天体物理","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Anna J Warren, Jose Trincao, Adam D Crawshaw, Emma V Beale, Graham Duller, Andrew Stallwood, Mark Lunnon, Richard Littlewood, Adam Prescott, Andrew Foster, Neil Smith, Guenther Rehm, Sandira Gayadeen, Christopher Bloomer, Lucia Alianelli, David Laundy, John Sutter, Leo Cahill, Gwyndaf Evans
{"title":"VMXm - A sub-micron focus macromolecular crystallography beamline at Diamond Light Source.","authors":"Anna J Warren, Jose Trincao, Adam D Crawshaw, Emma V Beale, Graham Duller, Andrew Stallwood, Mark Lunnon, Richard Littlewood, Adam Prescott, Andrew Foster, Neil Smith, Guenther Rehm, Sandira Gayadeen, Christopher Bloomer, Lucia Alianelli, David Laundy, John Sutter, Leo Cahill, Gwyndaf Evans","doi":"10.1107/S1600577524009160","DOIUrl":"10.1107/S1600577524009160","url":null,"abstract":"<p><p>VMXm joins the suite of operational macromolecular crystallography beamlines at Diamond Light Source. It has been designed to optimize rotation data collections from protein crystals less than 10 µm and down to below 1 µm in size. The beamline has a fully focused beam of 0.3 × 2.3 µm (vertical × horizontal) with a tuneable energy range (6-28 keV) and high flux (1.6 × 10<sup>12</sup> photons s<sup>-1</sup> at 12.5 keV). The crystals are housed within a vacuum chamber to minimize background scatter from air. Crystals are plunge-cooled on cryo-electron microscopy grids, allowing much of the liquid surrounding the crystals to be removed. These factors improve the signal-to-noise during data collection and the lifetime of the microcrystals can be prolonged by exploiting photoelectron escape. A novel in vacuo sample environment has been designed which also houses a scanning electron microscope to aid with sample visualization. This combination of features at VMXm allows measurements at the physical limits of X-ray crystallography on biomacromolecules to be explored and exploited.</p>","PeriodicalId":48729,"journal":{"name":"Journal of Synchrotron Radiation","volume":" ","pages":"1593-1608"},"PeriodicalIF":2.5,"publicationDate":"2024-11-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC11542661/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142548457","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"物理与天体物理","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
David Marco Just, Marcel Brüstle, Simon Guntli, Johannes Mück, Claude Pradervand
{"title":"Upgraded front ends for SLS 2.0 with next-generation high-power diaphragms and slits.","authors":"David Marco Just, Marcel Brüstle, Simon Guntli, Johannes Mück, Claude Pradervand","doi":"10.1107/S160057752400907X","DOIUrl":"10.1107/S160057752400907X","url":null,"abstract":"<p><p>The upgrade of the Swiss Light Source, called SLS 2.0, necessitates comprehensive updates to all 18 user front ends. This upgrade is driven by the increased power of the synchrotron beam, reduced floor space, changing source points, new safety regulations and enhanced beam properties, including a brightness increase by up to a factor of 40. While some existing front-end components are being thoroughly refurbished and upgraded for safety reasons, other components, especially those designed to tailor the new synchrotron beam, are being completely rebuilt. These new designs feature innovative and enhanced cooling systems to manage the high-power load and meet new requirements such as mechanical stability and compact footprints.</p>","PeriodicalId":48729,"journal":{"name":"Journal of Synchrotron Radiation","volume":" ","pages":"1582-1592"},"PeriodicalIF":2.5,"publicationDate":"2024-11-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC11542664/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142478293","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"物理与天体物理","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
M Saleh, M Hedberg, P L Tam, K Spahiu, I Persson, C Ekberg
{"title":"Coprecipitation of Ce(III) oxide with UO<sub>2</sub>.","authors":"M Saleh, M Hedberg, P L Tam, K Spahiu, I Persson, C Ekberg","doi":"10.1107/S1600577524008336","DOIUrl":"10.1107/S1600577524008336","url":null,"abstract":"<p><p>The neutralization of acidic solutions containing U (IV) and Ce (III) at room temperature in glove box atmosphere and in the presence of dithionite results in coprecipitation of these elements as amorphous solid solutions Ce<sub>x</sub>U<sub>1-x</sub>O<sub>2±y</sub>. The solubilities of the precipitates with different mole fractions (x) of Ce(OH)<sub>3</sub> (x = 0.01 or 0.1) were determined in 1 M NaClO<sub>4</sub> solutions between pH 2.2 and 12.8 under reducing conditions. The solids were investigated by a variety of methods (chemical analysis, SEM-EDX, XRD, XPS, XAS) to determine the nature of the solid solutions formed, their composition and the valence state of Ce and U. X-ray photoelectron spectroscopy confirmed the oxidation states of the solids both before and after the equilibration as Ce (III) and U (IV). The amorphous coprecipitates reached equilibrium relatively fast (∼1 week). The release of Ce from the coprecipitates was totally dominated by the release of uranium over the whole pH range. The Ce concentrations decrease slightly with the decrease of Ce content in the solid, suggesting that Ce<sub>x</sub>U<sub>1-x</sub>O<sub>2±y</sub> solids behave thermodynamically as solid solutions. The concentrations of U in equilibrium with the coprecipitate were in excellent agreement with the solubility of UO<sub>2</sub>(s) under reducing conditions reported in the literature. The conditional solubility product of Ce(OH)<sub>3</sub> from the coprecipitate was several orders of magnitude (∼4 in the near neutral pH range and ∼18 in the acidic range) lower than that of pure Ce(OH)<sub>3</sub>(s). The activities and activity coefficients of Ce(OH)<sub>3</sub>(s) in the coprecipitate were also estimated. Activity coefficients are much less than 1, indicating that the mixing of Ce(OH)<sub>3</sub> with UO<sub>2</sub> is highly favorable.</p>","PeriodicalId":48729,"journal":{"name":"Journal of Synchrotron Radiation","volume":" ","pages":"1489-1504"},"PeriodicalIF":2.5,"publicationDate":"2024-11-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC11542660/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142356516","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"物理与天体物理","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
F Capone, O Muntada, J C Ramírez, M J Esplandiu, R Dedryvère, A Grimaud, B Lassalle-Kaiser, D Céolin, F Pérez-Murano, J P Rueff, Jordi Fraxedas
{"title":"Development of hard X-ray photoelectron spectroscopy in liquid cells using optimized microfabricated silicon nitride membranes.","authors":"F Capone, O Muntada, J C Ramírez, M J Esplandiu, R Dedryvère, A Grimaud, B Lassalle-Kaiser, D Céolin, F Pérez-Murano, J P Rueff, Jordi Fraxedas","doi":"10.1107/S1600577524008865","DOIUrl":"10.1107/S1600577524008865","url":null,"abstract":"<p><p>We present first hard X-ray photoelectron spectroscopy (HAXPES) results of aqueous salt solutions and dispersions of gold nanoparticles in liquid cells equipped with specially designed microfabricated thin silicon nitride membranes, with thickness in the 15-25 nm range, mounted in a high-vacuum-compatible environment. The experiments have been performed at the HAXPES endstation of the GALAXIES beamline at the SOLEIL synchrotron radiation facility. The low-stress membranes are fabricated from 100 mm silicon wafers using standard lithography techniques. Platinum alignment marks are added to the chips hosting the membranes to facilitate the positioning of the X-ray beam on the membrane by detecting the corresponding photoemission lines. Two types of liquid cells have been used, a static one built on an Omicron-type sample holder with the liquid confined in the cell container, and a circulating liquid cell, in which the liquid can flow in order to mitigate the effects due to beam damage. We demonstrate that the membranes are mechanically robust and able to withstand 1 bar pressure difference between the liquid inside the cell and vacuum, and the intense synchrotron radiation beam during data acquisition. This opens up new opportunities for spectroscopic studies of liquids.</p>","PeriodicalId":48729,"journal":{"name":"Journal of Synchrotron Radiation","volume":" ","pages":"1505-1513"},"PeriodicalIF":2.5,"publicationDate":"2024-11-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC11542648/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142478288","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"物理与天体物理","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Elisa Borfecchia, Kirill A Lomachenko, Kristina Kvashnina
{"title":"Foreword to the special virtual issue on X-ray spectroscopy to understand functional materials: instrumentation, applications, data analysis.","authors":"Elisa Borfecchia, Kirill A Lomachenko, Kristina Kvashnina","doi":"10.1107/S1600577524008695","DOIUrl":"10.1107/S1600577524008695","url":null,"abstract":"<p><p>Foreword to the virtual focused issue of Journal of Synchrotron Radiation on X-ray spectroscopy to understand functional materials: instrumentation, applications, data analysis.</p>","PeriodicalId":48729,"journal":{"name":"Journal of Synchrotron Radiation","volume":" ","pages":"1417-1419"},"PeriodicalIF":2.5,"publicationDate":"2024-11-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC11542663/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142478289","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"物理与天体物理","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Jiayi Wang, Zheng Dong, Yi Zhang, Wenqiang Hua, Zudeng Wang, Huilong Guo, Yiming Yang, Xiaoxue Bi
{"title":"StreamSAXS: a Python-based workflow platform for processing streaming SAXS/WAXS data.","authors":"Jiayi Wang, Zheng Dong, Yi Zhang, Wenqiang Hua, Zudeng Wang, Huilong Guo, Yiming Yang, Xiaoxue Bi","doi":"10.1107/S1600577524005149","DOIUrl":"10.1107/S1600577524005149","url":null,"abstract":"<p><p>StreamSAXS is a Python-based small- and wide-angle X-ray scattering (SAXS/WAXS) data analysis workflow platform with graphical user interface (GUI). It aims to provide an interactive and user-friendly tool for analysis of both batch data files and real-time data streams. Users can easily create customizable workflows through the GUI to meet their specific needs. One characteristic of StreamSAXS is its plug-in framework, which enables developers to extend the built-in workflow tasks. Another feature is the support for both already acquired and real-time data sources, allowing StreamSAXS to function as an offline analysis platform or be integrated into large-scale acquisition systems for end-to-end data management. This paper presents the core design of StreamSAXS and provides user cases demonstrating its utilization for SAXS/WAXS data analysis in offline and online scenarios.</p>","PeriodicalId":48729,"journal":{"name":"Journal of Synchrotron Radiation","volume":" ","pages":"1249-1256"},"PeriodicalIF":2.5,"publicationDate":"2024-09-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC11371052/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"141617451","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"物理与天体物理","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
{"title":"Spexwavepy: an open-source Python package for X-ray wavefront sensing using speckle-based techniques.","authors":"Lingfei Hu, Hongchang Wang, Kawal Sawhney","doi":"10.1107/S1600577524005861","DOIUrl":"10.1107/S1600577524005861","url":null,"abstract":"<p><p>In situ wavefront sensing plays a critical role in the delivery of high-quality beams for X-ray experiments. X-ray speckle-based techniques stand out among other in situ techniques for their easy experimental setup and various data acquisition modes. Although X-ray speckle-based techniques have been under development for more than a decade, there are still no user-friendly software packages for new researchers to begin with. Here, we present an open-source Python package, spexwavepy, for X-ray wavefront sensing using speckle-based techniques. This Python package covers a variety of X-ray speckle-based techniques, provides plenty of examples with real experimental data and offers detailed online documentation for users. We hope it can help new researchers learn and apply the speckle-based techniques for X-ray wavefront sensing to synchrotron radiation and X-ray free-electron laser beamlines.</p>","PeriodicalId":48729,"journal":{"name":"Journal of Synchrotron Radiation","volume":" ","pages":"1037-1042"},"PeriodicalIF":2.5,"publicationDate":"2024-09-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC11371044/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"141793836","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"物理与天体物理","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
{"title":"Effectiveness of ab initio molecular dynamics in simulating EXAFS spectra from layered systems.","authors":"F d'Acapito, M A Rehman","doi":"10.1107/S1600577524005484","DOIUrl":"10.1107/S1600577524005484","url":null,"abstract":"<p><p>The simulation of EXAFS spectra of thin films via ab initio methods is discussed. The procedure for producing the spectra is presented as well as an application to a two-dimensional material (WSe<sub>2</sub>) where the effectiveness of this method in reproducing the spectrum and the linear dichroic response is shown. A series of further examples in which the method has been employed for the structural determination of materials are given.</p>","PeriodicalId":48729,"journal":{"name":"Journal of Synchrotron Radiation","volume":" ","pages":"1078-1083"},"PeriodicalIF":2.5,"publicationDate":"2024-09-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC11371032/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"141753118","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"物理与天体物理","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Elizaveta Kozyr, Sara Martí-Sánchez, Alina Skorynina, Jordi Arbiol, Carlos Escudero, Lorenzo Mino, Aram Bugaev
{"title":"In situ photodeposition of ultra-small palladium particles on TiO<sub>2</sub>.","authors":"Elizaveta Kozyr, Sara Martí-Sánchez, Alina Skorynina, Jordi Arbiol, Carlos Escudero, Lorenzo Mino, Aram Bugaev","doi":"10.1107/S1600577524004788","DOIUrl":"10.1107/S1600577524004788","url":null,"abstract":"<p><p>In situ and operando investigation of photocatalysts plays a fundamental role in understanding the processes of active phase formation and the mechanisms of catalytic reactions, which is crucial for the rational design of more efficient materials. Using a custom-made operando photocatalytic cell, an in situ procedure to follow the formation steps of Pd/TiO<sub>2</sub> photocatalyst by synchrotron-based X-ray absorption spectroscopy (XAS) is proposed. The procedure resulted in the formation of ∼1 nm Pd particles with a much narrower size distribution and homogeneous spreading over TiO<sub>2</sub> support compared with the samples generated in a conventional batch reactor. The combination of in situ XAS spectroscopy with high-angle annular dark-field scanning transmission electron microscopy demonstrated the formation of single-atom Pd(0) sites on TiO<sub>2</sub> as the initial step of the photodeposition process. Palladium hydride particles were observed for all investigated samples upon exposure to formic acid solutions.</p>","PeriodicalId":48729,"journal":{"name":"Journal of Synchrotron Radiation","volume":" ","pages":"1071-1077"},"PeriodicalIF":2.5,"publicationDate":"2024-09-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC11371036/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"141617450","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"物理与天体物理","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}