Journal of Synchrotron Radiation最新文献

{"title":"In situ beam reduction of Pu(IV) and Bk(IV) as a route to trivalent transuranic coordination complexes with hydroxypyridinone chelators.","authors":"Korey P Carter, Jennifer N Wacker, Kurt F Smith, Gauthier J P Deblonde, Liane M Moreau, Julian A Rees, Corwin H Booth, Rebecca J Abergel","doi":"10.1107/S1600577522000200","DOIUrl":"10.1107/S1600577522000200","url":null,"abstract":"<p><p>The solution-state interactions of plutonium and berkelium with the octadentate chelator 3,4,3-LI(1,2-HOPO) (343-HOPO) were investigated and characterized by X-ray absorption spectroscopy, which revealed in situ reductive decomposition of the tetravalent species of both actinide metals to yield Pu(III) and Bk(III) coordination complexes. X-ray absorption near-edge structure (XANES) measurements were the first indication of in situ synchrotron redox chemistry as the Pu threshold and white-line position energies for Pu-343-HOPO were in good agreement with known diagnostic Pu(III) species, whereas Bk-343-HOPO results were found to mirror the XANES behavior of Bk(III)-DTPA. Extended X-ray absorption fine structure results revealed An-O_HOPO bond distances of 2.498 (5) and 2.415 (2) Å for Pu and Bk, respectively, which match well with bond distances obtained for trivalent actinides and 343-HOPO via density functional theory calculations. Pu(III)- and Bk(III)-343-HOPO data also provide initial insight into actinide periodicity as they can be compared with previous results with Am(III)-, Cm(III)-, Cf(III)-, and Es(III)-343-HOPO, which indicate there is likely an increase in 5f covalency and heterogeneity across the actinide series.</p>","PeriodicalId":17114,"journal":{"name":"Journal of Synchrotron Radiation","volume":null,"pages":null},"PeriodicalIF":2.4,"publicationDate":"2022-03-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC8900832/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"44737816","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":"Synchrotron radiation transmission by two coupled flat microchannel plates: new opportunities to control the focal spot characteristics.","authors":"M I Mazuritskiy, A M Lerer, A Marcelli, S B Dabagov","doi":"10.1107/S1600577521012893","DOIUrl":"10.1107/S1600577521012893","url":null,"abstract":"<p><p>An improved theoretical model to calculate the focal spot properties of coherent synchrotron radiation (SR) soft X-ray beams by combining and aligning two microchannel plates (MCPs) is presented. The diffraction patterns of the radiation behind the MCP system are simulated in the framework of the electrodynamical model of the radiation emission from two-dimensional finite antenna arrays. Simulations show that this particular optical device focuses the soft X-ray radiation in a circular central spot with a radius of ∼4 µm. The study points out that such MCP-based devices may achieve micrometre and sub-micrometre spot sizes as required by many applications in the soft X-ray range. Finally, based on experimental and theoretical results of the radiation transmission by this MCP-based device, a new method to characterize the spatial properties of brilliant SR sources is discussed.</p>","PeriodicalId":17114,"journal":{"name":"Journal of Synchrotron Radiation","volume":null,"pages":null},"PeriodicalIF":2.4,"publicationDate":"2022-03-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC8900856/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"45831181","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":"Generating coherent and ultrashort X-ray pulses via HHG-seeding in storage rings.","authors":"Yujie Lu, Chao Feng, Lingjun Tu, Changliang Li, Bocheng Jiang, Dong Wang","doi":"10.1107/S1600577521013382","DOIUrl":"10.1107/S1600577521013382","url":null,"abstract":"<p><p>The generation of fully coherent and femtosecond time-scale radiation pulses in the X-ray regime is one of the most common demands of ring-based synchrotron light source users. In this paper, a method that utilizes the recent proposed angular dispersion induced microbunching technique to convert external light from high-harmonic generation (HHG) to coherent light at shorter wavelength is proposed. Numerical simulations using the practical parameters of a diffraction-limited storage ring demonstrate the generation of coherent pulse trains with photon energy as high as 2 keV, pulse duration as short as ∼10 fs and high peak brightness directly from an HHG source at 13 nm.</p>","PeriodicalId":17114,"journal":{"name":"Journal of Synchrotron Radiation","volume":null,"pages":null},"PeriodicalIF":2.4,"publicationDate":"2022-03-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC8900847/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"48183846","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":"ID23-2: an automated and high-performance microfocus beamline for macromolecular crystallography at the ESRF.","authors":"Max Nanao, Shibom Basu, Ulrich Zander, Thierry Giraud, John Surr, Matias Guijarro, Mario Lentini, Franck Felisaz, Jeremy Sinoir, Christian Morawe, Amparo Vivo, Antonia Beteva, Marcus Oscarsson, Hugo Caserotto, Fabien Dobias, David Flot, Didier Nurizzo, Jonathan Gigmes, Nicolas Foos, Ralf Siebrecht, Thomas Roth, Pascal Theveneau, Olof Svensson, Gergely Papp, Bernard Lavault, Florent Cipriani, Ray Barrett, Carole Clavel, Gordon Leonard","doi":"10.1107/S1600577522000984","DOIUrl":"10.1107/S1600577522000984","url":null,"abstract":"<p><p>ID23-2 is a fixed-energy (14.2 keV) microfocus beamline at the European Synchrotron Radiation Facility (ESRF) dedicated to macromolecular crystallography. The optics and sample environment have recently been redesigned and rebuilt to take full advantage of the upgrade of the ESRF to the fourth generation Extremely Brilliant Source (ESRF-EBS). The upgraded beamline now makes use of two sets of compound refractive lenses and multilayer mirrors to obtain a highly intense (>10¹³ photons s^-1) focused microbeam (minimum size 1.5 µm × 3 µm full width at half-maximum). The sample environment now includes a FLEX-HCD sample changer/storage system, as well as a state-of-the-art MD3Up high-precision multi-axis diffractometer. Automatic data reduction and analysis are also provided for more advanced protocols such as synchrotron serial crystallographic experiments.</p>","PeriodicalId":17114,"journal":{"name":"Journal of Synchrotron Radiation","volume":null,"pages":null},"PeriodicalIF":2.4,"publicationDate":"2022-03-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC8900849/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"62055930","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":"Synchrotron radiation analysis of root dentin: the roles of fluoride and calcium ions in hydroxyapatite remineralization.","authors":"Nutthapong Kantrong, Krassawan Khongkhaphet, Nutnicha Sitornsud, Pakaporn Lo-Apirukkul, Waraporn Phanprom, Catleya Rojviriya, Penphitcha Amonpattaratkit, Watcharaphong Ariyakriangkai","doi":"10.1107/S1600577521013655","DOIUrl":"10.1107/S1600577521013655","url":null,"abstract":"<p><p>Although the use of fluoride for root caries control is reported to be effective, the mechanism of maintaining hydroxyapatite is still unclear. This study elucidates the roles of fluoride in the recrystallization of hydroxyapatite, and the impact of calcium to maintain the abundance of hydroxyapatite on acid-challenged root dentin with a novel approach - using synchrotron radiation. Root dentin samples obtained from 40 extracted human premolars were subjected to pH challenge in combination with fluoride treatment. The effect of fluoride on hydroxyapatite regeneration on the root was investigated by using a range of fluoride concentrations (1000-5000 p.p.m.) and the EDTA-chelation technique in vitro. Synchrotron radiation X-ray micro-computed tomography and X-ray absorption spectroscopy were utilized to characterize the chemical composition of calcium species on the surface of prepared samples. The percentage of hydroxyapatite and the relative abundance of calcium species were subsequently compared between groups. The absence of calcium or fluoride prevented the complete remineralization of hydroxyapatite on the surface of early root caries. Different concentrations of fluoride exposure did not affect the relative abundance of hydroxyapatite. Sufficient potency of 1000 p.p.m. fluoride solution in promoting hydroxyapatite structural recrystallization on the root was demonstrated. Both calcium and fluoride ions are prerequisites in a caries-prone environment. Orchestration of F^- and Ca²⁺ is required for structural homeostasis of root dentin during acid attack. Sustainable levels of F^- and Ca²⁺ might thus be a strict requirement in the saliva of the population prone to root caries. Fluoride and calcium contribute to structural homeostasis of tooth root, highlighting that routine fluoride use in combination with calcium replenishment is recommended for maintaining dental health. This study also demonstrates that utilization of synchrotron radiation could provide a promising experimental platform for laboratory investigation especially in the dental material research field.</p>","PeriodicalId":17114,"journal":{"name":"Journal of Synchrotron Radiation","volume":null,"pages":null},"PeriodicalIF":2.4,"publicationDate":"2022-03-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC8900867/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"47736047","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":"3D printed devices and infrastructure for liquid sample delivery at the European XFEL.","authors":"Mohammad Vakili, Johan Bielecki, Juraj Knoška, Florian Otte, Huijong Han, Marco Kloos, Robin Schubert, Elisa Delmas, Grant Mills, Raphael de Wijn, Romain Letrun, Simon Dold, Richard Bean, Adam Round, Yoonhee Kim, Frederico A Lima, Katerina Dörner, Joana Valerio, Michael Heymann, Adrian P Mancuso, Joachim Schulz","doi":"10.1107/S1600577521013370","DOIUrl":"10.1107/S1600577521013370","url":null,"abstract":"<p><p>The Sample Environment and Characterization (SEC) group of the European X-ray Free-Electron Laser (EuXFEL) develops sample delivery systems for the various scientific instruments, including systems for the injection of liquid samples that enable serial femtosecond X-ray crystallography (SFX) and single-particle imaging (SPI) experiments, among others. For rapid prototyping of various device types and materials, sub-micrometre precision 3D printers are used to address the specific experimental conditions of SFX and SPI by providing a large number of devices with reliable performance. This work presents the current pool of 3D printed liquid sample delivery devices, based on the two-photon polymerization (2PP) technique. These devices encompass gas dynamic virtual nozzles (GDVNs), mixing-GDVNs, high-viscosity extruders (HVEs) and electrospray conical capillary tips (CCTs) with highly reproducible geometric features that are suitable for time-resolved SFX and SPI experiments at XFEL facilities. Liquid sample injection setups and infrastructure on the Single Particles, Clusters, and Biomolecules and Serial Femtosecond Crystallography (SPB/SFX) instrument are described, this being the instrument which is designated for biological structure determination at the EuXFEL.</p>","PeriodicalId":17114,"journal":{"name":"Journal of Synchrotron Radiation","volume":null,"pages":null},"PeriodicalIF":2.4,"publicationDate":"2022-03-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC8900844/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"43674839","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":"Environmental cell for in situ X-ray synchrotron micro-CT imaging with simultaneous acoustic measurements.","authors":"Arkady N Drobchik, Viktor V Nikitin, Mikhail I Fokin, Geser A Dugarov, Pavel D Shevchenko, Alex L Deriy, Andrey Yu Manakov, Konstantin E Kuper, Anton A Duchkov","doi":"10.1107/S1600577521013308","DOIUrl":"10.1107/S1600577521013308","url":null,"abstract":"<p><p>Synchrotron radiation provides the necessary spatial and temporal resolution for non-invasive operando studies of dynamic processes under complex environmental conditions. Here a new environmental cell for simultaneous in situ dynamic X-ray imaging and measuring acoustic properties of geological samples is presented. The primary purpose of this cell is to study gas-hydrate formation in porous geo-materials and its influence on their acoustic properties. The cell is designed for cylindrical samples of 9 mm in diameter, confining and pore pressures up to 12 MPa, and temperatures from -20°C to room temperature. The cell is portable and can be easily assembled and operated at different X-ray sources. This cell enables a wide range of experiments studying physical/chemical processes in the Earth subsurface that change the mechanical properties of rocks (geochemical reactions, phase transitions, etc.).</p>","PeriodicalId":17114,"journal":{"name":"Journal of Synchrotron Radiation","volume":null,"pages":null},"PeriodicalIF":2.4,"publicationDate":"2022-03-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC8900851/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"44294477","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":"Scanning structural mapping at the Life Science X-ray Scattering Beamline.","authors":"Lin Yang, Jiliang Liu, Shirish Chodankar, Stephen Antonelli, Jonathan DiFabio","doi":"10.1107/S1600577521013266","DOIUrl":"10.1107/S1600577521013266","url":null,"abstract":"<p><p>This work describes the instrumentation and software for microbeam scattering and structural mapping at the Life Science X-ray Scattering (LiX) beamline at NSLS-II. Using a two-stage focusing scheme, an adjustable beam size between a few micrometres and a fraction of a millimetre is produced at the sample position. Scattering data at small and wide angles are collected simultaneously on multiple Pilatus detectors. A recent addition of an in-vacuum Pilatus 900k detector, with the detector modules arranged in a C-shaped configuration, has improved the azimuthal angle coverage in the wide-angle data. As an option, fluorescence data can be collected simultaneously. Fly scans have been implemented to minimize the time interval between scattering patterns and to avoid unnecessary radiation damage to the sample. For weakly scattering samples, an in-vacuum sample environment has been developed here to minimize background scattering. Data processing for these measurements is highly sample-specific. To establish a generalized data process workflow, first the data are reduced to reciprocal coordinates at the time of data collection. The users can then quantify features of their choosing from these intermediate data and construct structural maps. As examples, results from in-vacuum mapping of onion epidermal cell walls and 2D tomographic sectioning of an intact poplar stem are presented.</p>","PeriodicalId":17114,"journal":{"name":"Journal of Synchrotron Radiation","volume":null,"pages":null},"PeriodicalIF":2.4,"publicationDate":"2022-03-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC8900859/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"47019826","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":"Effective coordination numbers from EXAFS: general approaches for lanthanide and actinide dioxides.","authors":"Anna Romanchuk, Alexander Trigub, Tatiana Plakhova, Anastasiia Kuzenkova, Roman Svetogorov, Kristina Kvashnina, Stepan Kalmykov","doi":"10.1107/S160057752101300X","DOIUrl":"10.1107/S160057752101300X","url":null,"abstract":"<p><p>Extended X-ray absorption fine structure (EXAFS) is a comprehensive and usable method for characterizing the structures of various materials, including radioactive and nuclear materials. Unceasing discussions about the interpretation of EXAFS results for actinide nanoparticles (NPs) or colloids were still present during the last decade. In this study, new experimental data for PuO₂ and CeO₂ NPs with different average sizes were compared with published data on AnO₂ NPs that highlight the best fit and interpretation of the structural data. In terms of the structure, PuO₂, CeO₂, ThO₂, and UO₂ NPs exhibit similar behaviors. Only ThO₂ NPs have a more disordered and even partly amorphous structure, which results in EXAFS characteristics. The proposed new core-shell model for NPs with calculated effective coordination number perfectly fits the results of the variations in a metal-metal shell with a decrease in NP size.</p>","PeriodicalId":17114,"journal":{"name":"Journal of Synchrotron Radiation","volume":null,"pages":null},"PeriodicalIF":2.4,"publicationDate":"2022-03-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC8900841/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"47594666","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":"Fully automated measurement system for temperature-dependent X-ray total scattering at beamline BL04B2 at SPring-8.","authors":"Hiroki Yamada, Kengo Nakada, Michitaka Takemoto, Koji Ohara","doi":"10.1107/S1600577521013527","DOIUrl":"10.1107/S1600577521013527","url":null,"abstract":"<p><p>Data-driven approaches in materials science demand the collection of large amounts of data on the target materials at synchrotron beamlines. To accurately gather suitable experimental data, it is essential to establish fully automated measurement systems to reduce the workload of the beamline staff. Moreover, the recent COVID-19 pandemic has further emphasized the necessity of automated and/or remote measurements at synchrotron beamlines. Here, the installation of a new sample changer combined with a high-temperature furnace and a fully automated alignment system on beamline BL04B2 at SPring-8 is reported. The system allows X-ray total scattering measurements of up to 21 samples at different temperatures (from room temperature to 1200°C) to be conducted without any human assistance.</p>","PeriodicalId":17114,"journal":{"name":"Journal of Synchrotron Radiation","volume":null,"pages":null},"PeriodicalIF":2.4,"publicationDate":"2022-03-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC8900857/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"43125870","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}