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Keywords = anomalous small-angle X-ray scattering

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21 pages, 3737 KiB  
Article
Structural Analysis of Erbium-Doped Silica-Based Glass-Ceramics Using Anomalous and Small-Angle X-Ray Scattering
by Helena Cristina Vasconcelos, Maria Meirelles, Reşit Özmenteş and Luís Santos
Foundations 2025, 5(1), 5; https://doi.org/10.3390/foundations5010005 - 12 Feb 2025
Cited by 1 | Viewed by 1393
Abstract
This study employs advanced structural characterization techniques, including anomalous small-angle X-ray scattering (ASAXS), small-angle X-ray scattering (SAXS), and X-ray photoelectron spectroscopy (XPS), to investigate erbium (Er3+)-doped silica-based glass-ceramic thin films synthesized via the sol–gel method. This research examines the SiO2 [...] Read more.
This study employs advanced structural characterization techniques, including anomalous small-angle X-ray scattering (ASAXS), small-angle X-ray scattering (SAXS), and X-ray photoelectron spectroscopy (XPS), to investigate erbium (Er3+)-doped silica-based glass-ceramic thin films synthesized via the sol–gel method. This research examines the SiO2-TiO2 and SiO2-TiO2-PO2.5 systems, focusing on the formation, dispersion, and structural integration of Er3+-containing nanocrystals within the amorphous matrix under different thermal treatments. Synchrotron radiation tuned to the LIII absorption edge of erbium enabled ASAXS measurements, providing element-specific details about the localization of Er3+ ions. The findings confirm their migration into crystalline phases, such as erbium phosphate (EPO) and erbium titanate (ETO). SAXS and Guinier analysis quantified nanocrystal sizes, revealing trends influenced by their composition and heat treatment. Complementary XPS analysis of the Er 5p core-level states provided detailed information on the chemical and electronic environment of the Er3+ ions, confirming their stabilization within the crystalline structure. Transmission electron microscopy (TEM) highlighted the nanoscale morphology, verifying the aggregation of Er3+ ions into well-defined nanocrystals. The results offer a deeper understanding of their size, distribution, and interaction with the surrounding matrix. Full article
(This article belongs to the Section Physical Sciences)
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21 pages, 2646 KiB  
Review
Anomalous Small-Angle X-ray Scattering and Its Application in the Dynamic Reconstruction of Electrochemical CO2 Reduction Catalysts
by Weidong Cheng, Zhongjun Chen, Xuehui Wu, Zhaojun Wu, Xin Wang, Mengyuan Zhao, Huanyan Liu, Hongge Jia, Chaohui Wang, Xuefeng Wang, Zhonghua Wu and Xueqing Xing
Symmetry 2023, 15(5), 1034; https://doi.org/10.3390/sym15051034 - 7 May 2023
Cited by 2 | Viewed by 3100
Abstract
The electrochemical CO2 reduction reaction (CO2RR) is a promising approach for mitigating the greenhouse effect arising from anthropogenic CO2 emission. Nonetheless, poor product selectivity associated with electrochemical catalysts is the main technical problem for the application of CO2 [...] Read more.
The electrochemical CO2 reduction reaction (CO2RR) is a promising approach for mitigating the greenhouse effect arising from anthropogenic CO2 emission. Nonetheless, poor product selectivity associated with electrochemical catalysts is the main technical problem for the application of CO2RR technology. The catalytic performance of nano-catalysts is strongly dependent on their microstructural features. Anomalous small-angle X-ray scattering (ASAXS) is one of the most effective techniques for studying nanostructural change in an operando way, especially for complex systems and mixed-element catalyst situations. Furthermore, based on the research results of ASAXS, appropriate catalyst components and nanostructures can be designed to achieve stable catalytic performance of the catalyst, promote catalytic reaction rate, or improve catalytic reaction selectivity. In this paper, the basic concept, principle, and applications in different systems of ASAXS are reviewed thoroughly. Finally, the development prospect of ASAXS in the field of electrocatalysis is prospected. It is hoped that this review will further promote ASAXS technology to play a more far-reaching impact in the field of electrocatalytic CO2RR. Full article
(This article belongs to the Special Issue Advances in the Capture and Transformation of Carbon Dioxide)
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8 pages, 11256 KiB  
Communication
Microstructure Investigation of Polymer Electrolyte Fuel Cell Catalyst Layers Containing Perfluorosulfonated Ionomer
by Maito Koga, Hidetoshi Matsumoto, Mitsunori Kunishima, Masatoshi Tokita, Hiroyasu Masunaga, Noboru Ohta, Akihisa Takeuchi, Junji Mizukado, Hidekazu Sugimori, Kazuhiko Shinohara, Suguru Uemura, Toshihiko Yoshida and Shuichiro Hirai
Membranes 2021, 11(7), 466; https://doi.org/10.3390/membranes11070466 - 24 Jun 2021
Cited by 3 | Viewed by 3911
Abstract
Perfluorosulfonated ionomers are the most successful ion-exchange membranes at an industrial scale. One recent, cutting-edge application of perfluorosulfonated ionomers is in polymer electrolyte fuel cells (PEFCs). In PEFCs, the ionomers are used as a component of the catalyst layer (CL) in addition to [...] Read more.
Perfluorosulfonated ionomers are the most successful ion-exchange membranes at an industrial scale. One recent, cutting-edge application of perfluorosulfonated ionomers is in polymer electrolyte fuel cells (PEFCs). In PEFCs, the ionomers are used as a component of the catalyst layer (CL) in addition to functioning as a proton-exchange membrane. In this study, the microstructures in the CLs of PEFCs were characterized by combined synchrotron X-ray scattering and transmission electron microscopy (TEM) analyses. The CL comprised a catalyst, a support, and an ionomer. Fractal dimensional analysis of the combined ultrasmall- and small-angle X-ray scattering profiles indicated that the carbon-black-supported Pt catalyst (Pt/CB) surface was covered with the ionomer in the CL. Anomalous X-ray scattering revealed that the Pt catalyst nanoparticles on the carbon surfaces were aggregated in the CLs. These findings are consistent with the ionomer/catalyst microstructures and ionomer coverage on the Pt/CB surface obtained from TEM observations. Full article
(This article belongs to the Special Issue Novel Ion-Exchange Membranes)
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3 pages, 176 KiB  
Editorial
Investigation of Nanostructures with X-ray Scattering Techniques
by Dominik Kriegner and Milan Dopita
Crystals 2019, 9(10), 500; https://doi.org/10.3390/cryst9100500 - 26 Sep 2019
Viewed by 2103
Abstract
n/a Full article
(This article belongs to the Special Issue Investigation of Nanostructures with X-ray Scattering Techniques)
9 pages, 1793 KiB  
Article
Elucidation of Spatial Distribution of Hydrophobic Aromatic Compounds Encapsulated in Polymer Micelles by Anomalous Small-Angle X-ray Scattering
by Shota Sasaki, Ginpei Machida, Ryosuke Nakanishi, Masaki Kinoshita and Isamu Akiba
Polymers 2018, 10(2), 180; https://doi.org/10.3390/polym10020180 - 12 Feb 2018
Cited by 7 | Viewed by 4584
Abstract
Spatial distribution of bromobenzene (BrBz) and 4-bromophenol (BrPh) as hydrophobic aromatic compounds incorporated in polymer micelles with vesicular structure consisting of poly(ethylene glycol)-b-poly(tert-butyl methacrylate) (PEG-b-PtBMA) in aqueous solution is investigated by anomalous small-angle X-ray scattering (ASAXS) analyses [...] Read more.
Spatial distribution of bromobenzene (BrBz) and 4-bromophenol (BrPh) as hydrophobic aromatic compounds incorporated in polymer micelles with vesicular structure consisting of poly(ethylene glycol)-b-poly(tert-butyl methacrylate) (PEG-b-PtBMA) in aqueous solution is investigated by anomalous small-angle X-ray scattering (ASAXS) analyses near Br K edge. Small-angle X-ray scattering (SAXS) intensities from PEG-b-PtBMA micelles containing BrBz and BrPh were decreased as the energy of incident X-ray approached to Br K edge corresponding to the energy dependence of anomalous scattering factor of Br. The analysis for the energy dependence of SAXS profiles from the PEG-b-PtBMA micelles containing BrBz revealed that BrBz molecules were located in hydrophobic layer of PEG-b-PtBMA micelles. On the contrary, it was found by ASAXS that BrPh existed not only in the hydrophobic layer but also in the shell layer. Since ASAXS analysis successfully accomplished to visualize the spatial distribution of hydrophobic molecules in polymer micelles, it should be expected to be a powerful tool for characterization of drug delivery vehicles. Full article
(This article belongs to the Special Issue Polymer Micelles)
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15 pages, 2764 KiB  
Article
Systematic Limitations in Concentration Analysis via Anomalous Small-Angle X-ray Scattering in the Small Structure Limit
by Guenter Goerigk, Sebastian Lages and Klaus Huber
Polymers 2016, 8(3), 85; https://doi.org/10.3390/polym8030085 - 16 Mar 2016
Cited by 2 | Viewed by 11278
Abstract
Anomalous small angle scattering measurements have been applied to diluted solutions of anionic polyacrylates decorated by specifically-interacting Pb2+ cations, revealing partial collapse of the polyacrylate into pearl-like subdomains with a size on the order of a few nanometers. From the pure-resonant scattering [...] Read more.
Anomalous small angle scattering measurements have been applied to diluted solutions of anionic polyacrylates decorated by specifically-interacting Pb2+ cations, revealing partial collapse of the polyacrylate into pearl-like subdomains with a size on the order of a few nanometers. From the pure-resonant scattering contribution of the Pb2+ cations, and from subsequent analysis of the resonant-invariant, the amount of Pb2+ cations condensed onto the polyanions with respect to the total amount of Pb2+ cations in the solvent was estimated. In order to scrutinize systematic limitations in the determination of the chemical concentrations of resonant scattering counterions in the collapsed phase, Monte Carlo simulations have been performed. The simulations are based on structural confinements at variable size in the range of few nanometers, which represent the collapsed subdomains in the polyanions. These confinements were gradually filled to a high degree of the volume fraction with resonant scattering counterions giving access to a resonant-invariant at a variable degree of filling. The simulations revealed in the limit of small structures a significant underestimation of the true degree of filling of the collapsed subdomains when determining chemical concentrations of Pb2+ cations from the resonant invariant. Full article
(This article belongs to the Collection Polyelectrolytes)
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