Journal of Applied Crystallography最新文献

{"title":"Interface densification in a microphase-separated diblock copolymer resolved by small-angle X-ray scattering.","authors":"Yu-Hsuan Lin, Yu-Chung Chen, Aditya Sahare, Yi-Cheng Lai, Chun-Jen Su, Jing-Cherng Tsai, Katsuhiro Yamamoto, Hsin-Lung Chen","doi":"10.1107/S1600576725002638","DOIUrl":"10.1107/S1600576725002638","url":null,"abstract":"<p><p>In block copolymers exhibiting lower critical ordering transition behavior, the segregation strength increases with temperature due to the significantly different thermal expansivities of the constituent blocks. Using synchrotron small-angle X-ray scattering, we reveal a phenomenon of segmental densification at the microdomain interface in this type of system, where the local electron density in a specific region of the interface surpasses that of the denser domain. As a result, the interfacial electron density profile deviates significantly from the hyperbolic tangent function expected for an incompressible melt. This unique densification effect can be attributed to the negative volume of mixing at the interface between the dissimilar segments and emerges when the electron densities of the constituent blocks are similar.</p>","PeriodicalId":14950,"journal":{"name":"Journal of Applied Crystallography","volume":"58 Pt 3","pages":"869-878"},"PeriodicalIF":6.1,"publicationDate":"2025-05-12","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC12135978/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144234172","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"材料科学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"A simple cryotransfer method for 3D electron diffraction measurements of highly sensitive samples.","authors":"Kshitij Gurung, Erik Uran, Klemen Motaln, Petr Brázda, Kristian Radan, Matic Lozinšek, Lukáš Palatinus","doi":"10.1107/S1600576725002456","DOIUrl":"10.1107/S1600576725002456","url":null,"abstract":"<p><p>The accurate characterization of highly sensitive materials using 3D electron diffraction (3D ED) is often challenged by sample degradation caused by exposure to moisture, air, temperature variations and high vacuum during the transfer and introduction into the transmission electron microscope (TEM). A cryogenic sample-transfer protocol is presented here, designed to enable the safe and effective transfer of reactive samples into the TEM, ensuring an inert and moisture-free environment throughout the process. The protocol was validated by redetermining the crystal structures of the moisture-sensitive, strongly oxidizing and highly reactive compounds XeF₂, XeF₄ and XeF₂·XeF₄ cocrystal. Crystal structures of all three compounds were successfully solved <i>ab initio</i> and dynamically refined, yielding results that showed good agreement with the previously reported X-ray and neutron diffraction structures. This approach holds significant promise for advancing the study of other reactive and moisture-sensitive samples, enabling precise structural characterization in cases where traditional TEM sample preparation is unsuitable.</p>","PeriodicalId":14950,"journal":{"name":"Journal of Applied Crystallography","volume":"58 Pt 3","pages":"1079-1084"},"PeriodicalIF":6.1,"publicationDate":"2025-05-02","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC12135996/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144234164","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"材料科学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Individual dislocation identification in dark-field X-ray microscopy.","authors":"Sina Borgi, Grethe Winther, Henning Friis Poulsen","doi":"10.1107/S1600576725002614","DOIUrl":"10.1107/S1600576725002614","url":null,"abstract":"<p><p>Dark-field X-ray microscopy (DFXM) has recently been introduced for 3D mapping of dislocations and their strain fields in bulk samples and with high angular resolution (10^-4°). In this work, we investigate the minimum information needed to identify the type of an isolated dislocation, parameterized by its Burgers vector, line direction and slip plane. Forward projections of DFXM weak-beam images are generated for a face-centred cubic symmetry using geometrical optics simulations with realistic noise levels. Cross correlating one DFXM image with similar images representing all possible combinations of dislocation types, we find that the cross-correlation values for all non-identical images are below 0.7, clearly demonstrating the feasibility of this method of identification. Experimental DFXM images of isolated dislocations are compared with forward-modelled ones. Complete identification is demonstrated, with the exception of the sign of the Burgers vector. The performance improvement obtained by acquiring data from a 3D volume is explored. This work verifies the use of geometrical optics to simulate DFXM weak-beam images and supports the interfacing of DFXM data with discrete dislocation dynamics simulations.</p>","PeriodicalId":14950,"journal":{"name":"Journal of Applied Crystallography","volume":"58 Pt 3","pages":"813-821"},"PeriodicalIF":6.1,"publicationDate":"2025-05-02","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC12135992/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144234171","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"材料科学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Optimal weights and priors in simultaneous fitting of multiple small-angle scattering datasets.","authors":"Andreas Haahr Larsen","doi":"10.1107/S1600576725002390","DOIUrl":"10.1107/S1600576725002390","url":null,"abstract":"<p><p>Small-angle X-ray and neutron scattering (SAXS and SANS) are powerful techniques in materials science and soft matter. This study addressed how multiple SAXS or SANS datasets are best weighted when performing simultaneous fitting. Three weighting schemes were tested: (1) equal weighting of all datapoints, (2) equal weighting of each dataset through normalization with the number of datapoints and (3) weighting proportional to the information content. The weighting schemes were assessed by model refinement against synthetic data under numerous conditions. The first weighting scheme led to the most accurate parameter estimation, especially when one dataset substantially outnumbered the other(s). Furthermore, it was demonstrated that inclusion of Gaussian priors significantly improves the accuracy of the refined parameters, as compared with common practice, where each parameter is constrained uniformly within an allowed interval.</p>","PeriodicalId":14950,"journal":{"name":"Journal of Applied Crystallography","volume":"58 Pt 3","pages":"934-947"},"PeriodicalIF":6.1,"publicationDate":"2025-05-02","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC12135988/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144234177","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"材料科学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"A SAXS/WAXD beamline with laboratory SAXS apparatus at NanoTerasu.","authors":"H Meguro, M Nishibori, H Yamane, Y Kotani, Y Watanabe, K Kamitani, T Nakamura, K Matsumura, M Takata, Y Takasaki, N Yagi","doi":"10.1107/S1600576725002547","DOIUrl":"10.1107/S1600576725002547","url":null,"abstract":"<p><p>NanoTerasu is a new 3 GeV synchrotron radiation facility in Sendai, Japan, which began user operation in April 2024. A station for small-angle X-ray scattering (SAXS) and wide-angle X-ray diffraction (WAXD) has been built at the wiggler beamline BL08W. The station was built in a branch for which an X-ray beam is provided by Bragg reflection from two Si crystals. The X-ray energy is 8.0 or 13.1 keV using either an Si(111) or an Si(220) crystal, respectively. The beam is focused with an Ru-coated bent cylindrical mirror. In the SAXS station, an Anton Paar SAXSpoint 5.0 laboratory X-ray apparatus has been installed. The original X-ray generator and focusing mirror in the laboratory equipment were removed and four-quadrant slits and an ion chamber have been installed. Low-scatter slits in SAXSpoint 5.0 are used as guard slits in front of the sample. The X-ray detector is a DECTRIS Eiger2 1M. The slits, sample and detector are enclosed in a vacuum chamber to reduce scattering from the air. The detector can be moved along the X-ray axis under vacuum to change the sample-to-detector distance between 53 and 1610 mm. The X-ray flux at 8.0 keV is 1.0 × 10¹¹ cps with a ring current of 200 mA, shortening the exposure time by nearly 1000 times compared with the original laboratory X-ray source. The purpose of employing SAXSpoint 5.0 is to provide a user-friendly SAXS/WAXD system. Anton Paar's measurement control system is employed in user operations. Many users utilize a multi-sample holder onto which 20 samples are fixed and measured in turn as programmed. The data analysis software is also provided by Anton Paar, but data can optionally be stored in TIFF format to be processed by any software that users are familiar with. Among the various sample attachments available from Anton Paar, a goniometer stage for grazing-incidence SAXS/WAXD is employed by many users.</p>","PeriodicalId":14950,"journal":{"name":"Journal of Applied Crystallography","volume":"58 Pt 3","pages":"927-933"},"PeriodicalIF":6.1,"publicationDate":"2025-04-25","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC12135981/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144234163","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"材料科学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Differences in hierarchical structural changes between unoriented P(3HB) and P(3HB-<i>co</i>-3HH) under stretching.","authors":"Masato Arakawa, Taizo Kabe, Tadahisa Iwata, Mikihito Takenaka","doi":"10.1107/S1600576725002365","DOIUrl":"10.1107/S1600576725002365","url":null,"abstract":"<p><p>Poly[(<i>R</i>)-3-hy-droxy-butyrate] [P(3HB)] is a promising environmentally friendly polymer. However, P(3HB) exhibits brittle fracture, and the brittleness makes P(3HB) unsuitable for practical application. To improve the brittleness, 3-hy-droxy-hexano-ate (3HH) is introduced as a second monomer into P(3HB). The random copolymer P(3HB-<i>co</i>-3HH) shows a reduction in brittleness. In this paper, we investigate the changes in the hierarchical structures in unoriented P(3HB) and P(3HB-<i>co</i>-11mol%-3HH) during uniaxial stretching using <i>in situ</i> ultra-small-angle, small-angle and wide-angle X-ray scattering to clarify the effects of the introduction of 3HH. We reveal that the introduction of amorphous component units to P(3HB) not only suppresses crystallization and reduces crystal thickness on the nanometre scale but also destabilizes the crystal structure. We observed stretch-induced density fluctuations near the yield point by <i>in situ</i>X-ray scattering, showing heterogeneous deformation on scales from slightly larger than the lamellae to submicrometres in P(3HB) and on the submicrometre scale in its copolymer under uniaxial stretching. The enhancement of density fluctuations in the copolymer was smaller than that in P(3HB) because stress dispersion was caused by the hierarchical structure formed with the suppression of crystallization.</p>","PeriodicalId":14950,"journal":{"name":"Journal of Applied Crystallography","volume":"58 Pt 3","pages":"886-896"},"PeriodicalIF":6.1,"publicationDate":"2025-04-25","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC12135995/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144234168","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"材料科学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Prediction of the space group and cell volume by training a convolutional neural network with primitive 'ideal' diffraction profiles and its application to 'real' experimental data.","authors":"Hiroyuki Ozaki, Naoya Ishida, Tetsu Kiyobayashi","doi":"10.1107/S1600576725002419","DOIUrl":"10.1107/S1600576725002419","url":null,"abstract":"<p><p>This study describes a deep learning approach to predict the space group and unit-cell volume of inorganic crystals from their powder X-ray diffraction profiles. Using an inorganic crystallographic database, convolutional neural network (CNN) models were successfully constructed with the δ-function-like 'ideal' X-ray diffraction profiles derived solely from the intrinsic properties of the crystal structure, which are dependent on neither the incident X-ray wavelength nor the line shape of the profiles. We examined how the statistical metrics (<i>e.g.</i> the prediction accuracy, precision and recall) are influenced by the ensemble averaging technique and the multi-task learning approach; six CNN models were created from an identical data set for the former, and the space group classification was coupled with the unit-cell volume prediction in a CNN architecture for the latter. The CNN models trained in the 'ideal' world were tested with 'real' X-ray profiles for eleven materials such as TiO₂, LiNiO₂ and LiMnO₂. While the models mostly fared well in the 'real' world, the cases at odds were scrutinized to elucidate the causes of the mismatch. Specifically for Li₂MnO₃, detailed crystallographic considerations revealed that the mismatch can stem from the state of the specific material and/or from the quality of the experimental data, and not from the CNN models. The present study demonstrates that we can obviate the need for emulating experimental diffraction profiles in training CNN models to elicit structural information, thereby focusing efforts on further improvements.</p>","PeriodicalId":14950,"journal":{"name":"Journal of Applied Crystallography","volume":"58 Pt 3","pages":"718-730"},"PeriodicalIF":6.1,"publicationDate":"2025-04-25","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC12135985/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144234179","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"材料科学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Analyzer-based X-ray phase contrast imaging using the forward-diffracted o-beam in a few-millimetre-thick Bragg-case asymmetrically cut crystal.","authors":"Marcelo Goncalves Honnicke, Juliana Manica, XianRong Huang","doi":"10.1107/S1600576725002985","DOIUrl":"10.1107/S1600576725002985","url":null,"abstract":"<p><p>An analyzer-based X-ray phase contrast imaging experiment employing the forward-diffracted o-beam in a few-millimetre-thick Bragg-case asymmetrically cut analyzer crystal has been implemented and tested in a geometry similar to that used in conventional radiography. The high angular stability requirements were overcome using specially designed crystals and a closed-loop feedback intensity system, monitoring the intensity of the diffracted h-beam. Analyzer-based images (ABis) taken at different angular positions on the forward-diffracted o-beam rocking curve show different contrasts, as expected. However, the ABis did not show sharp borders. This was closely investigated by X-ray topography and Δ<i>d</i>/<i>d</i> mapping and was attributed to the stresses caused by the analyzer crystal's own weight in the bulk. Further investigation of the crystal design using finite element analysis coupled with dynamical theory of X-ray diffraction is envisaged.</p>","PeriodicalId":14950,"journal":{"name":"Journal of Applied Crystallography","volume":"58 Pt 3","pages":"789-795"},"PeriodicalIF":6.1,"publicationDate":"2025-04-25","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC12135994/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144234165","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"材料科学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Rheo-SAXS study on electrically responsive hydro-gels with shear-induced conductive micellar networks for on-demand drug release.","authors":"Thuy Thien Ngan Vo, Yi-Wei Chang, Chun-Jen Su, U-Ser Jeng, Chih-Chia Cheng, Ya-Sen Sun, Wei-Tsung Chuang","doi":"10.1107/S1600576725002808","DOIUrl":"10.1107/S1600576725002808","url":null,"abstract":"<p><p>This study presents a novel approach to creating electrically responsive hydro-gels utilizing a poly(ethyl-ene oxide)-poly(propyl-ene oxide)-poly(ethyl-ene oxide) (PEO₁₀₀-PPO₆₅-PEO₁₀₀) triblock copolymer, functionalized with benzene-sulfonate end groups to form sF127. This functionalization allows the incorporation of sF127 into F127 micelles, resulting in tailored micelles designated as F₁₈S₂P when combined with poly(3,4-ethyl-ene-dioxy-thio-phene):poly(benzene-sulfonate) (PEDOT:PSS). For comparison, a control system using non-functionalized PEDOT:PSS/F127 micelles, designated F₂₀S₀P, was also developed. Using piroxicam as a model hydro-phobic drug, we evaluated the hydro-gel's drug encapsulation efficiency and electrical responsiveness. The functionalized F₁₈S₂P hydro-gel demonstrated superior performance of electrically stimulated drug release, especially when prepared with a blade-coating process. <i>In situ</i> rheological small-angle X-ray scattering (rheo-SAXS) measurements under large amplitude oscillatory shear revealed that function-alization facilitates crystal plane sliding, leading to the formation of a randomly hexagonal close-packed (rHCP) sliding layer structure. This behavior contrasts with the face-centered cubic to rHCP phase transition observed in the unfunctionalized hydro-gel. <i>In situ</i> SAXS analysis under applied electric fields (E-SAXS) further confirmed the electroresponsive micellar deformation. By integrating the rheo-SAXS and E-SAXS findings with blade-coating processing insights, we identify a clear structure-function relationship that governs the performance of these hydro-gels. The enhanced drug delivery of the function-al-ized F₁₈S₂P hydro-gel is attributed to the electrostatic attraction between the positively charged PEDOT and the negatively charged benzene-sulfonate-functionalized micelles. This interaction creates conductive nanonetworks within the hydro-gel, significantly improving its ability to release drugs in response to electrical stimulation. This work highlights the potential of electrically responsive hydro-gels for precise, localized drug delivery applications.</p>","PeriodicalId":14950,"journal":{"name":"Journal of Applied Crystallography","volume":"58 Pt 3","pages":"909-918"},"PeriodicalIF":6.1,"publicationDate":"2025-04-25","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC12135972/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144234180","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"材料科学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"New features in <i>ATSAS-4</i>, a program suite for small-angle scattering data analysis.","authors":"D Franke, T Gräwert, D I Svergun","doi":"10.1107/S1600576725002481","DOIUrl":"10.1107/S1600576725002481","url":null,"abstract":"<p><p>The <i>ATSAS</i> release 4 series introduces substantial architectural updates and enhanced user-friendly tools for analyzing biological macromolecules and nanostructured objects. In particular, highly requested project support for graphical user interfaces (GUIs) has been implemented. Here the state of the main window of each GUI application can be saved as a project and then restored to continue or extend analyses. All GUI applications now share a common framework, enabling various plot annotations and export as figures or text for easy data exchange with other plotting applications. The main interactive data processing and interpretation program, <i>PRIMUS</i>, has been significantly expanded with new features and integrated analysis modules. A new GUI for the program <i>PEAK</i> allows for multiple fitting functions, including Gaussian, Lorentzian and pseudo-Voigt. The online chromatography analysis program <i>CHROMIXS</i> supports multiple frame selections and subtractions, along with a newly included <i>EFAMIX</i> module for resolving partially overlapping components. The new <i>ATSAS</i> application <i>LAUNCHER</i> provides user-friendly wizards to configure and run command-line applications. Wherever feasible, operations like file reading and calculations have been parallelized to take advantage of available local compute resources. Command-line interfaces of many applications have been updated, <i>e.g.</i> with renaming and unification of common options. Improved readers/writers are implemented for Protein Data Bank and macromolecular CIF (mmCIF) file handling. The program <i>MIXTURES</i> now combines the functionalities of <i>BILMIX</i>, <i>LIPMIX</i> and <i>MIXTURE</i>, offering simplified and more versatile analyses for polydisperse systems of different shapes, also with single- or multi-layered organization. Installer packages of <i>ATSAS</i> are available for the latest versions of Windows, frequently used Linux distributions and recent macOS releases, both for Intel and ARM architectures, and are free for academic use.</p>","PeriodicalId":14950,"journal":{"name":"Journal of Applied Crystallography","volume":"58 Pt 3","pages":"1027-1033"},"PeriodicalIF":6.1,"publicationDate":"2025-04-15","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC12135997/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144234176","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"材料科学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}