Journal of Applied Crystallography最新文献

{"title":"Structure factors of random hard disk packing in 2D by explicit modeling.","authors":"Yoshiharu Nishiyama","doi":"10.1107/S1600576725002407","DOIUrl":"10.1107/S1600576725002407","url":null,"abstract":"<p><p>This paper describes a method that can (1) generate random packing of hard disks in 2D using Monte Carlo simulation, (2) extract the corresponding pair distribution function using normalization by disk line picking probability and (3) convert it to the structure factor. The generated structure factor agrees well with the analytical form based on the Percus-Yevick equation at a low area fraction (that is, within 1% at an area fraction below 0.2 and 2% at an area fraction of 0.3) but differs at a higher area fraction with more pronounced peaks and oscillations. Above an area fraction of 0.69, the hexagonal packing feature appears as sharp peaks at low <i>Q</i>, which are absent in the analytical solution. The structure factors up to an area fraction of 0.65 as a function of <i>QR</i> and the area fraction are stored in table form. The structure factor table can be combined with the cylinder form factors to simulate the X-ray/neutron scattering intensity of wood cell wall scattering.</p>","PeriodicalId":14950,"journal":{"name":"Journal of Applied Crystallography","volume":"58 Pt 3","pages":"1015-1021"},"PeriodicalIF":6.1,"publicationDate":"2025-04-15","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC12135971/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144234184","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":"Local orthorhombic phase in zirconium oxide nanocrystals: insights from X-ray pair distribution function analysis.","authors":"Rohan Pokratath, Kumara Cordero-Edwards, Maryame Bina, Simon J L Billinge, Jonathan De Roo","doi":"10.1107/S1600576725001761","DOIUrl":"10.1107/S1600576725001761","url":null,"abstract":"<p><p>Zirconium dioxide (ZrO₂) and hafnium dioxide (HfO₂) have emerged as promising alternatives to conventional ferroelectric materials. Understanding the crystal phases of these oxides under different conditions is crucial for optimizing their properties. There are several theories for the (anti)ferroelectric properties; however, comprehensive analysis, particularly at the local structure level, is lacking. In this study, we investigate the local structure of ZrO₂ nanocrystals using X-ray pair distribution function (PDF) analysis, revealing an unexpected local orthorhombic distortion irrespective of crystallite size. This finding suggests the potential existence of an intermediate orthorhombic phase during the microscopic switching pathway observed in previous studies. Additionally, we explore the influence of crystallite size and surface effects on the PDF. These results contribute to a deeper understanding of the structural dynamics in ZrO₂ and offer insights for the design of next-generation ferroelectric materials.</p>","PeriodicalId":14950,"journal":{"name":"Journal of Applied Crystallography","volume":"58 Pt 3","pages":"688-695"},"PeriodicalIF":6.1,"publicationDate":"2025-04-04","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC12135986/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144234174","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":"Strain-induced density fluctuations in linear low-density polyethyl-ene.","authors":"Mizuki Kishimoto, Kazuki Mita, Hiroki Ogawa, Kazuki Shibasaki, Masato Arakawa, Mikihito Takenaka","doi":"10.1107/S1600576725002183","DOIUrl":"10.1107/S1600576725002183","url":null,"abstract":"<p><p>In our previous study [Kishimoto <i>et al.</i> (2020). <i>Macromolecules</i>, <b>53</b>, 9097-9107], density fluctuations were induced on the submicrometre scale in polyethyl-ene (PE) during strain and led to the generation of voids. The strength of the induction was found to increase with the amplitude of the spatial inhomogeneity of the stress field. In this work, we investigated how comonomer species and content affect the behaviors of the strain-induced density fluctuations in linear low-density PE. We found that the strength of the induction decreased with an increase in the spatial homogeneity before stretching and the mechanical melting during strain and that the degree of spatial homogeneity and mechanical melting depend on the species and content of the comonomer.</p>","PeriodicalId":14950,"journal":{"name":"Journal of Applied Crystallography","volume":"58 Pt 3","pages":"879-885"},"PeriodicalIF":6.1,"publicationDate":"2025-04-04","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC12135982/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144234183","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":"Synthesis and quantum crystallographic evaluation of WYLID: YLID's red rival.","authors":"Florian Meurer, Maximilian Schimpf, Birgit Hischa, Christoph Hennig, Julia Rehbein, Florian Kleemiss, Michael Bodensteiner","doi":"10.1107/S160057672500175X","DOIUrl":"10.1107/S160057672500175X","url":null,"abstract":"<p><p>The synthesis and characterization of WYLID [2-(di-methyl-λ⁴-sulfane-ylidene)-[1,2'-bi-indenyl-idene]-1',3,3'(2<i>H</i>)-trione], a side product that appears during the synthesis of YLID, is presented in this study. Quantum crystallographic insights into the bonding situation in WYLID are provided on the basis of Hirshfeld atom refinement (HAR), multipolar modelling and X-ray restrained wavefunction fitting. We compare these results with theoretical calculations on a gas-phase optimized density functional theory and a Hartree-Fock calculation based on the geometry obtained by HAR. The S-C bond in WYLID is best described as an ylid-type bond and the SMe₂ fragment does not affect the nearest C-O carbonyl/enolate equilibrium. This work may contribute to an ongoing debate in the quantum crystallography community about the bonding situation in YLID and provides a routine for distinguishing between carbonyls and enolates.</p>","PeriodicalId":14950,"journal":{"name":"Journal of Applied Crystallography","volume":"58 Pt 3","pages":"678-687"},"PeriodicalIF":6.1,"publicationDate":"2025-04-04","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC12135977/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144234185","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":"Reliability of pair distribution function analysis in <i>in situ</i> experiments.","authors":"Rasmus Baden Stubkjær, Magnus Kløve, Andreas Bertelsen, Anders Bæk Borup, Martin Roelsgaard, Bo Brummerstedt Iversen","doi":"10.1107/S1600576725001694","DOIUrl":"10.1107/S1600576725001694","url":null,"abstract":"<p><p><i>In situ</i> and <i>operando</i> pair distribution function (PDF) studies are becoming commonly used to study chemical reactions, nucleation and growth of nanoparticles, or structural changes during the operation of batteries, catalysts, thermoelectric devices <i>etc.</i> However, repeated time-resolved total scattering experiments and subsequent PDF analysis are often not prioritized due to the scarce synchrotron beam time available. This means that the experimental uncertainty and reproducibility of the experimental methods are unknown, and the full potential of <i>in situ</i> PDF experiments may not be exploited. Here, we quantify the experimental uncertainty of the PDF technique in an <i>in situ</i> study of the hydro-thermal synthesis of ZrO₂ nanoparticles. Systematic variation of the parameters used to obtain the PDF shows that the user-defined parameters can potentially affect the chemical conclusions obtained from the time-resolved experiment. We found that comparable results are best obtained using the same input parameters across different experiments. We also compare different PDF algorithms to examine whether the processing algorithm influences the chemical analysis.</p>","PeriodicalId":14950,"journal":{"name":"Journal of Applied Crystallography","volume":"58 Pt 2","pages":"495-503"},"PeriodicalIF":6.1,"publicationDate":"2025-03-19","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC11957418/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143763416","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":"Upgrade of the KWS-2 high-intensity/extended-<i>Q</i>-range SANS diffractometer of JCNS for soft matter and biophysics: <i>in situ</i> SEC, controlled <i>in situ</i> RH/T variation and WANS detection.","authors":"Jia-Jhen Kang, Ralf Biehl, Georg Brandl, Helmut Korb, Kimio Yoshimura, Vladimir Ossovyi, Andreas Nebel, Jacqueline Lippertz, Ralf Engels, Günter Kemmerling, Alexander Zaft, Hiroki Iwase, Hiroshi Arima-Osonoi, Shin-Ichi Takata, Alexander Weber, Simon Staringer, Baohu Wu, Yue Zhao, Stefan Mattauch, Aurel Radulescu","doi":"10.1107/S160057672500158X","DOIUrl":"10.1107/S160057672500158X","url":null,"abstract":"<p><p>The KWS-2 small-angle neutron scattering (SANS) diffractometer operated by Jülich Centre for Neutron Science (JCNS) at Heinz Maier-Leibnitz Zentrum, Garching, Germany, is dedicated to the investigation of mesoscopic multi-scale structures and structural changes due to rapid kinetic processes in soft condensed matter and biophysical systems. Following requests from the user community, it has been repeatedly upgraded with respect to the most important methodological parameters of an instrument of this type, namely the intensity on the sample, the instrumental resolution and the minimum scattering variable <i>Q</i> _min. Here we report on further specific improvements to the sample environment and detection capabilities which have just been completed or are being implemented. Complementary size-exclusion chromatography (SEC) for <i>in situ</i> protein purification was developed and optimized at KWS-2 to provide the instrument with biological samples of controlled quality. The instrument is also currently being equipped with a wide-angle neutron scattering (WANS) detector which will allow it to bridge the atomic and mesoscale, benefiting from the instrument's adjustable resolution down to Δλ/λ = 2%. For controlled relative humidity and temperature (RH/T) on ionic conductive samples for energy applications or biomembranes for biophysical and health applications, a precise dew point generator has recently been characterized and commissioned; this offers great versatility with regard to varying the contrast <i>in situ</i> in the beam on hydrated samples.</p>","PeriodicalId":14950,"journal":{"name":"Journal of Applied Crystallography","volume":"58 Pt 2","pages":"581-594"},"PeriodicalIF":6.1,"publicationDate":"2025-03-19","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC11957400/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143763624","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":"Solvent-annealing-induced microphase separation in polyether polyurethane: a small-angle X-ray scattering study.","authors":"Shanshan Wang, Jiayao Song, Keping Chen, Mark Julian Henderson, Qiang Tian, László Almásy","doi":"10.1107/S1600576725001633","DOIUrl":"10.1107/S1600576725001633","url":null,"abstract":"<p><p>This study investigated the effects of solvent vapor annealing on the microphase separation structure of polyurethane (PU) using small-angle X-ray scattering (SAXS) and complementary techniques. Solvent annealing, as an alternative to thermal annealing, offers a lower-temperature method to refine the microstructure of PU. We examined the impact of methyl ethyl ketone (MEK), acetone and toluene vapors on a commercial polyether PU, focusing on changes in microphase structure, adsorption kinetics and thermal stability. The SAXS data, analyzed by a polydisperse hard-sphere model, indicated that the degree of phase separation increased upon solvent annealing, and the order of influence exerted by the solvent vapors on the microphase structure follows MEK > acetone > toluene. The <i>in situ</i> variable-temperature SAXS results showed that the solvent-annealed sample had superior thermal stability to the quenched sample. Compared with high-temperature annealing, solvent annealing induced a higher degree of phase separation but did not lead to significant growth of the hard-urethane-segment-rich domains. These findings provide valuable insights into optimizing solvent annealing processes, allowing for advanced applications of PUs where excessive heat may lead to degradation or other undesirable changes.</p>","PeriodicalId":14950,"journal":{"name":"Journal of Applied Crystallography","volume":"58 Pt 2","pages":"564-572"},"PeriodicalIF":6.1,"publicationDate":"2025-03-19","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC11957403/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143763635","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 <i>st</i>-PMMA/C₆₀ helical inclusion complexes via tunable energy landscapes for the application of an Ag SERS-active substrate.","authors":"Song-Yu Tsai, Wen-Tsung Tseng, Jina-Hua Su, Yu-Hao Wang, Yi-Wei Chang, Chia-Hsin Wang, U-Ser Jeng, Kuan-Yi Wu, Chien-Lung Wang, Wei-Tsung Chuang","doi":"10.1107/S1600576725001712","DOIUrl":"10.1107/S1600576725001712","url":null,"abstract":"<p><p>In bio-inspired systems, the hierarchical structures of biomolecules are mimicked to impart desired functions to self-assembled materials. However, these hierarchical architectures are based on multicomponent systems, which require not only a well defined primary structure of functional molecules but also the programming of self-assembly pathways. In this study, we investigate pathway complexity in the energy landscape of the syndiotactic poly(methyl methacrylate) (<i>st</i>-PMMA)/C₆₀/toluene complex system, where C₆₀ and toluene serve as guests in the <i>st</i>-PMMA helical host. Structural characterization revealed that <i>st</i>-PMMA preferentially wraps around C₆₀, forming a thermodynamically favorable helical inclusion complex (HIC). However, during the preparation of the <i>st</i>-PMMA/C₆₀ HIC, a lengthy guest-exchange pathway was discovered, where the <i>st</i>-PMMA/toluene HIC transformed into the <i>st</i>-PMMA/C₆₀ HIC. This pathway complexity may hinder the formation of the <i>st</i>-PMMA/C₆₀ HIC within a feasible timeframe. Given that the energy landscape can be modulated by temperature, the <i>st</i>-PMMA host can directly wrap around C₆₀ in higher temperature ranges, thereby bypassing the guest-exchange process and increasing the <i>st</i>-PMMA/C₆₀ HIC formation efficiency. Additionally, after self-assembly programming, the <i>st</i>-PMMA/C₆₀ HIC can serve as an excellent photochemical reduction site. The well dispersed nanodomains of the <i>st</i>-PMMA/C₆₀ HICs act as nanoparticle templates for surface-enhanced Raman scattering (SERS) hotspot fabrication. We successfully utilized these HIC templates to synthesize self-assembled SERS-active silver nanoparticle arrays, demonstrating their potential for use in chemical sensing applications. In summary, a clear energy landscape can guide supramolecular engineering to achieve the desired supramolecular architectures by selecting appropriate self-assembly pathways.</p>","PeriodicalId":14950,"journal":{"name":"Journal of Applied Crystallography","volume":"58 Pt 2","pages":"553-563"},"PeriodicalIF":6.1,"publicationDate":"2025-03-19","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC11957412/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143764098","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":"Complete online database of maximal subgroups of subperiodic groups at the Bilbao Crystallographic Server.","authors":"Gemma de la Flor, Hans Wondratschek, Mois I Aroyo","doi":"10.1107/S1600576725001499","DOIUrl":"10.1107/S1600576725001499","url":null,"abstract":"<p><p>The section of the Bilbao Crystallographic Server (https://www.cryst.ehu.es) dedicated to subperiodic groups includes the program <i>MAXSUB</i>, which gives online access to the complete database of maximal subgroups of subperiodic groups. All maximal non-isotypic subgroups as well as all maximal isotypic subgroups of indices up to 9 are listed individually, together with the series of maximal isotypic subgroups of subperiodic groups. These data were compared with those of Litvin [(2013), <i>Magnetic group tables, 1-, 2- and 3-dimensional subperiodic groups and magnetic space groups</i>], which revealed several differences, discussed here in detail.</p>","PeriodicalId":14950,"journal":{"name":"Journal of Applied Crystallography","volume":"58 Pt 2","pages":"622-629"},"PeriodicalIF":6.1,"publicationDate":"2025-03-13","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC11957414/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143764090","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 critical step toward far-field laboratory diffraction contrast tomography in Laue focusing geometry.","authors":"Yubin Zhang, Adam Lindkvist","doi":"10.1107/S1600576725001396","DOIUrl":"10.1107/S1600576725001396","url":null,"abstract":"<p><p>Recent simulations have demonstrated the promising potential of far-field laboratory diffraction contrast tomography (FF-LabDCT) in the Laue focusing geometry for 3D mapping of grain-averaged deviatoric strain tensors, achieving a strain uncertainty as low as 1 × 10^-4 [Lindkvist & Zhang (2022). <i>J. Appl. Cryst.</i> <b>55</b>, 21-32]. The present work takes a critical step towards realizing this tool. It presents the first attempt at implementing FF-LabDCT using a Zeiss Xradia 520 Versa X-ray microscope, including both hardware and software development. A new algorithm, LabDBB, which adapts the previously developed dictionary-based branch and bound (DBB) principles, is implemented for indexing FF-LabDCT data. The performance of LabDBB is evaluated by comparing the indexed grain crystallographic orientations and center of mass positions with those obtained using near-field LabDCT within the same gauge volume of a fully recrystallized iron sample. Finally, the challenges related to fitting the grain-averaged deviatoric strain tensor using the current FF-LabDCT setup are identified. The strain analysis suggests that, once these challenges are addressed, a strain uncertainty as low as 2 × 10^-4 could potentially be achieved. This work demonstrates the possibility for developing a tool capable of 3D grain-scale strain analysis with high strain precision in home laboratories.</p>","PeriodicalId":14950,"journal":{"name":"Journal of Applied Crystallography","volume":"58 Pt 2","pages":"447-457"},"PeriodicalIF":2.8,"publicationDate":"2025-03-13","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC11957408/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143764086","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}