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3,139 items found (0 items not approved), displaying 1 to 10.[First/Prev] 1, 2, 3, 4, 5, 6, 7, 8 [Next/Last]

Instruments / Technical Area	Publication Details	Published
I22-Small angle scattering & Diffraction	Tailoring viscoelastic properties of dynamic supramolecular poly(butadiene)-based elastomers M. Hyder , A. D. O'Donnell , A. M. Chippindale , I.m. German , J.l. Harries , O. Shebanova , I. W. Hamley , W. Hayes Materials Today Chemistry 26 DOI: 10.1016/j.mtchem.2022.101008 Diamond Proposal Number(s): [22909] Open Access Show Abstract ▼ Abstract: The discovery and development of new adhesive materials is critical for real-world applications of polymeric composite materials. Herein, we report the design and synthesis of a library of structurally related phase-separated supramolecular polyurethanes whose mechanical properties and adhesive characteristics can be enhanced through minor structural modifications of the polymer end-group. The interplay between phase separation of the hard domain polar end-groups and soft polybutadiene domains, coupled with tuneable self-assembly afforded by the polar end-groups, gives rise to a class of materials with tuneable mechanical properties. Exceptionally strong supramolecular adhesives and mechanically robust self-healing elastomers were identified. The mechanical properties were investigated through tensile testing. Finally, rheological analysis of the supramolecular materials was used to identify suitable healing and adhesive temperatures in addition to elucidate the supramolecular polyurethanes' thermal-responsive nature.	Dec 2022
	Mechanical performance and deformation mechanisms at cryogenic temperatures of 316L stainless steel processed by laser powder bed fusion: In situ neutron diffraction Lei Tang , Oxana V. Magdysyuk , Fuqing Jiang , Yiqiang Wang , Alexander Evans , Saurabh Kabra , Biao Cai Scripta Materialia 218 DOI: 10.1016/j.scriptamat.2022.114806 Show Abstract ▼ Abstract: Manufacturing austenitic stainless steels (ASSs) using additive manufacturing is of great interest for cryogenic applications. Here, the mechanical and microstructural responses of a 316L ASS built by laser powder bed fusion were revealed by performing in situ neutron diffraction tensile tests at the low-temperature range (from 373 to 10 K). The stacking fault energy almost linearly decreased from 29.2 ± 3.1 mJm−2 at 373 K to 7.5 ± 1.7 mJm−2 at 10 K, with a slope of 0.06 mJm−2K−1, leading to the transition of the dominant deformation mechanism from strain-induced twinning to martensite formation. As a result, excellent combinations of strength and ductility were achieved at the low-temperature range.	Sep 2022
	Emerging chemical heterogeneities in a commercial 18650 NCA Li-ion battery during early cycling revealed by synchrotron X-ray diffraction tomography D. Matras , T. E. Ashton , H. Dong , M. Mirolo , I. Martens , J. Drnec , J. A. Darr , P. D. Quinn , S. D. M. Jacques , A. M. Beale , A. Vamvakeros Journal Of Power Sources 539 DOI: 10.1016/j.jpowsour.2022.231589 Show Abstract ▼ Abstract: Synchrotron X-ray diffraction computed tomography (XRD-CT) was employed to study a commercial 18650 cylindrical LiNi0.8Co0.15Al0.5O2 (NCA) battery under operating conditions and during seven cycles. The analysis of the spatially-resolved diffraction patterns revealed multiple chemical heterogeneities related to the lithium distribution in both the cathode and the anode. It is shown that during the charging of the battery, the anode exhibits different degrees of activity regarding the lithiation process. Explicitly, the following three regions were identified: a uniform/homogenous lithiation, a delayed lithiation and an inactive-to-lithiation region. The inactive-to-lithiation anode region was a result of the specific cell geometry (i.e. due to lack of cathode tape opposite these anode areas) and throughout the cycling experiments remained present in the form of LiC30-30+. The delayed lithiation region was seen to have a direct impact on the properties of NCA in its close proximity during the battery discharging, preventing its full lithiation. Further to this, the aluminum tab negatively affected the NCA in direct contact with it, leading to different lattice parameter a and c evolution compared to the rest of the cathode.	Aug 2022
I12-JEEP: Joint Engineering, Environmental and Processing	Mechanistic insights into the initial explosion in the deflagration-to-detonation transition Trevor A. Feagin , Eric M. Heatwole , David S. Eastwood , Ian Lopez-Pulliam , Thomas Connolley , Neil K. Bourne , Gary Parker Combustion And Flame 242 DOI: 10.1016/j.combustflame.2022.112175 Diamond Proposal Number(s): [22393] Show Abstract ▼ Abstract: This work presents an imaging study of the complex and often overlooked early-onset mechanisms of the deflagration-to-detonation transition (DDT). Columns of granular octahydro-1,3,5,7-tetranitro-1,3,5,7-tetrazocine (HMX) doped with tungsten tracer particles are ignited thermally by hot wire and the resulting reactions are studied via high-speed X-ray radiography utilizing the Diamond Light Source synchrotron. The observed results provide insights into the initial development of the DDT process, resulting in a proposed mechanism for the slow initial steps in DDT for thermally ignited, low bulk-density granular explosive contained in a quasi-one dimensional tube configuration. In order to clarify the proposed mechanism, the terms preferential flow channel and matrix burning are adapted from the soil mechanics and hydrology literature to further elucidate the role of convective burning in DDT. The proposed mechanism helps to clarify the ongoing debate on the transport of gases in the Baer–Nunziato and reduced Baer–Nunziato models and suggests that applicability of each interpretation depends on which step in the mechanism is being described.	Aug 2022
I22-Small angle scattering & Diffraction	A structural study of the self-association of different starches in presence of bacterial cellulose fibrils P. Díaz-Calderón , E. Simone , A. I. I. Tyler , J. Enrione , T. Foster Carbohydrate Polymers 288 DOI: 10.1016/j.carbpol.2022.119361 Diamond Proposal Number(s): [22659] Show Abstract ▼ Abstract: A multi-analytical study was performed to analyse the effect of bacterial cellulose (BCF) on the self-association of starches with different amylose content (wheat, waxy-maize), assessing macrostructural properties (rheology, gel strength) and some nano and sub-nano level features (small and wide-angle X-ray scattering). Although pasting viscosities and G′ were significantly increased by BCF in both starches, cellulose did not seem to promote the self-association of amylose in short-range retrogradation. A less elastic structure was reflected by a 2–3-fold increase in loss factor (G″/G′) at the highest BCF concentration tested. This behavior agreed with the nano and sub-nano characterisation of the samples, which showed loss of starch lamellarity and incomplete full recovery of an ordered structure after storage at 4 °C for 24 h. The gel strength data could be explained by the contribution of BCF to the mechanical response of the sample. The information gained in this work is relevant for tuning the structure of tailored starch-cellulose composites.	Jul 2022
B21-High Throughput SAXS	3D-printed SAXS chamber for controlled in situ dialysis and optical characterization Tamara Ehm , Julian Philipp , Martin Barkey , Martina Ober , Achim Theo Brinkop , David Simml , Miriam Von Westphalen , Bert Nickel , Roy Beck , Joachim O. Rädler Journal Of Synchrotron Radiation 29 DOI: 10.1107/S1600577522005136 Diamond Proposal Number(s): [24693, 21971] Open Access Show Abstract ▼ Abstract: 3D printing changes the scope of how samples can be mounted for small-angle X-ray scattering (SAXS). In this paper a 3D-printed X-ray chamber, which allows for in situ exchange of buffer and in situ optical transmission spectroscopy, is presented. The chamber is made of cyclic olefin copolymers (COC), including COC X-ray windows providing ultra-low SAXS background. The design integrates a membrane insert for in situ dialysis of the 100 µl sample volume against a reservoir, which enables measurements of the same sample under multiple conditions using an in-house X-ray setup equipped with a 17.4 keV molybdenum source. The design's capabilities are demonstrated by measuring reversible structural changes in lipid and polymer systems as a function of salt concentration and pH. In the same chambers optical light transmission spectroscopy was carried out measuring the optical turbidity of the mesophases and local pH values using pH-responsive dyes. Microfluidic exchange and optical spectroscopy combined with in situ X-ray scattering enables vast applications for the study of responsive materials.	Jul 2022
I12-JEEP: Joint Engineering, Environmental and Processing	Implementing and evaluating far-field 3D X-ray diffraction at the I12 JEEP beamline, Diamond Light Source James A. D. Ball , Anna Kareer , Oxana V. Magdysyuk , Stefan Michalik , Anastasia Vrettou , Neal Parkes , Thomas Connolley , David M. Collins Journal Of Synchrotron Radiation 29 DOI: 10.1107/S1600577522004088 Diamond Proposal Number(s): [26376] Open Access Show Abstract ▼ Abstract: Three-dimensional X-ray diffraction (3DXRD) is shown to be feasible at the I12 Joint Engineering, Environmental and Processing (JEEP) beamline of Diamond Light Source. As a demonstration, a microstructually simple low-carbon ferritic steel was studied in a highly textured and annealed state. A processing pipeline suited to this beamline was created, using software already established in the 3DXRD user community, enabling grain centre-of-mass positions, orientations and strain tensor elements to be determined. Orientations, with texture measurements independently validated from electron backscatter diffraction (EBSD) data, possessed a ∼0.1° uncertainty, comparable with other 3DXRD instruments. The spatial resolution was limited by the far-field detector pixel size; the average of the grain centre of mass position errors was determined as ±∼80 µm. An average per-grain error of ∼1 × 10−3 for the elastic strains was also measured; this could be reduced in future experiments by improving sample preparation, geometry calibration, data collection and analysis techniques. Application of 3DXRD onto I12 shows great potential, where its implementation is highly desirable due to the flexible, open architecture of the beamline. User-owned or designed sample environments can be used, thus 3DXRD could be applied to previously unexplored scientific areas.	Jul 2022
I11-High Resolution Powder Diffraction	Highly efficient proton conduction in the metal–organic framework material MFM-300(Cr)·SO4(H3O)2 Jin Chen , Qingqing Mei , Yinlin Chen , Christopher Marsh , Bing An , Xue Han , Ian P. Silverwood , Ming Li , Yongqiang Cheng , Meng He , Xi Chen , Weiyao Li , Meredydd Kippax-Jones , Danielle Crawshaw , Mark D. Frogley , Sarah J. Day , Victoria García-Sakai , Pascal Manuel , Anibal J. Ramirez-Cuesta , Sihai Yang , Martin Schroeder Journal Of The American Chemical Society DOI: 10.1021/jacs.2c04900 Diamond Proposal Number(s): [29649] Open Access Show Abstract ▼ Abstract: The development of materials showing rapid proton conduction with a low activation energy and stable performance over a wide temperature range is an important and challenging line of research. Here, we report confinement of sulfuric acid within porous MFM-300(Cr) to give MFM-300(Cr)·SO4(H3O)2, which exhibits a record-low activation energy of 0.04 eV, resulting in stable proton conductivity between 25 and 80 °C of >10–2 S cm–1. In situ synchrotron X-ray powder diffraction (SXPD), neutron powder diffraction (NPD), quasielastic neutron scattering (QENS), and molecular dynamics (MD) simulation reveal the pathways of proton transport and the molecular mechanism of proton diffusion within the pores. Confined sulfuric acid species together with adsorbed water molecules play a critical role in promoting the proton transfer through this robust network to afford a material in which proton conductivity is almost temperature-independent.	Jul 2022
B22-Multimode InfraRed imaging And Microspectroscopy	Nanoconfinement of tetraphenylethylene in zeolitic metal-organic framework for turn-on mechanofluorochromic stress sensing Yang Zhang , Tao Xiong , Annika F. Moeslein , Samraj Mollick , Vishal Kachwal , Arun Singh Babal , Nader Amin , Jin-Chong Tan Applied Materials Today 27 DOI: 10.1016/j.apmt.2022.101434 Diamond Proposal Number(s): [25407] Show Abstract ▼ Abstract: Mechanofluorochromic materials are of great significance for the fabrication of innovative sensors and optoelectronics. However, efficient mechanofluorochromic materials are rarely explored due to the deficiency of existing design strategies. Here, we demonstrate the incarceration of aggregation-induced emission (AIE) materials within metal-organic framework (MOF) single crystals to construct a composite system with turn-on mechanofluorochromism. A new type of AIE@MOF material was designed: integrating a zeolitic MOF (ZIF-71) and tetraphenylethylene (TPE, a topical AIE material) to generate a TPE@ZIF-71 system with exceptional turn-on type mechanofluorochromism. Using terahertz vibrational spectroscopy, we show the unique fluorochromism mainly emanates from the enhanced nanoconfinement effect exerted by ZIF-71 host on TPE guest under pressure. Compared with pure TPE, we demonstrate the nanoconfinement in AIE@MOF not only changes the TPE's turn-off type sensing behavior to a turn-on type, but boosts the original sensitivity markedly by tenfold. Significantly, because ZIF-71 prevents the spontaneous recrystallization of TPE upon unloading, this allows TPE@ZIF-71 to record the stress history. This is the first demonstration of the Guest@MOF system combining the concepts of AIE and MOF; its promising properties and potential engineering applications will stimulate new directions pertaining to luminescent stress sensors and smart optics.	Jun 2022
I11-High Resolution Powder Diffraction	Modulated self-assembly of an interpenetrated MIL-53 Sc metal–organic framework with excellent volumetric H2 storage and working capacity A. J. R. Thom , D. G. Madden , R. Bueno-Perez , A.n. Al Shakhs , C. T. Lennon , R. J. Marshall , C. A. Walshe , C. Wilson , C. A. Murray , S. P. Thompson , G. F. Turner , D. Bara , S. A. Moggach , D. Fairen-Jimenez , R. S. Forgan Materials Today Chemistry 24 DOI: 10.1016/j.mtchem.2022.100887 Diamond Proposal Number(s): [22028] Open Access Show Abstract ▼ Abstract: To achieve optimal performance in gas storage and delivery applications, metal–organic frameworks (MOFs) must combine high gravimetric and volumetric capacities. One potential route to balancing high pore volume with suitable crystal density is interpenetration, where identical nets sit within the void space of one another. Herein, we report an interpenetrated MIL-53 topology MOF, named GUF-1, where one-dimensional Sc(μ2-OH) chains are connected by 4,4′-(ethyne-1,2-diyl)dibenzoate linkers into a material that is an unusual example of an interpenetrated MOF with a rod-like secondary building unit. A combination of modulated self-assembly and grand canonical Monte Carlo simulations are used to optimise the porosity of GUF-1; H2 adsorption isotherms reveal a moderately high Qst for H2 of 7.6 kJ/mol and a working capacity of 41 g/L in a temperature–pressure swing system, which is comparable to benchmark MOFs. These results show that interpenetration is a potentially viable route to high-performance gas storage materials comprised of relatively simple building blocks.	Jun 2022

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