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Instruments / Technical Area	Publication Details	Published
I12-JEEP: Joint Engineering, Environmental and Processing	Vitrification of non-meltable zeolitic-imidazolate frameworks Mohamed. A. Ali , Zhihua Qiao , Wessel M. W. Winters , Biao Cai , Moushira. A. Mohamed , Yanfei Zhang , Xiaofeng Liu , Yuanzheng Yue , Jianrong Qiu Materials Chemistry Frontiers 43 DOI: 10.1039/D4QM00971A Diamond Proposal Number(s): [36935] Show Abstract ▼ Abstract: The decomposition of porous zeolitic-imidazolate frameworks (ZIFs) poses a significant challenge in discovering new melt-quenched ZIF glasses characterized by high porosity. This challenge has sparked tremendous interest among scientists, driving the pursuit of innovative methods to vitrify non-meltable ZIFs for various applications. Herein, we show a universal approach for synthesizing glasses and foams from non-meltable and porous ZIFs, such as 2D ZIF-7 and 3D ZIF-8, which stand as the most promising porous materials of the ZIF family. This approach is based on the combination of liquid-mediated sequential structure perturbation and post-heat treatment, yielding a variety of highly microporous ZIF foams like glass. The synthesized ZIF foams exhibit superior gas adsorption capacities compared to melt-quenched ones. The as-fabricated membranes based on ZIF foams demonstrate ultrahigh H2 permeance and good H2/CH4 selectivity. In comparison to the melt-quenching technique, our structural perturbation strategy allows for the synthesis of a significantly greater quantity of glasses and foams from a single batch. It greatly broadens the composition range of ZIFs for glass and foam formation. Consequently, this study holds significant potential for upscaling the synthesis of microporous ZIF foams like glass to address a diverse array of applications such as energy storage, gas sorption and separation. Our work provides insight into the formation mechanism of non-melt-quenched glasses.	Jan 2025
I12-JEEP: Joint Engineering, Environmental and Processing	In-situ synchrotron investigation of the elastic and tensile properties of oxide dispersion strengthened EUROFER97 steel Tay Sparks , Slava Kuksenko , Michael Gorley , Jan Hoffmann , Yu-Lung Chiu , Thomas Connolley , Michael Rieth , Yiqiang Wang , Biao Cai Acta Materialia 45 DOI: 10.1016/j.actamat.2024.119876 Diamond Proposal Number(s): [19251] Open Access Show Abstract ▼ Abstract: The augmentation of mechanical properties of reduced activation ferritic martensitic steels through the introduction of creep resistant nano-oxide particles produces a class of oxide dispersion strengthened steels, which have attracted significant interest as candidates for first wall supporting structural materials in future nuclear fusion reactors. In the present work, the effect of temperature on the elastic properties and micro-mechanics of 0.3 wt% Y2O3 oxide dispersion strengthened steel EUROFER97 is investigated using synchrotron high energy X-ray diffraction in-situ tensile testing at elevated temperatures, alongside the non-oxide strengthened base steel as a point of comparison. The single crystal elastic constants of both steels are experimentally determined through analysis of the diffraction peaks corresponding to specific grain families in the polycrystalline samples investigated. The effect of temperature on the evolving dislocation density and character in both materials is interrogated, providing insight into deformation mechanisms. Finally, a constitutive flow stress model is used to evaluate the factors affecting yield strength, allowing the strengthening contribution of the oxide particles to be assessed, and correlation between the thermally driven microstructural behaviour and macroscopic mechanical response to be determined.	Apr 2024
I15-1-X-ray Pair Distribution Function (XPDF)	Fabrication of super-sized metal inorganic-organic hybrid glass with supramolecular network via suppressing crystallization approach Mohamed. A. Ali , Wessel M. W. Winters , Moushira A. Mohamed , Dezhi Tan , Guojun Zheng , Rasmus S. K. Madsen , Oxana V. Magdysyuk , Maria Diaz-Lopez , Biao Cai , Nan Gong , Yijue Xu , Ivan Hung , Zhehong Gan , Sabyasachi Sen , Hong-Tao Sun , Thomas D. Bennett , Xiaofeng Liu , Yuanzheng Yue , Jianrong Qiu Angewandte Chemie International Edition DOI: 10.1002/anie.202218094 Diamond Proposal Number(s): [30401] Show Abstract ▼ Abstract: Glassy metal coordination compounds (MCC) [e.g., metal-organic framework (MOF), coordination polymer, and metal inorganic-organic complex (MIOC)] are emerging members of the hybrid glass family. So far, a limited number of crystalline MCCs can be converted into glasses by the melt-quenching. Here, we report a universal wet-chemistry method, by which the super-sized supramolecular MIOC glasses can be synthesized from non-meltable MOFs. Alcohol and acid were used as agents to inhibit crystallization. The MIOC glasses demonstrate unique features including high transparency, shaping capability, and anisotropic network. Directional photoluminescence with a large polarization ratio (~47%) was observed from samples doped with organic dyes. This crystallization-suppressing approach enables fabrication of MCC glasses, which cannot be achieved by conventional vitrification methods, and thus allows for exploring new MCC glasses possessing photonic functionalities.	Feb 2023
	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
I12-JEEP: Joint Engineering, Environmental and Processing	Mechanical characterisation of V-4Cr-4Ti alloy: tensile tests under high energy synchrotron diffraction Tay Sparks , Duc Nguyen-Manh , Pengfei Zheng , Jan S. Wróbel , Damian Sobieraj , Michael Gorley , Thomas Connolley , Christina Reinhard , Yiqiang Wang , Biao Cai Journal Of Nuclear Materials 29 DOI: 10.1016/j.jnucmat.2022.153911 Diamond Proposal Number(s): [19251] Show Abstract ▼ Abstract: Vanadium base alloys represent potentially promising candidate structural materials for use in nuclear fusion reactors due to vanadium's low activity, high thermal strength, and good swelling resistance. In this work, the mechanical properties of the current frontrunner vanadium base alloy, V-4Cr-4Ti, have been interrogated using in-situ high energy X-ray diffraction (XRD) tensile testing at varying temperatures. The single crystal elastic constants of the samples were determined from the in-situ XRD data and used to evaluate results from density functional theory calculations. Polycrystalline elastic properties and Zener anisotropy were calculated from the single crystal elastic constants produced, revealing the effect of elevated temperature on the alloy's elastic properties. These results characterise important thermomechanical properties, valuable in mechanical modelling, that will allow further and improved analysis of the structural suitability of V-4Cr-4Ti ahead of alloy adoption in the mainstream.	Jul 2022
I12-JEEP: Joint Engineering, Environmental and Processing	Mechanisms controlling ductility loss from abrupt Strain Path Changes in a low carbon steel Anastasia Vrettou , Hiroto Kitaguchi , Biao Cai , Thomas Connolley , David M. Collins Materials Science And Engineering: A 4 DOI: 10.1016/j.msea.2022.143091 Diamond Proposal Number(s): [21103] Show Abstract ▼ Abstract: The effect of Strain Path Changes (SPCs) on the mechanical properties and crystal-level features of deformation for a single phase, ferritic steel has been investigated. SPCs were applied via a two-step deformation process, which included pre-straining via cold rolling, followed by uniaxial tension. The pre-strain magnitude and direction, as well as the tensile direction, varied between the specimens. The role of texture and micromechanics were examined in-situ, via Synchrotron X-ray Diffraction (SXRD), and ex-situ, via Electron Backscatter Diffraction (EBSD). Abrupt strain paths (i.e. strain paths where the pre-strain and the subsequent loading directions differ; here they are orthogonal) result in a significant ductility reduction, becoming more prevalent for high pre-strain magnitudes. The macroscopic response, as well as the texture configuration were greatly dependent on the pre-strain direction but were insensitive to the direction of uniaxial tension. Increasing pre-strain magnitudes resulted in a stagnation of lattice strain hardening rates in all macroscopic directions and in a significant increase in the Geometrically Necessary Dislocation (GND) densities. This was vastly increased for specimens rolled perpendicular to the as-received prior rolling direction. No correlation was found between the GND density and the grain orientation, eliminating this as a controlling ductility factor for BCC ferrite. Instead, the initial texture and the texture developed in a subsequent pre-strain influences the density of dislocations accumulated in all grains, and ultimately determines ductility.	Apr 2022
I12-JEEP: Joint Engineering, Environmental and Processing	Revealing growth mechanisms of faceted Al2Cu intermetallic compounds via high-speed synchrotron X-ray tomography Zihan Song , Oxana V. Magdysyuk , Tay Sparks , Yu-Lung Chiu , Biao Cai Acta Materialia 5 DOI: 10.1016/j.actamat.2022.117903 Diamond Proposal Number(s): [19216] Open Access Show Abstract ▼ Abstract: This study usedhigh-speed synchrotron X-ray tomography to image the growth of Al2Cu intermetallic compoundsin 4D (3D plus time) during solidification of Al-45wt%Cu alloy. Two categories of growth patterns (basic units and dendrites) are identified. Basic unitsare elongated rods whose cross-section areL, U orhollow-rectangularshapes. The transition from L pattern to U and finally to hollow-rectangularshaped morphologywas observed. Faceted dendritic patterns include equiaxed prism and columnar dendrites. Self-repeated layer-by-layer stacking of the basic units (such as L shaped particles) is proposed as a governing mechanism for the growth of Al2Cu faceted dendrites. The growth orientation and morphologies of these patterns are strongly influenced by solidification conditions (temperature gradients, cooling rates and external magnetic fields). Another finding is that when rotating Al-45wt%Cu during upwards directional solidification,under a transverse magnetic field of 0.5T, highly refined and well aligned Al2Cu intermetallic compounds are obtained, much finer than those without the imposition of the magnetic field. This is attributed to a rotational stirring flow that modulates and regulates the temperature and solute distribution.The developed experimental findings provide a physical understanding of the formation of faceted intermetallic compounds during solidification.	Mar 2022
B16-Test Beamline	Influence of microdefects in rust layer of weathering steel on corrosion resistance from 3D observation by synchrotron X-ray micro tomography Shunichi Tachibana , Biao Cai , Alison Davenport , Shinichi Miura , Hongchang Wang , Igor P. Dolbnya Materials Today Communications 83 DOI: 10.1016/j.mtcomm.2022.103219 Diamond Proposal Number(s): [20251] Show Abstract ▼ Abstract: Microdefects in the rust layer of conventional steel and weathering steel were investigated by synchrotron X-ray micro tomography to understand the effect of defects on corrosion resistance. The rust layer of the weathering steel contained fewer and smaller defects than that of the conventional steel. A good correlation existed between the volume of defects and ion permeation of the rust layer obtained by EIS. In comparison with the conventional steel, the tomography results indicated that a protective layer formed on the weathering steel.	Feb 2022
I12-JEEP: Joint Engineering, Environmental and Processing	Synchrotron characterisation of ultra-fine grain TiB2/Al-Cu composite fabricated by laser powder bed fusion Sheng Li , Biao Cai , Ranxi Duan , Lei Tang , Zihan Song , Dominic White , Oxana Magdysyuk , Moataz M. Attallah Acta Metallurgica Sinica (english Letters) 23 DOI: 10.1007/s40195-021-01317-y Diamond Proposal Number(s): [22506] Open Access Show Abstract ▼ Abstract: Isotropy in microstructure and mechanical properties remains a challenge for laser powder bed fusion (LPBF) processed materials due to the epitaxial growth and rapid cooling in LPBF. In this study, a high-strength TiB2/Al-Cu composite with random texture was successfully fabricated by laser powder bed fusion (LPBF) using pre-doped TiB2/Al-Cu composite powder. A series of advanced characterisation techniques, including synchrotron X-ray tomography, correlative focussed ion beam–scanning electron microscopy (FIB-SEM), scanning transmission electron microscopy (STEM), and synchrotron in situ X-ray diffraction, were applied to investigate the defects and microstructure of the as-fabricated TiB2/Al-Cu composite across multiple length scales. The study showed ultra-fine grains with an average grain size of about 0.86 μm, and a random texture was formed in the as-fabricated condition due to rapid solidification and the TiB2 particles promoting heterogeneous nucleation. The yield strength and total elongation of the as-fabricated composite were 317 MPa and 10%, respectively. The contributions of fine grains, solid solutions, dislocations, particles, and Guinier–Preston (GP) zones were calculated. Failure was found to be initiated from the largest lack-of-fusion pore, as revealed by in situ synchrotron tomography during tensile loading. In situ synchrotron diffraction was used to characterise the lattice strain evolution during tensile loading, providing important data for the development of crystal-plasticity models.	Sep 2021
I12-JEEP: Joint Engineering, Environmental and Processing	In situ quantification of crystallisation kinetics of plagioclase and clinopyroxene in basaltic magma: Implications for lava flow Nolwenn Le Gall , Fabio Arzilli , Giuseppe La Spina , Margherita Polacci , Biao Cai , Margaret E. Hartley , Nghia T. Vo , Robert C. Atwood , Danilo Di Genova , Sara Nonni , Edward W. Llewellin , Mike R. Burton , Peter D. Lee Earth And Planetary Science Letters 568 DOI: 10.1016/j.epsl.2021.117016 Diamond Proposal Number(s): [12392] Show Abstract ▼ Abstract: Crystallisation is a complex process that significantly affects the rheology of magma, and thus the flow dynamics during a volcanic eruption. For example, the evolution of crystal fraction, size and shape has a strong impact on the surface crust formation of a lava flow, and accessing such information is essential for accurate modelling of lava flow dynamics. To investigate the role of crystallisation kinetics on lava flow behaviour, we performed real-time, in situ synchrotron X-ray microtomography, studying the influence of temperature-time paths on the nucleation and growth of clinopyroxene and plagioclase in an oxidised, nominally anhydrous basaltic magma. Crystallisation experiments were performed at atmospheric pressure in air and temperatures from 1250 °C to 1100 °C, using a bespoke high-temperature resistance furnace. Depending on the cooling regime (single step versus continuous), two different crystal phases (either clinopyroxene or plagioclase) were produced, and we quantified their growth from both global and individual 3D texture analyses. The textural evolution of charges suggests that suppression of crystal nucleation is due to changes in the melt composition with increasing undercooling and time. Using existing viscosity models, we inferred the effect of crystals on the viscosity evolution of our crystal-bearing samples to trace changes in rheological behaviour during lava emplacement. We observe that under continuous cooling, both the onsets of the pāhoehoe-‘a‘ā transition and of non-Newtonian behaviour occur within a shorter time frame. With varying both temperature and time, we also either reproduced or approached the clinopyroxene and plagioclase phenocryst abundances and compositions of the Etna lava used as starting material, demonstrating that real-time synchrotron X-ray tomography is an ideal approach to unravel the final solidification history of basaltic lavas. This imaging technology has indeed the potential to provide input into lava flow models and hence our ability to forecast volcanic hazards.	Aug 2021

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