I12-JEEP: Joint Engineering, Environmental and Processing
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Ilaria
Quaratesi
,
Ioan
Călinescu
,
Petre
Chipurici
,
Elisa-Gabriela
Dumbravă
,
Andrei
Cucos
,
Mohamed Yassine
Zaki
,
Pellegrino
La Manna
,
Adrian
Bercea
,
Miruna Silvia
Stan
,
Stefan
Michalik
,
Chloe
Pearce
,
Marianne
Odlyha
,
Genoveva
Burca
,
Elena
Badea
Diamond Proposal Number(s):
[35634]
Open Access
Abstract: This study presents an ultrasound-assisted synthesis of β-cyclodextrin/hydroxyapatite composites to be used as green and safe auxiliaries in the tanning process. A combination of spectroscopic and non-spectroscopic techniques such as DLS (dynamic light scattering), ZP (zeta potential), XRD (X-ray diffraction), SEM (scanning electron microscopy) and ATR-FTIR (attenuated total reflectance-Fourier transform infrared spectroscopy) were used to thoroughly characterize the eight composites obtained by varying the ultrasound process parameters. While not cytotoxic, all composites had strong antibacterial action against Brevibacterium lines, Staphylococcus aureus, Escherichia coli, and Staphylococcus epidermis. All composites underwent lab-scale tanning tests, but only those exhibiting the most suitable set of tanning abilities underwent pilot-scale testing. The composites' interaction with the collagen matrix was assessed by micro-DSC (micro-differential scanning calorimetry), TG/DTG/DTA (thermal analysis), 1H unilateral NMR (proton nuclear magnetic resonance), ATR-FTIR, in-situ temperature synchrotron-based XRD and standard tests (UNI EN ISO 3380: 2015, UNI EN ISO 2589: 2016, UNI EN ISO 105- B02:2014). Thermal stability, dye penetration, thickness, colour fastness, surface appearance and microbiological protection were all improved for the leather treated with a small amount of composite added to the wet finish float. These findings demonstrate the benefits of β-cyclodextrin/hydroxyapatite composites as safe and sustainable tanning additives.
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Apr 2025
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I12-JEEP: Joint Engineering, Environmental and Processing
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Diamond Proposal Number(s):
[37256]
Open Access
Abstract: he high brilliance and coherence of light generated at synchrotron facilities make synchrotron X-ray imaging an invaluable tool for the non-destructive analysis of samples across a range of interdisciplinary sciences. For samples with low attenuation contrast, phase-contrast imaging and phase-retrieval techniques can be used to enhance image contrast and provide complementary phase-shift information. In this work, we demonstrate the phase-contrast imaging capabilities of the Diamond Light Source I12-JEEP beamline using two samples: a fly encased in 4 mm of steel, and a lower chicken leg (drumstick) bones with surrounding soft tissue. Techniques such as X-ray phase-contrast imaging, near-field speckle-based phase-contrast tomography and propagation-based (in-line) phase-contrast tomography are investigated; additionally, the effects of propagation distance, speckle mask material, number of speckle positions, and phase-retrieval algorithm on the quality of radiographic images and reconstructed tomography volumes are compared. The experimental setup, data acquisition settings, as well as phase retrieval and tomography reconstruction parameters are detailed, and concluding remarks are made regarding the strengths and weaknesses of each technique, their use case, and how the data acquisition parameters can be optimised for an extended field-of-view or in-situ imaging setup available at I12.
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Jan 2025
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B18-Core EXAFS
I11-High Resolution Powder Diffraction
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Prathmesh
Bhadane
,
Dhruv
Menon
,
Prateek
Goyal
,
Mohammad Reza
Alizadeh Kiapi
,
Biraj
Kanta Satpathy
,
Arianna
Lanza
,
Iuliia
Mikulska
,
Rebecca
Scatena
,
Stefan
Michalik
,
Priya
Mahato
,
Mehrdad
Asgari
,
Xu
Chen
,
Swaroop
Chakraborty
,
Abhijit
Mishra
,
Iseult
Lynch
,
David
Fairen-Jimenez
,
Superb K.
Misra
Diamond Proposal Number(s):
[39677, 38403]
Abstract: Recycling and recovery of rare earth elements (REEs) from electronic wastes can accelerate efforts to mitigate the environmental burden associated with their excessive mining, while catering for their growing demand. Contemporary recovery strategies are yet to make an impact at an industrial scale due to low REE uptakes, complex mechanisms, and high regeneration energies, leading to an overall poor scalability. Here, we report a two-dimensional metal–organic framework (BNMG-1) featuring a dense arrangement of active adsorption sites for the high uptake of heavy and light REEs. BNMG-1 with a lateral dimension of ca. 350 nm and a thickness of 14 nm was synthesized via a facile one-pot reaction using a green solvent under room temperature and atmospheric pressure. The two-dimensional structure of BNMG-1 was resolved using three-dimensional electron diffraction and EXAFS analysis. Batch experiments showed BNMG-1 to have an adsorption capacity of 355.8 mg/g for Nd3+, 323.1 mg/g for Y3+, 331 mg/g for Dy3+, 329mg/g for Tb3+ and 333 mg/g for Eu3+, which is a near-benchmark performance for a non-functionalised MOF. The adsorption efficiency for Nd3+ reached 99 % by 6 h and 88 % by 48 h for Y3+. The adsorption efficiency did not get affected over a pH range of 3 to 6 and retained > 99 % of its adsorption capacity for up to 4 cycles. For application on real-life samples, CFL lamp waste and waste magnets were used as a reservoir of heavy (Yttrium) and light (Neodymium) REEs. BNMG-1 demonstrates an efficient recovery of 57 % for Neodymium from scrap magnets and 27 % for Yttrium from waste fluorescent lamps. This performance, which is maintained under acidic conditions and over multiple cycles, highlights the competitiveness of BNMG-1 for the economic large-scale recovery of REEs.
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Dec 2024
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I15-1-X-ray Pair Distribution Function (XPDF)
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Diamond Proposal Number(s):
[20770]
Abstract: The structure of evaporated amorphous GexSbxTe100−2x (x = 6, 9, 13) alloys was investigated by neutron diffraction, X-ray diffraction, and extended X-ray absorption spectroscopy at the Ge, Sb, and Te K-edges. Large-scale structural models were generated by fitting the experimental datasets (five for each composition) simultaneously in the framework of the reverse Monte Carlo simulation technique. It was found that the alloys are chemically ordered (Ge and Sb have predominantly Te neighbors) and within the experimental uncertainty, each component satisfies the 8 – N rule. A comparison with the pair correlation functions of melt-quenched Ge20Te80 revealed that the first minimum of gTeTe(r) is shallower in the ternary alloys than in Ge20Te80. On the other hand, the separation of the first and second coordination environments of Ge atoms is stronger in the Ge–Sb–Te alloys investigated.
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Nov 2024
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Open Access
Abstract: Short range order of a ternary Mg82Ca8Au10 biodegradable amorphous alloy was studied by combining diffraction datasets and Au L3 edge EXAFS data by the Reverse Monte Carlo simulation technique. It was found that while the Mg–Mg bond length agrees well with the empirical atomic diameter of Mg, both the Mg–Ca and Mg–Au mean interatomic distances are ∼9 % shorter than the sum of the corresponding atomic radii. The Ca–Au bond length exhibits ∼14 % shortening. The linear expansion coefficients of the glass determined from the temperature induced shift of the first peak of the structure factor and the reduced pair distribution function are ∼3.7 × 10−5 K−1 and ∼3.1 × 10−5 K−1, respectively. During devitrification, two crystalline phases emerge from the amorphous alloy: hexagonal AuMg3 and the solid solution of Ca in hexagonal close packed Mg. The thermal expansion behaviour of the AuMg3 unit cell was also determined using diffraction data.
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Oct 2024
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I12-JEEP: Joint Engineering, Environmental and Processing
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Diamond Proposal Number(s):
[34953]
Open Access
Abstract: We use in situ synchrotron X-ray diffraction measurements to monitor the solvothermal crystallization mechanism of the aperiodic metal–organic framework TRUMOF-1. Following an initial incubation period, TRUMOF-1 forms as a metastable intermediate that subsequently transforms into an ordered product with triclinic crystal symmetry. We determine the structure of this ordered phase, which we call msw-TRUMOF-1, and show that it is related to TRUMOF-1 through topotactic reorganization of linker occupancies. Our results imply that the connectivity of TRUMOF-1 can be reorganized, as required for data storage and manipulation applications.
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Sep 2024
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I12-JEEP: Joint Engineering, Environmental and Processing
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Jiaxu
Zuo
,
Kutsi
Akcicek
,
Shivansh
Nauriyal
,
Barrie
Dams
,
Stefan
Michalik
,
Thomas
Zillhardt
,
Martin
Ansell
,
Richard
Ball
,
Genoveva
Burca
,
Brian
Sheil
,
James
Marrow
,
Sinan
Acikgoz
Open Access
Abstract: Fibrous plaster (FP) ceilings, prevalent in late 19th- and early 20th-century UK theatres, are suspended using ‘wads’. Wads are hangers made of Plaster of Paris, reinforced with twisted woven jute fabric. Several recent collapses in historic fibrous plaster ceilings have been attributed to tensile failures in wads. To understand the failure mechanisms involved, tensile tests were performed on laboratory-produced wad-like samples at the I12 beamline of the UK Diamond Light Source. The tested samples were designed with a dog bone shape and mounted with clevis-grips at each end, to ensure controlled failures along the gauge length. The beamline offered the opportunity to conduct simultaneous synchrotron X-ray computed tomography (sCT) and diffraction measurements during loading, enabling the monitoring of internal crack formation and strain propagation at the microstructural scale. Simultaneously, acoustic emission (AE) and digital image correlation (DIC) measurements were conducted. Preliminary results from these datasets are discussed in this paper. The datasets will provide useful information to validate the ongoing development of algorithms which can categorise the internal failure mechanisms and damage state of wads using only AE signals.
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Sep 2024
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I12-JEEP: Joint Engineering, Environmental and Processing
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J. F. S.
Markanday
,
N.
D’souza
,
N. L.
Church
,
J. R.
Miller
,
J. J. C.
Pitchforth
,
L. D.
Connor
,
S.
Michalik
,
B.
Roebuck
,
N. G.
Jones
,
K. A.
Christofidou
,
H. J.
Stone
Diamond Proposal Number(s):
[33375]
Abstract: Factors affecting strain-age cracking (SAC) have been quantitatively assessed in a range of Ni-base superalloys with differing γ′ contents. Differences in the amount of γ′ present in the as-built condition of HA282, STAL 15DE, CM247LC, and IN713LC are highlighted. In the as-built condition, γ′ are absent in HA282, but appear as nano-clusters in IN713LC. On heating, γ′ precipitates coherently in the γ phase, increasing the yield strength. The kinetics of precipitation are dependent on the heating rate and precipitation terminates at different temperatures in different alloys. The propensity to SAC is assessed via volume changes accompanying precipitation, increase in elastic modulus accompanying γ′ precipitation, and a loss in ductility/grain boundary cohesive strength with increasing temperature. A marked feature of additively built microstructures is the dramatically low grain boundary cohesive strength at ~800 °C, which is related to the segregation within the terminal liquid film at the grain boundary. The most important factor contributing to SAC is the lack of ductility and reduced grain boundary cohesive strength.
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Aug 2024
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I12-JEEP: Joint Engineering, Environmental and Processing
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Kai
Zhang
,
Tim
Wigger
,
Rosa
Pineda
,
Simon A.
Hunt
,
Ben
Thomas
,
Thomas
Kwok
,
David
Dye
,
Gorka
Plata
,
Jokin
Lozares
,
Inaki
Hurtado
,
Stefan
Michalik
,
Michael
Preuss
,
Peter D.
Lee
,
Mohammed A.
Azeem
Diamond Proposal Number(s):
[23749]
Abstract: Microstructure evolution during high-strain rate and high-temperature thermo-mechanical processing of a 44MnSiV6 microalloyed steel is investigated using in situ synchrotron high-energy powder X-ray diffraction. The conditions selected replicate a newly developed near solidus high-strain rate process designed for reducing raw material use during the hot processing of steels. High temperatures (exceeding 1300 °C) and high strain rate
= 9 s-1 processing regimes are explored. The lattice strains and dislocation activity estimated from diffraction observations reveal that the microstructure evolution is primarily driven by dynamic recrystallisation. A steady-state stress regime is observed during deformation, which develops due to intermittent and competing work hardening and recovery processes. The texture evolution during the heating, tension, shear deformation and cooling stages is systematically investigated. The direct observation of phase evolution at high-temperature and high-strain rate deformation enables a comprehensive understanding of new manufacturing processes and provides deep insights for the development of constitutive models for face-centred cubic alloys.
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Aug 2024
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I11-High Resolution Powder Diffraction
I12-JEEP: Joint Engineering, Environmental and Processing
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Kay
Song
,
Guanze
He
,
Abdallah
Reza
,
Tamas
Ungar
,
Phani
Karamched
,
David
Yang
,
Ivan
Tolkachev
,
Kenichiro
Mizohata
,
Stephen P.
Thompson
,
Eamonn T.
Connolly
,
Robert C.
Atwood
,
Stefan
Michalik
,
David E. J.
Armstrong
,
Felix
Hofmann
Diamond Proposal Number(s):
[28444, 32094]
Open Access
Abstract: Severe plastic deformation changes the microstructure and properties of steels, which may be favourable for their use in structural components of nuclear reactors. In this study, high-pressure torsion (HPT) was used to refine the grain structure of Eurofer-97, a ferritic/martensitic steel. Electron microscopy and X-ray diffraction were used to characterise the microstructural changes. Following HPT at room temperature to a maximum shear strain of 230, the average grain size reduced by a factor of ~30, with a marked increase in high-angle grain boundaries. Dislocation density also increased by more than one order of magnitude. The thermal stability of the deformed material was investigated via in-situ annealing during synchrotron X-ray diffraction. This revealed substantial recovery between 450 K – 800 K. Irradiation with 20 MeV Fe-ions to ~0.1 dpa caused a 20% reduction in dislocation density compared to the as-deformed material. However, HPT deformation prior to irradiation only had a minor effect in mitigating the irradiation-induced reductions in thermal diffusivity and surface acoustic wave velocity of the material. Microstructural and material property changes are dominated by deformation compared to irradiation. In light of this, the benefits of using HPT to improve the irradiation resistance of Eurofer-97 are limited. These results provide a multi-faceted view of the changes in ferritic/martensitic steels due to severe plastic deformation, and how these changes can be used to alter material properties.
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Jul 2024
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