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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.
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Sep 2022
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I12-JEEP: Joint Engineering, Environmental and Processing
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Diamond Proposal Number(s):
[26376]
Open Access
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.
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Jul 2022
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B16-Test Beamline
E01-JEM ARM 200CF
I12-JEEP: Joint Engineering, Environmental and Processing
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Zifan
Wang
,
Jingwei
Chen
,
Radim
Kocich
,
Samuel
Tardif
,
Igor P.
Dolbnya
,
Lenka
Kunčická
,
Jean-Sébastien
Micha
,
Konstantinos
Liogas
,
Oxana
Magdysyuk
,
Ivo
Szurman
,
Alexander M.
Korsunsky
Diamond Proposal Number(s):
[25467, 28397, 28418]
Open Access
Abstract: To explore an effective route of customizing the superelasticity (SE) of NiTi shape memory alloys via modifying the grain structure, binary Ni55Ti45 (wt) alloys were fabricated in as-cast, hot swaged, and hot-rolled conditions, presenting contrasting grain sizes and grain boundary types. In situ synchrotron X-ray Laue microdiffraction and in situ synchrotron X-ray powder diffraction techniques were employed to unravel the underlying grain structure mechanisms that cause the diversity of SE performance among the three materials. The evolution of lattice rotation, strain field, and phase transformation has been revealed at the micro- and mesoscale, and the effect of grain structure on SE performance has been quantified. It was found that (i) the Ni4Ti3 and NiTi2 precipitates are similar among the three materials in terms of morphology, size, and orientation distribution; (ii) phase transformation happens preferentially near high-angle grain boundary (HAGB) yet randomly in low-angle grain boundary (LAGB) structures; (iii) the smaller the grain size, the higher the phase transformation nucleation kinetics, and the lower the propagation kinetics; (iv) stress concentration happens near HAGBs, while no obvious stress concentration can be observed in the LAGB grain structure during loading; (v) the statistical distribution of strain in the three materials becomes asymmetric during loading; (vi) three grain lattice rotation modes are identified and termed for the first time, namely, multi-extension rotation, rigid rotation, and nondispersive rotation; and (vii) the texture evolution of B2 austenite and B19′ martensite is not strongly dependent on the grain structure.
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Jun 2022
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I12-JEEP: Joint Engineering, Environmental and Processing
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Diamond Proposal Number(s):
[25467]
Abstract: Tracking texture evolution during in situ loading is critical to understand and simulate the dynamic behaviour of microstructure in polycrystalline materials, yet conventional texture quantification methods are sometimes restricted due to various factors, such as acquisition time, sample environment and complex setup. To address this, a novel approach to extract texture information from single shot Time-Of-Flight neutron diffraction pattern has been developed. Another texture analysis approach based on single shot synchrotron X-ray diffraction has also been demonstrated. The effectiveness of two methods is assessed for polycrystalline Nickel-based superalloy polycrystalline samples possessing different textures. Both methods feature a moderate acquisition time of ~10 min and 30 s respectively, as well as a simplified setup which allows adding complex sample environments and the use of additional equipment. Comparison with the referential EBSD texture suggests that both approaches achieve a satisfactory match, though some details of the complex contour profiles in inverse pole figures may be missing. Besides that, a novel metric has been proposed to quantify the matching quality of pole figures. By employing the EPSC modelling approach, it is shown that the texture deviation due to the technique chosen for its evaluation exerts a subtle influence on th macro- and mesoscale simulation results, highlighting the significance of this approach for underpinning robust computational modelling.
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Apr 2022
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I12-JEEP: Joint Engineering, Environmental and Processing
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Chun
Huang
,
Matthew
Wilson
,
Kosuke
Suzuki
,
Enzo
Liotti
,
Thomas
Connolley
,
Oxana
Magdysyuk
,
Stephen
Collins
,
Frederic
Van Assche
,
Matthieu N
Boone
,
Matthew C.
Veale
,
Andrew
Lui
,
Rhian-Mair
Wheater
,
Chu Lun Alex
Leung
Diamond Proposal Number(s):
[23400]
Open Access
Abstract: The performance of Li+ ion batteries (LIBs) is hindered by steep Li+ ion concentration gradients in the electrodes. Although thick electrodes (≥300 µm) have the potential for reducing the proportion of inactive components inside LIBs and increasing battery energy density, the Li+ ion concentration gradient problem is exacerbated. Most understanding of Li+ ion diffusion in the electrodes is based on computational modeling because of the low atomic number (Z) of Li. There are few experimental methods to visualize Li+ ion concentration distribution of the electrode within a battery of typical configurations, for example, coin cells with stainless steel casing. Here, for the first time, an interrupted in situ correlative imaging technique is developed, combining novel, full-field X-ray Compton scattering imaging with X-ray computed tomography that allows 3D pixel-by-pixel mapping of both Li+ stoichiometry and electrode microstructure of a LiNi0.8Mn0.1Co0.1O2 cathode to correlate the chemical and physical properties of the electrode inside a working coin cell battery. An electrode microstructure containing vertically oriented pore arrays and a density gradient is fabricated. It is shown how the designed electrode microstructure improves Li+ ion diffusivity, homogenizes Li+ ion concentration through the ultra-thick electrode (1 mm), and improves utilization of electrode active materials.
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Apr 2022
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I12-JEEP: Joint Engineering, Environmental and Processing
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Lorna
Sinclair
,
Yunhui
Chen
,
Samuel J.
Clark
,
Sebastian
Marussi
,
Saurabh
Shah
,
Oxana
Magdysyuk
,
Robert
Atwood
,
Gavin J.
Baxter
,
Martyn
Jones
,
Graham
Mccartney
,
Chu Lun Alex
Leung
,
Peter D.
Lee
Diamond Proposal Number(s):
[20096]
Open Access
Abstract: During directed energy deposition (DED) additive manufacturing, powder agglomeration and sintering can occur outside of the melt pool when using titanium alloy powders. Using in situ synchrotron radiography we investigate the mechanisms by which sintering of Ti6242 powder occurs around the pool, performing a parametric study to determine the influence of laser power and stage traverse speed on sinter build-up. The results reveal that detrimental sinter can be reduced using a high laser power or increased stage traverse speed, although the latter also reduces deposition layer thickness. The mechanism of sinter formation during DED was determined to be in-flight heating of the powder particles in the laser beam. Calculations of particle heating under the processing conditions explored in this study confirm that powder particles can reasonably exceed 700 °C, the threshold for Ti surface oxide dissolution, and thus the powder is prone to sintering if not incorporated into the melt pool. The build-up of sinter powder layer on deposit surfaces led to lack of fusion pores. To mitigate sinter formation and its detrimental effects on DED component quality, it is essential that the powder delivery spot area is smaller than the melt pool, ensuring most powder lands in the melt pool.
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Apr 2022
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I12-JEEP: Joint Engineering, Environmental and Processing
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Diamond Proposal Number(s):
[19216]
Open Access
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.
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Mar 2022
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I12-JEEP: Joint Engineering, Environmental and Processing
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Diamond Proposal Number(s):
[18720, 21819]
Abstract: Flufenamic acid (FFA) is a highly polymorphic drug molecule with nine crystal structures reported in the Cambridge Structural Database. This study explores the use of synchrotron X-ray powder diffraction combined with differential scanning calorimetry to study crystallization and polymorphic phase transitions upon heating FFA–polymer amorphous solid dispersions (ASDs). Ethyl cellulose (EC, 4 cp) and hydroxypropylmethylcellulose (HPMC) grades with different viscosities and substitution patterns were used to prepare dispersions with FFA at 5:1, 2:1, 1:1, and 1:5 w/w drug/polymer ratios by quench cooling. We employed a 6 cp HPMC 2910 material and two HPMC 2208 samples at 4000 and 100 000 cp. Hyphenated X-ray diffraction (XRD)–differential scanning calorimetry (DSC) studies show that the 6 and 100 000 cp HPMCs and 4 cp EC polymers can stabilize FFA form IV by inhibiting the transition to form I during heating. It appears that the polymers stabilize FFA in both amorphous and metastable forms via a combination of intermolecular interactions and viscosity effects. Increasing the polymer content of the ASD also inhibits polymorphic transitions, with drug/polymer ratios of 1:5 w/w resulting in FFA remaining amorphous during heating. The comparison of FFA ASDs prepared with different samples of HPMCs and ECs suggests that the chemical substitution of the polymer (HPMC 2208 has 19–24% methoxy groups and 4–12% hydroxypropyl groups, while HPMC 2910 has 28–30% methoxy groups and 7–12% hydroxypropyl groups) plays a more significant role in directing polymorphic transitions than the viscosity. A previously unreported polymorph of FFA was also noted during heating but its structure could not be determined.
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Mar 2022
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I12-JEEP: Joint Engineering, Environmental and Processing
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William Q.
Walker
,
Kylie
Cooper
,
Peter
Hughes
,
Ian
Doemling
,
Mina
Akhnoukh
,
Sydney
Taylor
,
Jacob
Darst
,
Julia
Billman
,
Matthew
Sharp
,
David
Petrushenko
,
Rhodri
Owen
,
Martin
Pham
,
Thomas
Heenan
,
Alexander
Rack
,
Oxana
Magdysyuk
,
Thomas
Connolley
,
Dan
Brett
,
Paul
Shearing
,
Donal
Finegan
,
Eric
Darcy
Diamond Proposal Number(s):
[24112, 20903, 17641]
Abstract: Consideration of thermal runaway heat output variability is paramount for the development of safe lithium-ion battery assemblies. This study utilizes data gathered from fractional thermal runaway calorimetry (FTRC) experiments to conduct a comparative analysis of thermal runaway heat output for three cell formats (18650, 21700, and 33600) as a function of trigger method (heaters, internal short-circuiting device, and nail penetration). The analysis is based on comparisons for the calculated total energy yield, fractional energy yield, heat rate, and heat flux. This study reveals that nail penetration tends to result in higher thermal runaway heat output for larger cells (21700 & 33600); these experiments also tended to result in higher fractions of the total energy being released through the cell body. The smaller cells (18650) did not appear to have significant variation in heat output as a function of trigger method. This finding suggests that, for this cell type, worst-case scenario heat output could be achievable in assembly level testing regardless of the utilized trigger method. This study also demonstrates successful translation of FTRC results, as recorded in the Battery Failure Databank, into meaningful analysis that breaks down the influence of specific conditions on thermal runaway heat output.
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Mar 2022
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I12-JEEP: Joint Engineering, Environmental and Processing
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Evgeny A.
Gorbachev
,
Lev A.
Trusov
,
Liudmila N.
Alyabyeva
,
Ilya V.
Roslyakov
,
Vasily A.
Lebedev
,
Ekaterina S.
Kozlyakova
,
Oxana V.
Magdysyuk
,
Alexey V.
Sobolev
,
Iana S.
Glazkova
,
Sergey A.
Beloshapkin
,
Boris P.
Gorshunov
,
Pavel E.
Kazin
Abstract: Herein, we demonstrate for the first time compact ferrite ceramics with giant coercivity. The materials are manufactured via sintering single-domain Sr0.67Ca0.33Fe8Al4O19 particles synthesized by a citrate-nitrate auto-combustion method. The obtained ceramics show coercivities up to 22.5 kOe and natural ferromagnetic resonance frequencies (NFMR) in a sub-THz range of 160–282 GHz. At a maximum density of 95%, the sample displays coercivity of 18.5 kOe, which is the highest value among dense ferrite materials reported so far. In addition, we report an unusual blueshift of the NFMR frequency from 160 to 200 GHz, which occurs during material sintering.
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Jan 2022
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