We report the results from the first 5D tomographic diffraction imaging experiment of a complex Ni-Pd/CeO
-ZrO
/Al
O
catalyst used for methane reforming. This five-dimensional (three spatial, one ...scattering and one dimension to denote time/imposed state) approach enabled us to track the chemical evolution of many particles across the catalyst bed and relate these changes to the gas environment that the particles experience. Rietveld analysis of some 2 × 10
diffraction patterns allowed us to extract heterogeneities in the catalyst from the Å to the nm and to the μm scale (3D maps corresponding to unit cell lattice parameters, crystallite sizes and phase distribution maps respectively) under different chemical environments. We are able to capture the evolution of the Ni-containing species and gain a more complete insight into the multiple roles of the CeO
-ZrO
promoters and the reasons behind the partial deactivation of the catalyst during partial oxidation of methane.
Vitrification from physical vapor deposition is known to be an efficient way for tuning the kinetic and thermodynamic stability of glasses and significantly improve their properties. There is a ...general consensus that preparing stable glasses requires the use of high substrate temperatures close to the glass transition one, T
. Here, we challenge this empirical rule by showing the formation of Zr-based ultrastable metallic glasses (MGs) at room temperature, i.e., with a substrate temperature of only 0.43T
. By carefully controlling the deposition rate, we can improve the stability of the obtained glasses to higher values. In contrast to conventional quenched glasses, the ultrastable MGs exhibit a large increase of T
of ∼60 K, stronger resistance against crystallization, and more homogeneous structure with less order at longer distances. Our study circumvents the limitation of substrate temperature for developing ultrastable glasses, and provides deeper insight into glasses stability and their surface dynamics.
Electric vehicles demand high charge and discharge rates creating potentially dangerous temperature rises. Lithium-ion cells are sealed during their manufacture, making internal temperatures ...challenging to probe
. Tracking current collector expansion using X-ray diffraction (XRD) permits non-destructive internal temperature measurements
; however, cylindrical cells are known to experience complex internal strain
. Here, we characterize the state of charge, mechanical strain and temperature within lithium-ion 18650 cells operated at high rates (above 3C) by means of two advanced synchrotron XRD methods: first, as entire cross-sectional temperature maps during open-circuit cooling and second, single-point temperatures during charge-discharge cycling. We observed that a 20-minute discharge on an energy-optimized cell (3.5 Ah) resulted in internal temperatures above 70 °C, whereas a faster 12-minute discharge on a power-optimized cell (1.5 Ah) resulted in substantially lower temperatures (below 50 °C). However, when comparing the two cells under the same electrical current, the peak temperatures were similar, for example, a 6 A discharge resulted in 40 °C peak temperatures for both cell types. We observe that the operando temperature rise is due to heat accumulation, strongly influenced by the charging protocol, for example, constant current and/or constant voltage; mechanisms that worsen with cycling because degradation increases the cell resistance. Design mitigations for temperature-related battery issues should now be explored using this new methodology to provide opportunities for improved thermal management during high-rate electric vehicle applications.
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GEOZS, IJS, IMTLJ, KISLJ, NLZOH, NUK, OILJ, PNG, SAZU, SBCE, SBMB, UL, UM, UPUK, ZAGLJ
In situ tensile tests have been carried out on a high-strength, dual-phase steel. These experiments show that it is possible to follow and quantify the evolution of damage nondestructively and in ...three dimensions in this type of material. The measurements were analyzed in terms of density, size, aspect ratio of the cavities but also of the local deformation and the stress triaxiality in the sample. It was found that damage initiation is progressive with the applied tensile strain and that the initiation of new small cavities reduces the average diameter while the growth of the previously created ones increases the average diameter. This information was used to develop a new model for void growth based on the classical Rice and Tracey approach. This simple approach was modified to account for progressive damage initiation. The results of the proposed model are in good agreement with the measurements.
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GEOZS, IJS, IMTLJ, KILJ, KISLJ, NUK, OILJ, PNG, SAZU, SBCE, SBJE, UL, UM, UPCLJ, UPUK
The freezing of colloidal suspensions is encountered in many natural and engineering processes such as the freezing of soils, food engineering and cryobiology. It can also be used as a bio-inspired, ...versatile and environmentally friendly processing route for porous materials and composites. Yet, it is still a puzzling phenomenon with many unexplained features, owing to the complexity of the system and the space and time scales at which the process should be investigated. This study demonstrates the interest in fast X-ray computed tomography for providing time-lapse, three-dimensional, in situ imaging of ice crystal growth in a colloidal silica suspension. The experimental measurements show that the local increase in colloid concentration does not affect the growth kinetics of the crystals until the colloidal particles become closely packed. For particles much smaller than ice crystals, the concentrated colloidal suspension is equivalent to a simple liquid phase with higher viscosity and a freezing point determined by the concentration of colloidal particles.
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GEOZS, IJS, IMTLJ, KILJ, KISLJ, NUK, OILJ, PNG, SAZU, SBCE, SBJE, UL, UM, UPCLJ, UPUK
Tungsten-fibre-reinforced tungsten composites (Wf/W) are supposed to enable enhanced toughness owing to extrinsic energy dissipation mechanisms such as interface debonding and plastic deformation of ...fibre. In particular, the latter is an effective source of toughening, since ductile tungsten fibres can absorb a considerable amount of plastic work. For a precise evaluation of the toughening capability, the energy dissipation mechanisms need to be analysed in detail. To this end, single-fibre tungsten composite specimens are fabricated and the stress–strain behaviour of the tungsten fibre bridging a matrix crack is measured by means of in situ high-energy synchrotron microtomography during a uniaxial tensile test. Despite the high X-ray attenuation in tungsten, a sufficiently high resolution is achieved and clear images of crack extension and deformation are obtained. The amount of absorbed energy due to plastic deformation of the tungsten fibre is determined and compared with values obtained conventionally from single-fibre tensile tests.
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GEOZS, IJS, IMTLJ, KILJ, KISLJ, NUK, OILJ, PNG, SAZU, SBCE, SBJE, UL, UM, UPCLJ, UPUK
When a granular material such as sand is mixed with a certain amount of liquid, the surface tension of the latter bestows considerable stiffness to the material, which enables, for example, sand ...castles to be sculpted. The geometry of the liquid interface within the granular pile is of extraordinary complexity and strongly varies with the liquid content. Surprisingly, the mechanical properties of the pile are largely independent of the amount of liquid over a wide range. We resolve this puzzle with the help of X-ray microtomography, showing that the remarkable insensitivity of the mechanical properties to the liquid content is due to the particular organization of the liquid in the pile into open structures. For spherical grains, a simple geometric rule is established, which relates the macroscopic properties to the internal liquid morphologies. We present evidence that this concept is also valid for systems with non-spherical grains. Hence, our results provide new insight towards understanding the complex physics of a large variety of wet granular systems including land slides, as well as mixing and agglomeration problems.
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IJS, IZUM, KILJ, KISLJ, NUK, PILJ, PNG, SAZU, UL, UM, UPUK
When a granular material such as sand is mixed with a certain amount of liquid, the surface tension of the latter bestows considerable stiffness to the material, which enables, for example, sand ...castles to be sculpted. The geometry of the liquid interface within the granular pile is of extraordinary complexity and strongly varies with the liquid content. Surprisingly, the mechanical properties of the pile are largely independent of the amount of liquid over a wide range. We resolve this puzzle with the help of X-ray microtomography, showing that the remarkable insensitivity of the mechanical properties to the liquid content is due to the particular organization of the liquid in the pile into open structures. For spherical grains, a simple geometric rule is established, which relates the macroscopic properties to the internal liquid morphologies. We present evidence that this concept is also valid for systems with non-spherical grains. Hence, our results provide new insight towards understanding the complex physics of a large variety of wet granular systems including land slides, as well as mixing and agglomeration problems.
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IJS, IZUM, KILJ, KISLJ, NUK, PILJ, PNG, SAZU, UL, UM, UPUK
The near equi-atomic intermetallic Ni Ti alloy Nitinol is used for medical implants, notably in self-expanding stent grafts and heart valve frames, which are subjected to several hundred million load ...cycles in service. Increasing the testing frequency to the ultrasonic range would drastically shorten the testing times and make the very-high cycle regime experimentally accessible. Such tests are, however, only meaningful if the material response at ultrasonic frequency is identical to that observed in conventional fatigue tests. A novel fatigue testing setup where superelastic Nitinol dog bone specimens are loaded at ultrasonic cycling frequency is presented. Loading conditions resemble in vivo loading (i.e., repeated cyclic loading with relatively small strain amplitudes, specimens in a pre-strained multi-phase state). Strains and phase transformations during ultrasonic frequency cycling are quantitatively measured in an X-ray diffraction (XRD) synchrotron experiment and compared to the material response at low frequency. The XRD experiment confirms that forward and reverse stress-induced phase transformation from austenite to martensite via the intermediate R-phase occurs during low frequency (0.1 Hz, strain rate
ε
˙
≈
10
−3
s
−1
) and ultrasonic frequency (20 kHz,
ε
˙
≈
10
2
s
−1
) cycling. Since the same deformation mechanisms are active at low and ultrasonic frequency, these findings imply a general applicability of the ultrasonic fatigue testing technique to Nitinol.
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EMUNI, FIS, FZAB, GEOZS, GIS, IJS, IMTLJ, KILJ, KISLJ, MFDPS, NLZOH, NUK, OBVAL, OILJ, PNG, SAZU, SBCE, SBJE, SBMB, SBNM, UKNU, UL, UM, UPUK, VKSCE, ZAGLJ
Accelerator magnets that can reach magnetic fields well beyond the Nb-Ti performance limits are presently being built and developed, using Nb3Sn superconductors. This technology requires reaction ...heat treatment (RHT) of the magnet coils, during which Nb3Sn is formed from its ductile precursor materials (a "wind and react" approach). The Nb3Sn microstructure and microchemistry are strongly influenced by the conductor fabrication route, and by the phase changes during RHT. By combining in situ differential scanning calorimetry, high energy synchrotron x-ray diffraction, and micro-tomography experiments, we have acquired a unique data set that describes in great detail the phase and microstructure changes that take place during the processing of restacked rod process (RRP), powder-in-tube (PIT), and internal tin (IT) Nb3Sn wires. At temperatures below 450 °C the phase evolutions in the three wire types are similar, with respectively solid state interdiffusion of Cu and Sn, Cu6Sn5 formation, and Cu6Sn5 peritectic transformation. Distinct differences in phase evolutions in the wires are found when temperatures exceed 450 °C. The volume changes of the conductor during RHT are a difficulty in the production of Nb3Sn accelerator magnets. We compare the wire diameter changes measured in situ by dilatometry with the phase and void volume evolution of the three types of Nb3Sn wire. Unlike the Nb3Sn wire length changes, the wire diameter evolution is characteristic for each Nb3Sn wire type. The strongest volume increase, of about 5%, is observed in the RRP wire, where the main diameter increase occurs above 600 °C upon Nb3Sn formation.
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