The temporally and spatially resolved tracking of lithium intercalation and electrode degradation processes are crucial for detecting and understanding performance losses during the operation of ...lithium-batteries. Here, high-throughput X-ray computed tomography has enabled the identification of mechanical degradation processes in a commercial Li/MnO
primary battery and the indirect tracking of lithium diffusion; furthermore, complementary neutron computed tomography has identified the direct lithium diffusion process and the electrode wetting by the electrolyte. Virtual electrode unrolling techniques provide a deeper view inside the electrode layers and are used to detect minor fluctuations which are difficult to observe using conventional three dimensional rendering tools. Moreover, the 'unrolling' provides a platform for correlating multi-modal image data which is expected to find wider application in battery science and engineering to study diverse effects e.g. electrode degradation or lithium diffusion blocking during battery cycling.
In recent years, low-temperature polymer electrolyte fuel cells have become an increasingly important pillar in a zero-carbon strategy for curbing climate change, with their potential to power ...multiscale stationary and mobile applications. The performance improvement is a particular focus of research and engineering roadmaps, with water management being one of the major areas of interest for development. Appropriate characterisation tools for mapping the evolution, motion and removal of water are of high importance to tackle shortcomings. This article demonstrates the development of a 4D high-speed neutron imaging technique, which enables a quantitative analysis of the local water evolution. 4D visualisation allows the time-resolved studies of droplet formation in the flow fields and water quantification in various cell parts. Performance parameters for water management are identified that offer a method of cell classification, which will, in turn, support computer modelling and the engineering of next-generation flow field designs.
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•Anosteocytic bone material is more water permeable than osteocytic bone material.•In osteocytic zebrafish bone, water flow appears to be confined to the lacunar-canalicular ...network.•Anosteocytic medaka bone is water permeable and containes far less proteoglycans.•3D correlation of neutron and X-ray tomographies with micron resolution reveals water diffusion across the bone matrix.
Vertebrate bones are made of a nanocomposite consisting of water, mineral and organics. Water helps bone material withstand mechanical stress and participates in sensation of external loads. Water diffusion across vertebrae of medaka (bone material lacking osteocytes) and zebrafish (bone material containing osteocytes) was compared using neutron tomography. Samples were measured both wet and following immersion in deuterated-water (D2O). By quantifying H+ exchange and mutual alignment with X-ray µCT scans, the amount of water expelled from complete vertebra was determined. The findings revealed that anosteocytic bone material is almost twice as amenable to D2O diffusion and H2O exchange, and that unexpectedly, far more water is retained in osteocytic zebrafish bone. Diffusion in osteocytic bones (only 33 % – 39 % water expelled) is therefore restricted as compared to anosteocytic bone (∼ 60 % of water expelled), presumably because water flow is confined to the lacunar-canalicular network (LCN) open-pore system. Histology and Raman spectroscopy showed that anosteocytic bone contains less proteoglycans than osteocytic bone. These findings identify a previously unknown functional difference between the two bone materials. Therefore, this study proposes that osteocytic bone retains water, aided by non-collagenous proteins, which contribute to its poroelastic mechano-transduction of water flow confined inside the LCN porosity.
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•7017 Al alloy admixed with 3 wt% Zr, 0.5 wt% TiC created fully dense samples (<0.2 % porosity) processed via PBF-LB process.•Microstructure shows strengthening as a combination of ...precipitation hardening and grain size strengthening.•In-situ combined with ex-situ tensile testing confirm Zr inclusions improve ductility by deflecting crack growth.
This study addressed a 7017 Al-alloy tailored for powder bed fusion – laser beam (PBF-LB) process. The alloy was prepared by mixing 3 wt% Zr and 0.5 wt% TiC powder to standard pre-alloyed 7017 grade aluminium powder. This made printing of the alloys possible avoiding solidification cracking in the bulk and achieving high relative density (99.8 %). Such advanced alloys have significantly higher Young’s modulus (>80 GPa) than conventional Al-alloys (70–75 GPa), thus making them attractive for applications requiring high stiffness. The resulting microstructure in as-printed condition was rich in particles originating from admixed powders and primary precipitates/inclusions originating from the PBF-LB process. After performing a T6-like heat treatment designed for the PBF-LB process, the microstructure changed: Zr-nanoparticles and Fe- or Mg/Zn- containing precipitates formed thus providing 75 % increase in yield strength (from 254 MPa to 444 MPa) at the cost of decreasing ductility (∼20 % to ∼9 %). In-situ tensile testing combined with SXCT, and ex-situ tensile testing combined with fracture analysis confirmed that the fracture initiation in both conditions is highly dependent on defects originated during printing. However, cracks are deflected from decohesion around Zr-containing inclusions/precipitates embedded in the Al-matrix. This deflection is seen to improve the ductility of the material.
A systematic study has been carried out to investigate the neutron transmission signal as a function of sample temperature. In particular, the experimentally determined wavelength‐dependent neutron ...attenuation spectra for a martensitic steel at temperatures ranging from 21 to 700°C are compared with simulated data. A theoretical description that includes the Debye–Waller factor in order to describe the temperature influence on the neutron cross sections was implemented in the nxsPlotter software and used for the simulations. The analysis of the attenuation coefficients at varying temperatures shows that the missing contributions due to elastic and inelastic scattering can be clearly distinguished: while the elastically scattered intensities decrease with higher temperatures, the inelastically scattered intensities increase, and the two can be separated from each other by analysing unique sharp features in the form of Bragg edges. This study presents the first systematic approach to quantify this effect and can serve as a basis , for example, to correct measurements taken during in situ heat treatments, in many cases being a prerequisite for obtaining quantifiable results.
A systematic study was carried out to investigate the neutron transmission signal as a function of sample temperature. In particular, the experimentally determined wavelength‐dependent neutron attenuation spectra for a martensitic steel at temperatures ranging from 21 to 700°C are compared with simulated data.
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•Neutron imaging reveals phase transformation behavior of metastable austenitic stainless steels under plastic deformation.•3D mapping of phase distributions in polycrystalline ...materials non-destructively.•In-situ investigation of the effect of a geometrical factor on phase transformation in a rectangular TRIP steel sample under torsion load.•New non-destructive spectroscopic technique based on neutron diffraction contrast is eligible for study of material phase.
Metastable austenitic stainless steel (304L) samples with a rectangular cross-section were plastically deformed in torsion during which they experienced multiaxial stresses that led to a complex martensitic phase distribution owing to the transformation induced plasticity effect. A three-dimensional characterization of the phase distributions in these cm-sized samples was carried out by wavelength-selective neutron tomography. It was found that quantitatively correct results are obtained as long as the samples do not exhibit any considerable preferential grain orientation. Optical microscopy, electron backscatter diffraction, and finite element modeling were used to verify and explain the results obtained by neutron tomography. Altogether, neutron tomography was shown to extend the range of microstructure characterization methods towards the meso- and macroscale.
Two proof-of-concept batteries were designed and prepared for X-ray microtomography and radiography characterizations to investigate the degradation mechanisms of silicon (Si) based half cells during ...the first cycle. It is highlighted here for the first time that, apart from the significant volume expansion-induced pulverization, the electrochemical “deactivation” mechanism contributes significantly to the capacity loss during the first charge process. In addition, the unexpected electrochemically inactive Si particles are also believed to substantially decrease the energy density due to the inefficient utilization of loaded active material. These unexpected findings, which cannot be deduced from macroscopic electrochemical characterizations, expand the inherent explanations for performance deterioration of Si-anode material based lithium ion batteries (LIBs) and emphasize the vital value of microscopic techniques in revealing the correlation between macroscopic electrode structure and the overall electrochemical performance.
•Two prototypes of lithium ion batteries were manufactured for micro X-ray imaging.•The first cycle of Si based half cells is investigated.•Volume change of electrochemically active Si particles are shown in 3D and 2D.•Electrochemical deactivation process is proved from the un-shifted X-ray attenuation.•Some of Si particles never experience the battery level electrochemical de/lithiation.
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