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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.

Neutron imaging was used to visualize and study invasion phenomena in fibrous porous transport layers (PTLs) of titanium felt under different flow conditions of gas and liquid phase. The experiments were realized with flow cells that contained a gas and a liquid flow channel separated by PTLs with different thicknesses and pore size distributions. The invasion can be characterized by counter‐current flow of water and air with joint imbibition and drainage processes. The dynamics were visualized with neutron radiography with a local resolution of 6.5 µm and a temporal resolution of 0.1 s. Individual static gas‐liquid distributions were additionally studied by neutron tomography, with a local resolution of 22 µm and an exposure time of 1.5 s per image (projections: 800/360°). It is shown and discussed that the invasion occurred in continuously repeated imbibition/drainage cycles with frequencies depending on the flow conditions and the PTL structure as well. The change of the PTL saturation with air or water appeared almost independent from the specific PTL structure and the breakthrough of the gas phase occurred at almost constant positions.

The Oak Ridge National Laboratory is planning to build the Second Target Station (STS) at the Spallation Neutron Source (SNS). STS will host a suite of novel instruments that complement the First Target Station’s beamline capabilities by offering an increased flux for cold neutrons and a broader wavelength bandwidth. A novel neutron imaging beamline, named the Complex, Unique, and Powerful Imaging Instrument for Dynamics (CUPI2D), is among the first eight instruments that will be commissioned at STS as part of the construction project. CUPI2D is designed for a broad range of neutron imaging scientific applications, such as energy storage and conversion (batteries and fuel cells), materials science and engineering (additive manufacturing, superalloys, and archaeometry), nuclear materials (novel cladding materials, nuclear fuel, and moderators), cementitious materials, biology/medical/dental applications (regenerative medicine and cancer), and life sciences (plant–soil interactions and nutrient dynamics). The innovation of this instrument lies in the utilization of a high flux of wavelength-separated cold neutrons to perform real time in situ neutron grating interferometry and Bragg edge imaging—with a wavelength resolution of δλ/λ ≈ 0.3%—simultaneously when required, across a broad range of length and time scales. This manuscript briefly describes the science enabled at CUPI2D based on its unique capabilities. The preliminary beamline performance, a design concept, and future development requirements are also presented.

Advanced batteries are critical to achieving net zero and are proposed within decarbonization strategies for transport and grid scale applications, alongside their ubiquitous application in consumer devices. Immense progress has been made in lithium battery technology in recent years, but significant challenges remain and new development strategies are required to improve performance, fully exploit power density capacities, utilize sustainable resources, and lower production costs. Suitable characterization techniques are crucial for understanding, inter alia, three dimensional 3D diffusion processes and formation of passivation layers or dendrites, which can lead to drastic capacity reduction and potentially to hazardous short circuiting. Studies of such phenomena typically utilize 2D or 3D imaging techniques, providing locally resolved information. 3D X ray imaging is a widely used standard method, while time lapse 4D tomography is increasingly required for understanding the processes and transformations in an operational battery. Neutron imaging overcomes some of the limitations of X ray tomography for battery studies. Notably, the high visibility of neutrons for light Z elements, in particular hydrogen and lithium, enables the direct observation of lithium diffusion, electrolyte consumption, and gas formation in lithium batteries. Neutron imaging as a non destructive analytical tool has been steadily growing in many disciplines as a result of improvements to neutron detectors and imaging facilities, providing increasingly higher spatial and temporal resolutions. Further, ongoing developments in diffraction imaging for mapping the structural and microstructural properties of battery components make the use of neutrons increasingly attractive. Here, we provide an overview of neutron imaging techniques, generally outlining advances and limitations for studies on batteries and reviewing imaging studies of lithium batteries. We conclude with an outlook on development methods in the field and discuss their potential and significance for future battery research

Purpose Microplastics have become a ubiquitous pollutant in marine, terrestrial and freshwater systems that seriously affects aquatic and terrestrial ecosystems. Common methods for analysing microplastic abundance in soil or sediments are based on destructive sampling or involve destructive sample processing. Thus, substantial information about local distribution of microplastics is inevitably lost. Methods Tomographic methods have been explored in our study as they can help to overcome this limitation because they allow the analysis of the sample structure while maintaining its integrity. However, this capability has not yet been exploited for detection of environmental microplastics. We present a bimodal 3D imaging approach capable to detect microplastics in soil or sediment cores non-destructively. Results In a first pilot study, we demonstrate the unique potential of neutrons to sense and localize microplastic particles in sandy sediment. The complementary application of X-rays allows mineral grains to be discriminated from microplastic particles. Additionally, it yields detailed information on the 3D surroundings of each microplastic particle, which supports its size and shape determination. Conclusion The procedure we developed is able to identify microplastic particles with diameters of approximately 1 mm in a sandy soil. It also allows characterisation of the shape of the microplastic particles as well as the microstructure of the soil and sediment sample as depositional background information. Transferring this approach to environmental samples presents the opportunity to gain insights of the exact distribution of microplastics as well as their past deposition, deterioration and translocation processes.

Purpose Root growth, respiration, water uptake as well as root exudation induce biogeochemical patterns in the rhizosphere that can change dynamically over time. Our aim is to develop a method that provides complementary information on 3D root system architecture and biogeochemical gradients around the roots needed for the quantitative description of rhizosphere processes. Methods We captured for the first time the root system architecture of maize plants grown in rectangular rhizotrons in 3D using neutron computed laminography (NCL). Simultaneously, we measured pH and oxygen concentration using fluorescent optodes and the 2D soil water distribution by means of neutron radiography. We co-registered the 3D laminography data with the 2D oxygen and pH maps to analyze the sensor signal as a function of the distance between the roots and the optode. Results The 3D root system architecture was successfully segmented from the laminographic data. We found that exudation of roots in up to 2 mm distance to the pH optode induced patterns of local acidification or alkalization. Over time, oxygen gradients in the rhizosphere emerged for roots up to a distance of 7.5 mm. Conclusion Neutron computed laminography allows for a three-dimensional investigation of root systems grown in laterally extended rhizotrons as the ones designed for 2D optode imaging studies. The 3D information on root position within the rhizotrons derived by NCL explained measured 2D oxygen and pH distribution. The presented new combination of 3D and 2D imaging methods facilitates systematical investigations of a wide range of dynamic processes in the rhizosphere.

Metal foam flow-fields have shown great potential in improving the uniformity of reactant distribution in polymer electrolyte fuel cells (PEFCs) by eliminating the ‘land/channel’ geometry of conventional designs. However, a detailed understanding of the water management in operational metal foam flow-field based PEFCs is limited. This study aims to provide the first clear evidence of how and where water is generated, accumulated and removed in the metal foam flow-field based PEFCs using in-operando neutron radiography, and correlate the water ‘maps’ with electrochemical performance and durability. Results show that the metal foam flow-field based PEFC has greater tolerance to dehydration at 1000 mA cm−2, exhibiting a ~50% increase in voltage, ~127% increase in total water mass and ~38% decrease in high frequency resistance (HFR) than serpentine flow-field design. Additionally, the metal foam flow-field promotes more uniform water distribution where the standard deviation of the liquid water thickness distribution across the entire cell active area is almost half that of the serpentine. These superior characteristics of metal foam flow-field result in greater than twice the maximum power density over serpentine flow-field. Results suggest that optimizing fuel cell operating condition and foam microstructure would partly mitigate flooding in the metal foam flow-field based PEFC.

A large and increasing number of scientific domains pushes for high neutron imaging resolution achieved in reasonable times. Here we present the principle, design and performance of a detector based on infinity corrected optics combined with a crystalline Gd3Ga5O12 : Eu scintillator, which provides an isotropic sub-4 µm true resolution. The exposure times are only of a few minutes per image. This is made possible also by the uniquely intense cold neutron flux available at the imaging beamline NeXT-Grenoble. These comparatively rapid acquisitions are compatible with multiple high quality tomographic acquisitions, opening new venues for in-operando testing, as briefly exemplified here.

While laser powder-bed fusion has overcome some of the design constraints of conventional manufacturing meth-ods, it requires careful selection of process parameters and scan strategies to obtain favorable properties. Here we show that even simple scan strategies, complex ones being inevitable when printing intricate designs, can inadvertently produce local alterations of the microstructure and preferential grain orientation over small areas - which easily remain unnoticed across the macroscale. We describe how a combined usage of neutron imaging and electron backscatter diffraction can reveal these localized variations and explain their origin within cm-sized parts. We explain the observed contrast variations by linking the neutron images to simulated data, pole figures and EBSD, providing an invaluable reference for future studies and showing that presumably minor changes of the scan strategy can have detrimental effects on the mechanical properties. In-situ tensile tests reveal that fracture occurs in a region that was re-melted during the building process.

Herein, the concept of constructing binder and carbon additive free organosulfur cathode was proved based on thiol containing conducting polymer poly 4 thiophene 3 yl benzenethiol PTBT . The PTBT featured the polythiophene structure main chain as a highly conducting framework and the benzenethiol side chain to copolymerize with sulfur and form a crosslinked organosulfur polymer namely S PTBT . Meanwhile, it could be in situ deposited on the current collector by electro polymerization, making it a binder free and free standing cathode for Li S batteries. The S PTBT cathode exhibited a reversible capacity of around 870 amp; 8197;mAh amp; 8201;g amp; 8722;1 at 0.1 amp; 8201;C and improved cycling performance compared to the physically mixed cathode namely S amp;PTBT . This multifunction cathode eliminated the influence of the additives carbon binder , making it suitable to be applied as a model electrode for operando analysis. Operando X ray imaging revealed the remarkable effect in the suppression of polysulfides shuttle via introducing covalent bonds, paving the way for the study of the intrinsic mechanisms in Li S batteries

In digital neutron imaging, the neutron scintillator screen is a limiting factor of spatial resolution and neutron capture efficiency and must be improved to enhance the capabilities of digital neutron imaging systems. Commonly used neutron scintillators are based on 6LiF and gadolinium oxysulfide neutron converters. This work explores boron-based neutron scintillators because 10B has a neutron absorption cross-section four times greater than 6Li, less energetic daughter products than Gd and 6Li, and lower γ-ray sensitivity than Gd. These factors all suggest that, although borated neutron scintillators may not produce as much light as 6Li-based screens, they may offer improved neutron statistics and spatial resolution. This work conducts a parametric study to determine the effects of various boron neutron converters, scintillator and converter particle sizes, converter-to-scintillator mix ratio, substrate materials, and sensor construction on image quality. The best performing boron-based scintillator screens demonstrated an improvement in neutron detection efficiency when compared with a common 6LiF/ZnS scintillator, with a 125% increase in thermal neutron detection efficiency and 67% increase in epithermal neutron detection efficiency. The spatial resolution of high-resolution borated scintillators was measured, and the neutron tomography of a test object was successfully performed using some of the boron-based screens that exhibited the highest spatial resolution. For some applications, boron-based scintillators can be utilized to increase the performance of a digital neutron imaging system by reducing acquisition times and improving neutron statistics.

Polychromatic and wavelength-selective neutron transmission radiography were applied during bead-on-plate welding on 5 mm thick sheets on the face side of martensitic low transformation temperature (LTT) steel plates using gas tungsten arc welding (GTAW). The in situ visualization of austenitization upon welding and subsequent α’-martensite formation during cooling could be achieved with a temporal resolution of 2 s for monochromatic imaging using a single neutron wavelength and of 0.5 s for polychromatic imaging using the full spectrum of the beam (white beam). The spatial resolution achieved in the experiments was approximately 200 µm. The transmitted monochromatic neutron beam intensity at a wavelength of λ = 0.395 nm was significantly reduced during cooling below the martensitic start temperature Ms since the emerging martensitic phase has a ~10% higher attenuation coefficient than the austenitic phase. Neutron imaging was significantly influenced by coherent neutron scattering caused by the thermal motion of the crystal lattice (Debye–Waller factor), resulting in a reduction in the neutron transmission by approx. 15% for monochromatic and by approx. 4% for polychromatic imaging.

The exploitation of high-capacity conversion-type materials such as sulfur in solid-state secondary batteries is a dream combination for achieving improved battery safety and high energy density in the push towards a sustainable future. Yet, the exact rate-limiting step, bottlenecking further development of solid-state lithium-sulfur batteries, has not been determined. Here, we directly visualize the spatial distribution of lithium via neutron imaging during operation and show that sluggish macroscopic ion transport within the composite cathode is rate-limiting. Observing a reaction front propagating from the separator side towards the current collector confirms detrimental influences of a low effective ionic conductivity. Furthermore, irreversibly concentrated lithium in the vicinity of the current collector, revealed via state-of-charge-dependent tomography, highlights a hitherto-overlooked loss mechanism triggered by sluggish effective ionic transport within a composite cathode. This discovery will be a cornerstone for future research on solid-state batteries, irrespective of the type of active material.

The exploitation of high-capacity conversion-type materials such as sulfur in solid-state secondary batteries is a dream combination for achieving improved battery safety and high energy density in the push towards a sustainable future. Yet, the exact rate-limiting step, bottlenecking further development of solid-state lithium-sulfur batteries, has not been determined. Here, we directly visualize the spatial distribution of lithium via neutron imaging during operation and show that sluggish macroscopic ion transport within the composite cathode is rate-limiting. Observing a reaction front propagating from the separator side towards the current collector confirms detrimental influences of a low effective ionic conductivity. Furthermore, irreversibly concentrated lithium in the vicinity of the current collector, revealed via state-of-charge-dependent tomography, highlights a hitherto-overlooked loss mechanism triggered by sluggish effective ionic transport within a composite cathode. This discovery will be a cornerstone for future research on solid-state batteries, irrespective of the type of active material.

Low temperature alkaline water electrolysis is a well-known technology for hydrogen production and advantageous because less noble metals are needed compared to Proton Exchange Membrane (PEM) electrolysis. However, the two-phase flow behavior and especially the gas bubble distribution and flow during the operation in a zero-gap alkaline electrolysis cell have not been investigated in sufficient detail. Previous studies used e.g. transparent model electrolysis cells or focused on single flow phenomena e.g. gas bubble nucleation, growth or detachment. Recent publications show evidence that the ohmic resistance of zero-gap alkaline electrolysis cells is greater than the ohmic resistance of the used diaphragm, which has been believed the only term contributing to the ohmic resistance in zero-gap cells [1]. This suggests that the evolving gas bubbles might have a relation to the total ohmic resistance of the cell. As possible reasons nano bubbles in the pores of the diaphragm and a possible finite gap between electrodes and diaphragm is mentioned [2]. Haverkort et al. assume that the frontal area of the electrodes might be inactive [3]. To prove the hypothesis and to deepen the general understanding of the two-phase flow inside an alkaline electrolysis cell we conducted operando cell measurements and visualized the electrolyte-gas bubble flow in an alkaline electrolysis cell by using neutron radiography. Thanks to the powerful neutron source at Institute Laue-Langevin in Grenoble, it was possible to observe the whole flow field with all flow channels at once with a sufficient temporal resolution to observe the movement of single gas bubbles, from nucleation to the moment of exiting the channel. The temporal resolution was 50 fps, which makes these measurement, to the best authors’ knowledge, the first to show the transient effects inside of a zero gap alkaline electrolysis cell. For the measurements, the NeXT (Neutron and X-Ray Tomograph) instrument was used which is the imaging station with one of the highest neutron fluxes of the world (1.4 E10 n/cm²/s at the end of the guide) [4]. The neutron beam was used to carry out through-plane measurements of the electrolysis cell. The measurements were conducted at a variety of operation conditions, varying the current density, the electrolyte volume flow and the operation temperature. At different operation conditions Electrical Impedance Spectroscopy (EIS) measurements have been conducted to measure the ohmic resistance of the cell. The used cell is an alkaline single cell out of a Nickel alloy with vertical parallel flow channel and a pocket milled to the backside of the cell in order to increase the transmission through the cell material. From the results of the measurements we observe a relation between current density (forming gas amount) and the ohmic resistance and thus establish a relation to the gas bubble behavior inside the electrolysis cell. Furthermore, we analyzed the velocity of the gas bubbles inside the channel depending on the different operation conditions, as well as the agglomeration behavior of the bubbles and their flow regime. [1] Phillips et al.,Minimising the ohmic resistance of an alkaline electrolysis cell through effective cell design, 2017 [2] de Groot et al., Ohmic resistance in zero gap alkaline electrolysis with a Zirfon diaphragm,2021 [3] Haverkort et al., Voltage losses in zero-gap alkaline water electrolysis,2021 [4] Tengattini et al., NeXT-Grenoble, the Neutron and X-ray tomograph in Grenoble, 2020 Figure 1

The fuel rod claddings in nuclear light water reactors are made of zirconium alloys. Corrosion of these alloys during operation and in particular high temperature oxidation during nuclear accidents results in the production of free hydrogen. The cladding can absorb this hydrogen. It affects the mechanical properties of the cladding material. Hydrogen embrittlement of these materials provides the risk of brittle fracture of the cladding by thermo-shock during emergency cooling. At KIT the behaviour of cladding materials under different hypothetical nuclear accident scenarios was investigated. One focus was on hydrogen absorption and distribution/re-distribution in the alloys. The hydrogen distribution was determined mainly by neutron tomography. Examples for the determination of the 3D hydrogen distribution in cladding tubes after loss of coolant accident simulation tests are given and discussed.

All the major clades of angiosperms have a fossil record that extends back to more than 100 million years ago (Early Cretaceous), mostly in agreement with molecular dating. However, the Early Cretaceous record of monocots is very poor compared to other angiosperms. Their herbaceous nature has been invoked to explain this rarity, but biogeography could also be an explanation. Unfortunately, most of the Early Cretaceous angiosperm record comes from northern mid-latitudes. The Crato plattenkalk limestone offers a unique window into the Early Cretaceous vegetation of the tropics and has already yielded monocot fossils. Here, we describe a whole monocotyledonous plant from root to reproductive organs that is anatomically preserved. The good preservation of the fossils allowed the evaluation of reproductive, vegetative and anatomical characteristics of monocots, leading to a robust identification of this fossil as a crown monocot. Its occurrence in Northern Gondwana supports the possibility of an early radiation of monocots in the tropics.

High‐speed neutron tomographies (1‐min acquisition) have been acquired during water invasion into air‐filled samples of both intact and deformed (ex situ) Vosges sandstone. Three‐dimensional volume images have been processed to detect and track the evolution of the waterfront and to calculate full‐field measurement of its speed of advance. The flow process correlates well with known rock properties and is especially sensitive to the distribution of the altered properties associated with observed localized deformation, which is independently characterized by Digital Volume Correlation of X‐ray tomographies acquired before and after the mechanical test. The successful results presented herein open the possibility of in situ analysis of the local evolution of hydraulic properties of rocks due to mechanical deformation. (Less)

In-depth understanding of water management is essential for the optimization of the performance and durability of polymer electrolyte fuel cells (PEFCs). Neutron imaging of liquid water has proven to be a powerful diagnostic technique, but it cannot distinguish between ‘legacy’ water that has accumulated in the system over time and ‘nascent’ water recently generated by reaction. Here, a novel technique is introduced to investigate the spatially resolved water exchange characteristics inside PEFCs. Hydro-electrochemical impedance imaging (HECII) involves making a small AC-sinusoidal perturbation to a cell and measuring the consequential water generated, using neutron radiographs, associated with the stimulus frequency. Subsequently, a least-squares estimation (LSE) analysis is applied to derive the spatial amplitude ratio and phase shift. This technique provides a complementary view to conventional neutron imaging and provides information on the source and ‘history’ of water in the system. By selecting a suitable perturbation frequency, HECII can be used to achieve an alternative image ‘contrast’ and identify different features involved in the water dynamics of operational fuel cells.

Hydrogen interaction with metals is well known to have severe detrimental effects on their mechanical properties. The use of modern high-strength steels, which are attractive to improve fuel economy by reducing weight as well as candidates for H storage cylinders and other components, is currently being severely limited by the fact that the presence of H can cause embrittlement of the material. In addition to steel, several other metals and alloys used in the nuclear industry, like Ti and Zr, are susceptible to H degradation through hydride formation and subsequent cracking. Microstructure-specific H mapping has been recognized as the most important challenge on the pathway towards a better understanding of the nature of H embrittlement in metallic alloys [1,2] as well as the development of H storage solutions based on metal hydrides [3]. Unfortunately, the characterization of H interactions with metals is an extremely challenging task and neutron-based techniques are of exceptional importance in this matter because - contrary to X-rays and electrons - thermal and cold neutrons interact strongly with the H nuclei [4], while the neutron beam is only weakly attenuated by the relevant metallic materials. Therefore, hydrogen distributions can be measured and quantified even in 3D by tomographic methods [5]. Here we present several neutron imaging investigations of embrittlement and cracking in Fe and Zr based metal alloys and optimization studies of hydrogen storage systems containing metal hydrides as an active substance. The advantages and the limitations of the experimental methods as well as the attempts for hydrogen quantification will be discussed in detail.

A review is presented on the strategic use of scattering and imaging tools to design immunologic complexes based on porous silica for oral vaccine formulations., This article summarizes developments attained in oral vaccine formulations based on the encapsulation of antigen proteins inside porous silica matrices. These vaccine vehicles show great efficacy in protecting the proteins from the harsh acidic stomach medium, allowing the Peyer’s patches in the small intestine to be reached and consequently enhancing immunity. Focusing on the pioneering research conducted at the Butantan Institute in Brazil, the optimization of the antigen encapsulation yield is reported, as well as their distribution inside the meso- and macroporous network of the porous silica. As the development of vaccines requires proper inclusion of antigens in the antibody cells, X-ray crystallography is one of the most commonly used techniques to unveil the structure of antibody-combining sites with protein antigens. Thus structural characterization and modelling of pure antigen structures, showing different dimensions, as well as their complexes, such as silica with encapsulated hepatitis B virus-like particles and diphtheria anatoxin, were performed using small-angle X-ray scattering, X-ray absorption spectroscopy, X-ray phase contrast tomography, and neutron and X-ray imaging. By combining crystallography with dynamic light scattering and transmission electron microscopy, a clearer picture of the proposed vaccine complexes is shown. Additionally, the stability of the immunogenic complex at different pH values and temperatures was checked and the efficacy of the proposed oral immunogenic complex was demonstrated. The latter was obtained by comparing the antibodies in mice with variable high and low antibody responses.