Compact and versatile neutron imaging detector with sub-4µm spatial resolution based on a single-crystal thin-film scintillator.

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.

External water transport is more important than vascular transport in the extreme atmospheric epiphyte Tillandsia usneoides (Spanish moss).

Most epiphytic bromeliads, especially those in the genus Tillandsia, lack functional roots and rely on the absorption of water and nutrients by large, multicellular trichomes on the epidermal surfaces of leaves and stems. Another important function of these structures is the spread of water over the epidermal surface by capillary action between trichome "wings" and epidermal surface. Although critical for the ultimate absorption by these plants, understanding of this function of trichomes is primarily based on light microscope observations. To better understand this phenomenon, the distribution of water was followed by its attenuation of cold neutrons following application of H2 O to the cut end of Tillandsia usneoides shoots. Experiments confirmed the spread of added water on the external surfaces of this "atmospheric" epiphyte. In a morphologically and physiologically similar plant lacking epidermal trichomes, water added to the cut end of a shoot clearly moved via its internal xylem and not on its epidermis. Thus, in T. usneoides, water moves primarily by capillarity among the overlapping trichomes forming a dense indumentum on shoot surfaces, while internal vascular water movement is less likely. T. usneoides, occupying xeric microhabitats, benefits from reduction of water losses by low-shoot xylem hydraulic conductivities.

What comes NeXT? - High-Speed Neutron Tomography at ILL.

Here, we report on a new record in the acquisition time for fast neutron tomography. With an optimized imaging setup, it was possible to acquire single radiographic projection images with 10 ms and full tomographies with 155 projections images and a physical spatial resolution of 200 µm within 1.5 s. This is about 6.7 times faster than the current record. We used the technique to investigate the water infiltration in the soil with a living lupine root system. The fast imaging setup will be part of the future NeXT instrument at ILL in Grenoble with a great field of possible future applications.

Spatially resolved time-of-flight neutron imaging using a scintillator CMOS-camera detector with kHz time resolution.

We herein report on using a compact and low cost scintillator-camera based neutron detection system for quantitative time-of-flight imaging applications. While powerful pulsed neutron sources emerge and enable unprecedented scientific achievements, one bottleneck is the availability of suitable detectors that provide high count- and high frame- rate capabilities. For imaging applications the achievable spatial resolution/pixel size is obviously another key characteristic. While major effort was so far directed towards the development of neutron counting type imaging detectors, this work demonstrates that a camera based detector system as commonly employed at steady state sources can also be used if a suitable camera is utilized. This is demonstrated at the ESS test beamline (V20) at Helmholtz-Zentrum Berlin by recording the time-of-flight transmission spectrum of steel samples using a CMOS camera at 1 kHz frame rate, revealing the characteristic Bragg edge pattern. This 'simple' setup in the current state presents a useful option of neutron detection and has the potential to overcome many of the existing limitations and could provide a reliable alternative for neutron detector technology in general, given that the camera and scintillator technology keep up the current development speed.

Inner ear development in cetaceans.

Cetaceans face the challenge of maintaining equilibrium underwater and obtaining sensory input within a dense, low-visibility medium. The cetacean ear represents a key innovation that marked their evolution from terrestrial artiodactyls to among the most fully aquatic mammals in existence. Using micro-CT and histological data, we document shape and size changes in the cetacean inner ear during ontogeny, and demonstrate that, as a proportion of gestation time, the cetacean inner ear is precocial in its growth compared with that of suid artiodactyls. Cetacean inner ears begin ossifying and reach near-adult shape as early as at 32% of the gestation period, and near-adult dimensions as early as at 27% newborn total length. Our earliest embryos with measurable inner ears (13% newborn length) exhibit a flattened cochlea (i.e. smaller distance from cochlear apex to round window) compared with later and adult stages. Inner ears of Sus scrofa have neither begun ossifying nor reached near-adult dimensions at 55% of the gestation period, but have an adult-like ratio of cochlear diameters to each other, suggesting an adult-like shape. The precocial development of the cetacean inner ear complements previous work demonstrating precocial development of other cetacean anatomical features such as the locomotor muscles to facilitate swimming at the moment of birth.

Eocene lizard from Germany reveals amphisbaenian origins.

Amphisbaenia is a speciose clade of fossorial lizards characterized by a snake-like body and a strongly reinforced skull adapted for head-first burrowing. The evolutionary origins of amphisbaenians are controversial, with molecular data uniting them with lacertids, a clade of Old World terrestrial lizards, whereas morphology supports a grouping with snakes and other limbless squamates. Reports of fossil stem amphisbaenians have been falsified, and no fossils have previously tested these competing phylogenetic hypotheses or shed light on ancestral amphisbaenian ecology. Here we report the discovery of a new lacertid-like lizard from the Eocene Messel locality of Germany that provides the first morphological evidence for lacertid-amphisbaenian monophyly on the basis of a reinforced, akinetic skull roof and braincase, supporting the view that body elongation and limblessness in amphisbaenians and snakes evolved independently. Morphometric analysis of body shape and ecology in squamates indicates that the postcranial anatomy of the new taxon is most consistent with opportunistically burrowing habits, which in combination with cranial reinforcement indicates that head-first burrowing evolved before body elongation and may have been a crucial first step in the evolution of amphisbaenian fossoriality.

Mammalian development does not recapitulate suspected key transformations in the evolutionary detachment of the mammalian middle ear.

The ectotympanic, malleus and incus of the developing mammalian middle ear (ME) are initially attached to the dentary via Meckel's cartilage, betraying their origins from the primary jaw joint of land vertebrates. This recapitulation has prompted mostly unquantified suggestions that several suspected--but similarly unquantified--key evolutionary transformations leading to the mammalian ME are recapitulated in development, through negative allometry and posterior/medial displacement of ME bones relative to the jaw joint. Here we show, using µCT reconstructions, that neither allometric nor topological change is quantifiable in the pre-detachment ME development of six marsupials and two monotremes. Also, differential ME positioning in the two monotreme species is not recapitulated. This challenges the developmental prerequisites of widely cited evolutionary scenarios of definitive mammalian middle ear (DMME) evolution, highlighting the requirement for further fossil evidence to test these hypotheses. Possible association between rear molar eruption, full ME ossification and ME detachment in marsupials suggests functional divergence between dentary and ME as a trigger for developmental, and possibly also evolutionary, ME detachment. The stable positioning of the dentary and ME supports suggestions that a 'partial mammalian middle ear' as found in many mammaliaforms--probably with a cartilaginous Meckel's cartilage--represents the only developmentally plausible evolutionary DMME precursor.

Visualization of embolism formation in the xylem of liana stems using neutron radiography.

BACKGROUND AND AIMS: Cold neutron radiography was applied to directly observe embolism in conduits of liana stems with the aim to evaluate the suitability of this method for studying embolism formation and repair. Potential advantages of this method are a principally non-invasive imaging approach with low energy dose compared with synchrotron X-ray radiation, a good spatial and temporal resolution, and the possibility to observe the entire volume of stem portions with a length of several centimetres at one time. METHODS: Complete and cut stems of Adenia lobata, Aristolochia macrophylla and Parthenocissus tricuspidata were radiographed at the neutron imaging facility CONRAD at the Helmholtz-Zentrum Berlin für Materialien und Energie, with each measurement cycle lasting several hours. Low attenuation gas spaces were separated from the high attenuation (water-containing) plant tissue using image processing. KEY RESULTS: Severe cuts into the stem were necessary to induce embolism. The formation and temporal course of an embolism event could then be successfully observed in individual conduits. It was found that complete emptying of a vessel with a diameter of 100 µm required a time interval of 4 min. Furthermore, dehydration of the whole stem section could be monitored via decreasing attenuation of the neutrons. CONCLUSIONS: The results suggest that cold neutron radiography represents a useful tool for studying water relations in plant stems that has the potential to complement other non-invasive methods.

The Complex, Unique, and Powerful Imaging Instrument for Dynamics (CUPI2D) at the Spallation Neutron Source (invited).

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.

Constructing Binder- and Carbon Additive-Free Organosulfur Cathodes Based on Conducting Thiol-Polymers through Electropolymerization for Lithium-Sulfur Batteries.

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 mAh g-1 at 0.1 C and improved cycling performance compared to the physically mixed cathode (namely S&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.

High-speed 4D neutron computed tomography for quantifying water dynamics in polymer electrolyte fuel cells.

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.

Tem-per-ature dependence in Bragg edge neutron transmission measurements.

A systematic study has been carried out to investigate the neutron transmission signal as a function of sample tem-per-ature. In particular, the experimentally de-ter-mined wavelength-dependent neutron attenuation spectra for a martensitic steel at tem-per-atures ranging from 21 to 700°C are com-pared with simulated data. A theoretical description that includes the Debye-Waller factor in order to describe the tem-per-ature influence on the neutron cross sections was im-plemented in the nxsPlotter software and used for the simulations. The analysis of the attenuation coefficients at varying tem-per-atures shows that the missing contributions due to elastic and inelastic scattering can be clearly distinguished: while the elastically scattered intensities decrease with higher tem-per-atures, 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 qu-antify 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 qu-anti-fiable results.

Using crystallography tools to improve 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.

Skeletal ossification and sequence heterochrony in xenarthran evolution.

Previous analyses of how mammals vary in their ossification sequences have focused on monotremes, marsupials, and boreoeutherian placentals. Here, we focus on the sequence of cranial and postcranial ossification events during growth in the xenarthran skull and skeleton, including armadillos, anteaters, and sloths. We use two different methods to quantify sequence heterochrony: sequence analysis of variance (ANOVA) and event-paring/Parsimov. Our results indicate that Parsimov is conservative and does not detect clear heterochronic shifts between xenarthran and boreoeutherian placentals. Sequence-ANOVA performs better, but both methods exhibit sensitivity to the artifactual accumulation of ties. By controlling for ties and taking into account results that the methods have in common, our analysis suggests that xenarthrans significantly differ from other placentals by a late ossification of the sternum and an early ossification of the phalanges and pubis. We interpret these differences as showing that heterochrony plays a role in the skeletal development of xenarthrans, a change from previous studies that have emphasized the developmental homogeneity of the skeleton across placental mammals.

Three-dimensional in vivo analysis of water uptake and translocation in maize roots by fast neutron tomography.

Root water uptake is an essential process for terrestrial plants that strongly affects the spatiotemporal distribution of water in vegetated soil. Fast neutron tomography is a recently established non-invasive imaging technique capable to capture the 3D architecture of root systems in situ and even allows for tracking of three-dimensional water flow in soil and roots. We present an in vivo analysis of local water uptake and transport by roots of soil-grown maize plants-for the first time measured in a three-dimensional time-resolved manner. Using deuterated water as tracer in infiltration experiments, we visualized soil imbibition, local root uptake, and tracked the transport of deuterated water throughout the fibrous root system for a day and night situation. This revealed significant differences in water transport between different root types. The primary root was the preferred water transport path in the 13-days-old plants while seminal roots of comparable size and length contributed little to plant water supply. The results underline the unique potential of fast neutron tomography to provide time-resolved 3D in vivo information on the water uptake and transport dynamics of plant root systems, thus contributing to a better understanding of the complex interactions of plant, soil and water.

Characterisation of Single-Phase Fluid-Flow Heterogeneity Due to Localised Deformation in a Porous Rock Using Rapid Neutron Tomography.

The behaviour of subsurface-reservoir porous rocks is a central topic in the resource engineering industry and has relevant applications in hydrocarbon, water production, and CO2 sequestration. One of the key open issues is the effect of deformation on the hydraulic properties of the host rock and, specifically, in saturated environments. This paper presents a novel full-field data set describing the hydro-mechanical properties of porous geomaterials through in situ neutron and X-ray tomography. The use of high-performance neutron imaging facilities such as CONRAD-2 (Helmholtz-Zentrum Berlin) allows the tracking of the fluid front in saturated samples, making use of the differential neutron contrast between "normal" water and heavy water. To quantify the local hydro-mechanical coupling, we applied a number of existing image analysis algorithms and developed an array of bespoke methods to track the water front and calculate the 3D speed maps. The experimental campaign performed revealed that the pressure-driven flow speed decreases, in saturated samples, in the presence of pre-existing low porosity heterogeneities and compactant shear-bands. Furthermore, the observed complex mechanical behaviour of the samples and the associated fluid flow highlight the necessity for 3D imaging and analysis.

The Neutron Imaging Instrument CONRAD-Post-Operational Review.

The neutron imaging instrument CONRAD was operated as a part of the user program of the research reactor BER-II at Helmholtz-Zentrum Berlin (HZB) from 2005 to 2020. The instrument was designed to use the neutron flux from the cold source of the reactor, transported by a curved neutron guide. The pure cold neutron spectrum provided a great advantage in the use of different neutron optical components such as focusing lenses and guides, solid-state polarizers, monochromators and phase gratings. The flexible setup of the instrument allowed for implementation of new methods including wavelength-selective, dark-field, phase-contrast and imaging with polarized neutrons. In summary, these developments helped to attract a large number of scientists and industrial customers, who were introduced to neutron imaging and subsequently contributed to the expansion of the neutron imaging community.

Multimodal ex vivo methods reveal that Gd-rich corrosion byproducts remain at the implant site of biodegradable Mg-Gd screws.

Extensive research is being conducted on magnesium (Mg) alloys for bone implant manufacturing, due to their biocompatibility, biodegradability and mechanical properties. Gadolinium (Gd) is among the most promising alloying elements for property control in Mg alloy implants; however, its toxicity is controversial. Investigating Gd behavior during implant corrosion is thus of utmost importance. In this study, we analyzed the degradation byproducts at the implant site of biodegradable Mg-5Gd and Mg-10Gd implants after 12 weeks healing time, using a combination of different imaging techniques: histology, energy-dispersive x-ray spectroscopy (EDX), x-ray microcomputed tomography (µCT) and neutron µCT. The main finding has been that, at the healing time in exam, the corrosion appears to have involved only the Mg component, which has been substituted by calcium and phosphorus, while the Gd remains localized at the implant site. This was observed in 2D by means of EDX maps and extended to 3D with a novel application of neutron tomography. X-ray fluorescence analysis of the main excretory organs also did not reveal any measurable accumulation of Gd, further reinforcing the conclusion that very limited or no removal at all of Gd-alloy happened during degradation. STATEMENT OF SIGNIFICANCE: Gadolinium is among the most promising alloying elements for property control in biodegradable magnesium alloy implants, but its toxicity is controversial and its behavior during corrosion needs to be investigated. We combine 2D energy dispersive x-ray spectroscopy and 3D neutron and x-ray tomography to image the degradation of magnesium-gadolinium implants after 12 weeks of healing time. We find that, at the time in exam, the corrosion has involved only the magnesium component, while the gadolinium remains localized at the implant site. X-ray fluorescence analysis of the main excretory organs also does not reveal any measurable accumulation of Gd, further reinforcing the conclusion that very limited or no removal at all of Gd-alloy has happened during degradation.

4D imaging of lithium-batteries using correlative neutron and X-ray tomography with a virtual unrolling technique.

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/MnO2 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†situ and Operando Tracking of Microstructure and Volume Evolution of Silicon Electrodes by using Synchrotron X-ray Imaging.

The internal microstructure of a silicon electrode in a lithium ion battery was visualized by operando synchrotron X-ray radioscopy during battery cycling. The silicon particles were found to change their sizes upon lithiation and delithiation and the changes could be quantified. It was found that volume change of a particle is related to its initial size and is also largely determined by the changing surrounding electron-conductive network and internal interface chemical environment (e.g., electrolyte migration, solid-electrolyte interphase propagation) within fractured particles. Moreover, an expansion prolongation phenomenon was discovered whereby some particles continue expanding even after switching the battery current direction and shrinkage would be expected, which is explained by assuming different expansion characteristics of particle cores and outer regions. The study provides new basic insights into processes inside Si particles during lithiation and delithiation and also demonstrates the unique possibilities of operando synchrotron X-ray imaging for studying degradation mechanisms in battery materials.