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International audience; Most of the post-Lithium-ion (Li-ion) devices, such as Li–sulfur, Li–O2, or all-solid-state Li batteries, have in common an negative electrode made of metallic Li.1 The main failure mode of Li based batteries is the inhomogeneity of the Li electrodeposits onto the Li metal negative electrode during charge steps, leading to dendrite growth and low Coulombic efficiency.2 Tomography and radiography imaging techniques are now vastly employed for battery materials analysis thanks to the possibility to perform noninvasive in situ and operando experiments.3 X-ray tomography is a powerful tool for studying dendrites as it provides useful information about their locations, dynamics, and microstructures. However, the use of neutron tomography is scarcely reported for Li electrodeposit analysis due to the difficulty to reach sufficient image resolution to capture the deposit microstructure, that is, typically below 10 to 20 µm. Furthermore, the different interactions of X-rays and neutrons with Li, which has significantly different opacity in the two cases, make the two techniques highly complementary.4 Notably, the capacity of neutrons to discern different Li isotopes is pivotal to get insight into the composition of Li deposits, by distinguishing between Li originating from an electrode (6Li in this study) and Li originating from the Li salt electrolyte (mainly in 7Li here). Indeed, the theoretical linear neutron attenuation coefficient of 6Li is about 15 and 2,000 times larger than that of natural Li and 7Li, respectively.In this study, we report as a proof of concept, an in situ neutron tomography imaging of Li electrodeposits in a cycled Li symmetric cell (see Figure 1).5 The electrochemical cell comprises a natural Li electrode, a 6Li electrode, and a deuterated liquid electrolyte. The neutron tomography is compared with X-ray tomography images of the same electrochemical cell acquired both at an X-ray synchrotron beamline and at a laboratory X-ray tomograph. Neutron tomography is shown to be compatible with in situ analysis and capable of capturing the overall morphology of the Li deposits in good accordance with X-ray tomography analyses.

This communication explores the influence of boundary effects, embedded sensors and crack opening on high-temperature experiments of concrete as revealed by in situ neutron tomography. The hypotheses routinely taken about these experimental aspects in common practice are hereby reassessed in light of the insight given by noninvasive full-field measurements. Notably, we directly assess the heat and moisture insulation techniques and reveal the influence of temperature and gas pressure monitoring on the testing conditions, opening new perspectives toward their improvement.

Frequency modulated continuous wave (FMCW) radar in the K-band has been shown to be an effective detector of geomaterial physical properties being highly sensitive to rock characteristics, particularly mineral composition and, for porous rock, variations in liquid water content. This research demonstrates that contrasts in FMCW return signals with time correlate with changes in geomaterial water content. FMCW signal returns were acquired for porous sandstone samples subjected to controlled water injection while also in a neutron beam, taking advantage of the well-known, and well-calibrated, attenuation of neutrons by hydrogen atoms for the water-containing porous sandstone samples. The sequential neutron tomographic images clearly show water moving up the sample with time while the FMCW observations show increases in radar reflection coefficient as a function of water position in the field of view. The observed FMCW detection of flood-front position is corroborated by the synchronous neutron tomographic images. We also observe repeatable variations in the radar reflection coefficient as a function of sample orientation during fluid injection, verifying that FMCW sensing offers real-time insight into the interactions between fluid movement and sample heterogeneity, via non-contact and non-invasive flood-front tracking. This research demonstrates that FMCW has potential to be a more accessible and easily deployable sensing modality than neutron tomography, enabling dynamic geomaterial testing to be conducted outwith the confines of the highly controlled laboratory environment required for neutron investigation.

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)

The bone tissue formed at the contact interface with metallic implants, particularly its 3D microstructure, plays a pivotal role for the structural integrity of implant fixation. X-ray tomography is the classical imaging technique used for accessing microstructural information from bone tissue. However, neutron tomography has shown promise for visualising the immediate bone-metal implant interface, something which is highly challenging with x-rays due to large differences in attenuation between metal and biological tissue causing image artefacts. To highlight and explore the complementary nature of neutron and x-ray tomography, proximal rat tibiae with titanium-based implants were imaged with both modalities. The two techniques were compared in terms of visualisation of different material phases and by comparing the properties of the individual images, such as the contrast-to-noise ratio. After superimposing the images using a dedicated image registration algorithm, the complementarity was further investigated via analysis of the dual modality histogram, joining the neutron and x-ray data. From these joint histograms, peaks with well-defined grey value intervals corresponding to the different material phases observed in the specimens were identified and compared. The results highlight differences in how neutrons and x-rays interact with biological tissues and metallic implants, as well as the benefits of combining both modalities. Future refinement of the joint histogram analysis could improve the segmentation of structures and tissues, and yield novel information about specimen-specific properties such as moisture content.

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 &gamma, 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.

Concrete has a tendency to spall, that is, to eject layers when subjected to high temperatures. This is an erratic phenomenon, and our understanding of the underlying physical process is still limited. A driving process is moisture transfer, whose experimental investigation has so far mostly been limited to macroscopic or point‐wise observations, limiting both our understanding and the validation of the proposed models. In this paper, a non‐contact technique, neutron imaging, is used to extract a the full‐field distribution of moisture in 3D and in real time, while the concrete is heated at high temperatures. This reveals a number of processes often underestimated or ignored in the traditional experimental approaches reported in the literature. Notably, the effect on the evolving moisture profiles of varying heating rates for multiple insulation techniques as well the strong influence of the addition of spalling‐mitigating additives is presented. The first ever example of neutron tomography of a spalled sample is also reported, and some preliminary analyses of the effect that moisture clog formation and heating rates have on it are revealed.

The drying of cement-based materials is intimately related to their durability, which has significant economic, social and environmental repercussions. The evolution of the saturation of the pore network and the associated drying shrinkage are in fact leading causes of cracking and of the ensuing penetration of aggressive chemicals. This process is highly heterogeneous, due to the thermo-hydric spatial gradients developing in the material from the exposed surfaces to its core and because of local effects, driven by the intrinsically heterogeneous micro-structure (e.g., by the distribution of pores and aggregates). It follows that macroscopic, sample-scale measurements cannot fully disclose the complexity of the underlying processes. In the last few decades, significant advances in full-field techniques have allowed an unprecedented insight into these local processes. For cement-based materials, x-ray and neutron tomography lend themselves as ideal, and highly complementary, tools for the study of their thermo-hydro-mechanical behavior. Notably, the high sensitivity to density variations of x-ray imaging gives access to the developments of fractures, in 4D (3D + time). On the other hand, neutron tomography allows the study of the evolution of the moisture field in 4D, thanks to its high hydrogen sensitivity. The combination of these two techniques provides a unique insight in thermo-hydro-mechanical couplings, e.g., the effect of cracks on the water content field. This contribution presents novel 5D datasets (3D tomographies along time, plus truly simultaneous x-ray and Neutron rapid acquisitions) in-operando of a cement paste and of a concrete sample heated at moderate temperatures (up to 140∘C). The analysis of this 5D data-set (once aligned in time and across modalities) allows for example a quantification of the 4D moisture profiles which were found to predict an overall water loss at hydric equilibrium coherent with the corresponding analytical analysis. In the cement paste sample, the x-ray dataset captures the evolution of an extensive cracking network, opening and propagation toward the core of the sample. A novel analysis procedure is here proposed which allows the extraction of these fractures and the analysis of their interplay with local drying as captured through neutron imaging. This for example reveals the depth of penetration of drying in the vicinity of the fractures along time, which is essential for the assessment and calibration of hydro-mechanical coupled models.

Bone properties and especially its microstructure around implants are crucial to evaluate the osseointegration of prostheses in orthopaedic, maxillofacial and dental surgeries. Given the intrinsic heterogeneous nature of the bone microstructure, an ideal probing tool to understand and quantify bone formation must be spatially resolved. X-ray imaging has often been employed, but is limited in the presence of metallic implants, where severe artifacts generally arise from the high attenuation of metals to x-rays. Neutron tomography has recently been proposed as a promising technique to study bone-implant interfaces, thanks to its lower interaction with metals. The aim of this study is to assess the potential of neutron tomography for the characterisation of bone tissue in the vicinity of a metallic implant. A standardised implant with a bone chamber was implanted in rabbit bone. Four specimens were imaged with neutron tomography and subsequently compared to non-decalcified histology to stain soft and mineralised bone tissues, used here as a ground-truth reference. An intensity-based image registration procedure was performed to place the 12 histological slices within the corresponding 3D neutron volume. Significant correlations (p BIC) ratio (R = 0.77) and the bone content inside the chamber (R = 0.89). The results indicate that mineralised bone tissue can be reliably detected by neutron tomography. However, the BIC ratio and bone content were found to be overestimated with neutron imaging, which may be explained by its sensitivity to non-mineralised soft tissues, as revealed by histological staining. This study highlights the suitability of neutron tomography for the analysis of the bone-implant interface. Future work will focus on further distinguishing soft tissues from bone tissue, which could be aided by the adoption of contrast agents.

International audience; The question of registering two images (or image volumes) acquired with different modalities, and thus exhibiting different contrast, at different positions is addressed based on an extension of global Digital Image (or Volume) Correlation. A specific comparison metric is introduced allowing the signature of the different phases to be related. A first solution consists of Gaussian mixture to describe the joint distribution of gray levels, which not only provides a matching of both images, but also offers a natural segmentation indicator. A second 'self-adapting' solution does not include any postulated a priori model for the joint histogram and leads to a registration of the images based on their initial histograms. The algorithm is implemented with a pyramidal multiscale framework for robustness. The proposed multiscale technique is tested on two 3D images obtained from X-ray and neutron tomography respectively. The proposed approach brings the two images to coincidence with a sub-pixel accuracy and allows for a " natural " segmentation of the different phases.