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By producing electricity and heat from hydrogen with high yield and with only water as a byproduct, the proton exchange membrane fuel cell (PEMFC) is one of the most promising carbon-free alternati...

X-ray and neutron imaging are widely employed for battery materials, thanks to the possibility to perform noninvasive in situ and in operando analyses. X-ray tomography can be performed either in synchrotron or in laboratory facilities and is particularly well-suited to analyze bulk materials and electrode/electrolyte interfaces. Several post-lithium-ion (Li-ion) devices, such as Li–sulfur, Li–O2, or all-solid-state Li batteries, have an anode made of metallic Li in common. The main failure mode of Li batteries is the inhomogeneity of the Li electrodeposits onto the Li anode during charge steps, leading to dendrite growth and low Coulombic efficiency. X-ray tomography is a powerful tool for studying dendrites as it provides useful information about their locations, dynamics, and microstructures. So far, the use of neutron tomography is scarcely reported for Li deposit analysis due to the difficulty in reaching sufficient image resolution to capture the deposit microstructure, that is, typically below 10–20 µm. The very different interactions of X-rays and neutrons with Li, which has significantly different opacity in the two cases, make the two techniques highly complementary. Notably, the capacity of neutrons to discern different Li isotopes is pivotal to getting an 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. Therefore, a high imaging contrast difference is obtained between 6Li (high attenuation) and natural Li and 7Li (lower attenuations), which could allow a better understanding of the origin of the Li comprising the electrodeposits. In this work, we report, as a proof of concept, an in situ neutron tomography imaging of Li electrodeposits in a cycled Li symmetric cell. The electrochemical cell comprises a natural Li electrode, a 6Li electrode, and a deuterated liquid electrolyte. The neutron tomographies are 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.

The performance of an alternative membrane based on aromatic multiblock copolymer was compared to that of the conventional perfluorosulfonic acid (PFSA) polymer membrane during fuel cell operation. The fuel cell with the alternative membrane exhibited more severe voltage loss than the conventional at current densities above 0.6 A/cm2 with fully saturated reactants. To rationalize this difference, operando high-resolution neutron imaging was used to investigate water distribution in the fuel cells, in parallel with impedance measurements. The type of membrane strongly affected water distribution, not only from anode to cathode, but also in-plane between ribs and channels. Specifically, in the alternative membrane, ionomer in cathode catalyst layer was less hydrated and dried as current density increased. The voltage loss with the alternative membrane was ascribed to ionomer drying rather than to the accumulation of liquid water, in accordance with the evolution of ohmic resistance. Furthermore, the alternative membrane experienced swell/shrinkage resulting in material shifts during the operation. These results pinpoint that developing new ionomers for fuel cells require not only to quantify the bulk transport properties of alternative membranes compared to PFSA, but also to evaluate their interfacial properties and the impact of ionomer on water management.

Hydraulic fracturing, the creation of fractures by high-pressure fluid injection into a solid medium, is of interest to enhance the permeability of rocks. This complex three-dimensional hydro-mechanical process, however, has only been studied in the laboratory by boundary measurements or acoustic techniques with low spatio-temporal resolutions until now. In this paper, direct, high spatial resolution, and near real-time visualisation results of hydraulic fracture generation and propagation in prismatic specimens of Marcellus shale rock under in situ conditions (70 MPa, plane strain) are presented. Poly-methyl methacrylate specimens are also tested under the same conditions to highlight the importance of rocks' internal structure on the response of the tested rock. The results reveal a complex interaction among the injected fluid, the pre-existing natural fractures in shale structure, and the hydraulically induced fracture highlighting the governing role of rock fabric even under high stresses. These measurements are possible due to the unique sensitivity of neutrons to water. Besides the intrinsic interest of the results presented, this exploratory investigation highlights the potential of neutron imaging in elucidating the evolution of fluid flow and fluid-driven fractures, as X-rays have done for the evolution of solid structure only. Further, understanding of the mechanics of fracking will lead to development of more accurate hydro-mechanical constitutive models thus enabling the design of field operations with higher efficiencies.

International audience; This article focuses on a new experimental apparatus for investigating fluid flow under high pressure gradients within low-permeability porous media by means of neutron imaging. A titanium Hassler cell which optimises neutron transparency while allowing high pressure confinement (up to 50 MPa) and injection is designed for this purpose and presented here. This contribution focuses on the development of the proposed methodology thanks to some preliminary results obtained using a new neutron imaging facility named NeXT on the D50 beamline at the Institute Laue Langevin (Grenoble). The preliminary test was conducted by injecting normal water into concrete sample prepared and saturated with heavy water to take advantage of the isotope sensitivity of neutrons. The front between these two types of water is tracked in space and time with a combination of neutron radiography and tomography.

Thermochemical heat storage may become a key technology in balancing intermittent renewables by regulating production and demand peaks and in increasing the efficiency of energy systems by reusing waste heat. Nowadays, there is a limited number of commercial products based on this technology, and for larger market penetration an improvement of the technology must be achieved. To advance thermochemical heat storage systems, one has to pay particular attention to studying the processes occurring inside the reactors. For the investigation of the sorption processes with further optimization of the reactor design, a local numerical model of the reactor, carefully validated at the local and global scales, is of significant importance. In the present study, we developed a three dimensional local model of a thermochemical reactor that utilizes ammonia sorption on solid SrCl2. This model simulates the effects of the chemical reaction, heat transfer, and mass transfer separately, and this is its main difference from already existing SrCl2-ammonia models. For the model validation, we used neutron radiography, an alternative to the conventional techniques, i.e., temperature and flowrate measurements. In contrast to these, neutron radiography allows following the state of the reactive bed not for a discrete number of points but via a 2D map. The results of the study demonstrate that the model developed herein is in a good agreement with the detailed neutron radiography data. Since neutron radiography was used as a validation tool for a numerical model for the first time, the procedure of the comparison between the results from our model and neutron radiography was carefully documented. An additional, successful, validation was provided through temperature and flowrate measurements.

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.

This paper presents, for the first time, full-field dynamic measurements of vapour injection and condensation within a fractured concrete, observed in-operando by means of rapid neutron radiography (acquisition rate of 30 Hz with 87 μ m pixel size). Time-dependant moisture evolution is analysed in terms of equivalent water thickness measurements. We observe that movement of condensed moisture along and transversely to the crack plane is non-monotonic in both space and time, exhibiting occasional sub-second jumps.

International audience; The Callovo Oxfordian clay-rock (COx) is studied in France for the disposal of radioactive waste, because of its extremely low permeability. This host rock is governed by a hydromechanical coupling of high complexity.This paper presents an experimental study into the mechanisms of water uptake in small, unconfined, prismatic specimens of COx, motivated by the comprehension of cracking observed during concrete/COx interface sample preparation. Water uptake is monitored using both x-ray tomography and neutron radiography, the combination of these imaging techniques allowing material deformation and water arrival to be quantified respectively.Given the speed of water entry and crack propagation, relatively fast imaging is required: 5 minute x-ray tomographies and ten-second neutron radiographies are used. In this study, pairs of similar COx samples from the same core are tested separately with each imaging technique. Two different orientations with respect to the core are also investigated. Analysis of the resulting images yields with micro-and macro-scale insights into hydro-mechanical mechanisms to be obtained. This allows the cracking to be interpreted as a rapid breakdown in capillary suction (supposed large both to drying and rebound from in-situ stress state) due to water arrival, which in turn causes a loss of effective stress, allowing cracks to propagate with ease, which in turn deliver water further into the material.