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Neutron imaging is used for direct observation of evolving water–air and deuterated water–normal water exchanges in flow experiments performed on a laboratory-deformed, microporous laminated limestone, an extremely fine-textured rock altered by arrays of superposed fractures generated in a rock mechanics apparatus. The neutron images document significant, evolving, water speed and flow direction variability at the deci-micron scale and spatially complex patterns of both increasing and decreasing water saturation. We infer that capillarity-driven and pressure-driven water movement occurs concurrently, in close proximity and in competition, and that as local and global water saturations evolve these two drivers can change their dominance in both matrix and deformed elements. Thin sections are used to obtain sub-micron resolution SEM images that provide multi-scale information on the textural features’ spatial arrangements. The textural characteristics are consistent with the inferences made from the coarser flow imaging. Alternating lamina types provide the primary lithological heterogeneity, while the experimentally created deformations lead to quasi-planar zones of highly comminuted matrix and fracture-like voids, each with lengths ranging from sub-mm to cm. Together deformation features delineate a partially connected array. The interplay between fluid movement through deformation features, and flow into (and out of) the laminae, implies near-equivalence of local driving pressure- and capillary-related energies, with subtle shifts in this balance as water saturation increases. The insights gained invite a re-examination of common rules-of-thumb for multi-phase fluid flow often adopted in fractured, low-permeability microporous rocks.

The most commonly used screens for neutron imaging consist of 6LiF + ZnS. This type of screen yields the highest light output per detected neutron. For high resolution, gadolinium oxysulfide (GOS, Gadox) screens are employed, which have a much higher detection efficiency, but a light output so much lower than LiF + ZnS that measurements are often limited by photon statistics. Historically, screens using boron as a neutron-sensitive material have not been very successful. However, a new preparation method was introduced recently that produces light output higher than Gadox with detection efficiency greater than LiF + ZnS. Measurements of these new borated screens were performed at the NeXT facility at ILL, Grenoble, in comparison to a high resolution Gadox screen.

Refractory castables are a promising alternative to shaped products when considering its potential for reducing direct and indirect carbon dioxide emissions. However, their drying stage is usually an overconservative and long process that refrains the share of green potential of this class of refractories. To reduce the drying times, a throughout understanding of its fundamental mechanisms is required. Various studies have relied on indirect measurements of properties at laboratory conditions that are far from the industrial context. Others made use of sensors which present technical limitations and also affect the local readings. Thus, the current work depicts the use of neutron tomography as a valuable tool to study the drying of refractories, especially by using a ceramic casing which is proposed for providing unidirectional drying. Finally, this setup is also used to explore the effect of different heating rates on the drying of monolithics.

Dry cathode operation is a desired operation mode in anion-exchange membrane water electrolyzers to minimize contamination of the generated hydrogen. However, water management under such operation conditions makes it challenging to maintain reliable performance and durability. Here, we utilize high-resolution

Water significantly influences the mechanical behaviour of all granular materials but none as much as hygroscopic amorphous particles. With sufficiently high water content, particles can swell, agglomerate and their mechanical properties can be reduced, having direct effects on the macroscopic response of the material. In the food and pharmaceutical industry this can cause loss of product functionality. Despite their relevance, very little is known about the microscopic processes that induce these phenomena. Previous studies focused on single particle behaviour, the strength of agglomerated particles and the material flowability, leaving unexplored the link connecting the particle behaviour and the bulk response. This experimental study aims to investigate this aspect with quantitative measurements at both particle and macroscopic scales. A sample of fine couscous is exposed to a high relative humidity (RH) air flow, while being subjected to oedometric conditions, in order to reproduce the storage-silo conditions. In the meantime, X-ray tomographies are acquired continuously and the resulting images are analysed. The designed spatial resolution allows each particle of the sample to be identified and tracked, allowing volumetric evolution to be compared to the properties of the whole sample. The analysis reveals a dilation-compaction macroscopic behaviour, a result of the competition between the particle swelling and the higher deformability as the water content increases. The number, orientations and inter-particle contacts are computed. Their area is related to the applied boundary conditions, and is found to be consistent with the particle swelling and dependent on the applied stress direction.

Due to their great performance and ease of installation, refractory castables are common ground materials to enable high temperature processes. However, their fully operational condition is slowed down by the gradual drying stage required. Therefore, better understanding of the moisture transport involved is essential to improve their efficiency and reduce the likelihood of explosive spalling events due to vapor pressurization. Neutron tomography provides a relevant inner view of the moisture distribution across a sample and its evolution over time. In this work, the effect of the heating rate on moisture clog was investigated and compared with available laboratory and industrial observations. It was found out that higher heating rates resulted in a faster and longer lasting water accumulation ahead of the drying front, in agreement with other macroscopic studies and explaining the common reasoning behind using slower heating rates and safer industrial operations. This study highlights the potential of neutron imaging for the ongoing effort to maximize the efficiency of refractory castables drying process by controlling the moisture accumulation without exclusively relying on slower heating rates. &nbsp

Nakhlite meteorites are igneous rocks from Mars that were aqueously altered ~630 million years ago. Hydrothermal systems on Earth are known to provide microhabitats; knowledge of the extent and duration of these systems is crucial to establish whether they could sustain life elsewhere in the Solar System. Here, we explore the three-dimensional distribution of hydrous phases within the Miller Range 03346 nakhlite meteorite using nondestructive neutron and x-ray tomography to determine whether alteration is interconnected and pervasive. The results reveal discrete clusters of hydrous phases within and surrounding olivine grains, with limited interconnectivity between clusters. This implies that the fluid was localized and originated from the melting of local subsurface ice following an impact event. Consequently, the duration of the hydrous alteration was likely short, meaning that the martian crust sampled by the nakhlites could not have provided habitable environments that could harbor any life on Mars during the Amazonian.

The electrochemical reduction of CO2 is a pivotal technology for the defossilization of the chemical industry. Although first pilot-scale electrolyzers exist, water management and salt precipitation remain a major hurdle to long-term operation. In this work, we present the first high resolution neutron imaging (6 µm) of a zero-gap CO2 electrolyzer to uncover water distribution and salt precipitation under application-relevant operating conditions (200 mA cm− 2 at 2.8 V with a Faraday efficiency for CO of 99%). Precipitated salts penetrating the cathode gas diffusion layer can be observed, which are believed to block the CO2 gas transport and are therefore the major cause for the commonly observed decay in Faraday efficiency. Neutron imaging further shows higher carbonate accumulation under the cathode channel of the flow field compared to the land. In fact, a higher local reaction rate under the land compared to the channel can be estimated from the gas bubble generation on the opposing anode side.

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.

Structural failure of concrete buildings on fire and complete destruction of the monolithic refractory lining during their drying stage are dangerous examples of the effect of explosive spalling on partially saturated porous media. Several observations in both cases indicated the presence of moisture accumulation ahead of the drying front, which are in tune with the most common theories on the explosive spalling of concrete. Previous studies have shown evidence of the existence of this phenomenon, however, they were biased by artifacts and experimental limitations (such as the beam hardening effect and changes in the microstructure of the material due to the presence of pressure and temperature sensors). In the current work, rapid neutron tomography was used to investigate thein-operandodrying behavior of a high-alumina refractory castable, proposing a novel experimental layout aimed at a truly one-dimensional drying front. This setup provided more realistic boundary conditions, such as the behavior of a larger wall heated from one of its sides, while also preventing some nonphysical artifacts (notably beam hardening). By eliminating these aspects, a direct proof that moisture accumulates ahead of the drying front was obtained. This work also lays the basis for further studies focusing on the response sensitivity analysis to boundary conditions and other parameters (e.g., heating rates and properties of the sample related to the moisture clog formation), as well as useful data for the validation and characterization stages of numerical models of partially saturated porousmedia.

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.

In this work, a new dual modality monitoring technique is presented to demonstrate its interest to investigate the salt precipitation dynamics induced by gas flow-through drying. It consists of imaging simultaneously a core flood using both Neutron and X-ray beams. A method to calibrate and process the two signals is presented. It takes advantage of the difference in attenuation between the two ionizing radiations to quantify the different phase saturations and compositions as well as the reduction of porosity caused by salt precipitation. A set of experiments has been conducted at the NeXT-Grenoble beamline of the Institute Laue-Langevin facilities (ILL, France). Experiments were conducted on a homogeneous rock sample of Bentheimer sandstone using dry nitrogen and a 100 g/L KBr brine. The two first experiments aimed to calibrate the dual modality for the different phases. The last two experiments have been conducted with a brine capillary contact maintained at the gas outlet. Experimental data have given new insights into the organization of the three phases (the brine, the gas, and the precipitated salt) when a salt bank is formed in the sample. These quantities computed using dual-modality imaging show great similarities with published work. The salt accumulation was used to estimate the flow rate of brine pumped through the capillary contact to compensate for the brine evaporation in the gas phase. Observations have shown that a reduction of the initial porosity in some sections of the sample by 12–14% was enough to trigger a gas draw-down characterized by the migration of the salt toward the gas inlet. In some conditions (low gas inlet pressure for example), the rise of the water could be fast enough to form a second salt bank higher in the sample. It has been observed that the formation of the second salt bank could spread the precipitated salt in a less damaging configuration for the gas flow, triggering a phase of gas build-up characterized by the withdrawal of the water. These phases of gas draw-down and build-up could alternate until the sample clogs.

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.

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...

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)

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 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.

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.

Dissolution of porous media introduces a positive feedback between fluid transport and chemical reactions at mineral surfaces leading to the formation of pronounced wormhole-like channels. While the impact of flow rate and reaction rate on the shapes of the wormholes is now well understood, much less is known about the dynamics of their propagation. In this study we capture the evolution of wormholes and their effects on flow patterns by in-situ X-ray microCT imaging of dissolving limestone cores. 4D tomography allows us in particular to correlate the permeability changes in a dissolving core with the advancement of the tip position of the wormhole. Surprisingly, we find that the relation between the two is highly nonlinear, with extensive periods of relatively fast growth of the wormhole which is nevertheless not reflected in any significant change in the overall permeability. We hypothesize that this is caused by the presence of highly cemented regions in the core which act as permeability barriers for the flow. The presence of such regions is confirmed by a detailed analysis of the pore geometry based on the tomographic data. The results demonstrate that the analysis of the wormhole dynamics in 4d tomography can be used to probe the internal structure of the rock.

Several granular materials are hydro-sensitive, i.e., contact with water severely affects their morphology and mechanical behaviour. To this broad class belong a series of materials of great relevance for the pharmaceutical and food industry. Former studies have been conducted on the effect that moisture or humidity have on granular flow or on the individual grain mechanical response, but the processes occurring at the microlevel and their influence on the overall granular packing behaviour is yet to be fully understood. This study presents an experimental investigation of the response of a water-sensitive material (couscous) exposed to high relative humidity (97%). 4D (3D plus time) x-ray tomographies were acquired in operando. A data treatment approach based on Dicrete Digital Image Correlation (dDIC) is developed and detailed here. This allows for following each individual grain throughout the 4+ days of the humidification test. This, in turn, allows the study of the interand intra-granular strain, which is particularly pronounced in water sensitive materials. The expansion of the individual grains also severely affects the contact network, whose evolving properties are here analysed and correlated to the macroscopic (sample-scale) deformation.

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.

Spam, the Software for the Practical Analysis of Materials is a Python library that has evolved to cover needs of data analysis from 3D x-ray tomography work and correlated random fields with mechanical applications. Spam is first and foremost a measurement package that extends the extremely convenient framework of NumPy and SciPy by providing or accelerating tools for the material- science/mechanics oriented analysis of 2D images or 3D volumes representing field measurements. Typical uses are either the measurement of displacements fields between images of a deforming sample from which strains can be computed, or the characterisation of a particular microstructure (correlation length or particle orientation). The package is organised into a library of Python tools which are expected to be used in user-written scripts and a number of more sophisticated standalone scripts. Please see the online documentation. Spam is developed on a git repository hosted at Université Grenoble Alpes. This deposit is the version 0.5.2 that was reviewed and accepted on the Journal of Open Source Software

Dissolution of porous media is a complex process involving nonlinear couplings between flow, transport, the evolving geometry of the media, and the process of dissolution itself. In some cases these couplings lead to the formation of intricate patterns, the characteristics of which depend strongly on flow, mineral dissolution rate, and initial pore space geometry. In particular, finger-like channels, termed "wormholes", are spontaneously formed where the majority of flow is focused. Capturing the dynamics of wormhole growth has so far been largely limited to numerical models, with few studies observing their time evolution in real rocks. In this study we capture the dynamics of both wormhole growth and their alteration of flow in the rock by placing the experiment within neutron and X-Ray tomographs and scanning while actively dissolving limestone cores. To observe the evolution of wormhole geometry limestone samples are dissolved in a cell translucent to X-Rays and neutrons. For each experiment a high (30-35 micrometer) resolution scan was taken of the initial sample geometry, as well as the geometry after dissolution. During acidization tomography was performed at 60-70 micrometer resolution with acquisition times ranging from three to six minutes. For several experiments dissolution was paused and and a contrasting agent injected to visualize the flow field within the sample. Flow field experiments were performed with neutron tomography by first injecting heavy water, followed by light water as the contrast agent, and with X-Ray tomography by injection a solution of potassium iodide into light water. Results of dissolution experiments show that wormhole growth can be tracked at sufficiently high spatial and temporal resolution to measure changes to the pore space.These experiments highlight the importance of the near-tip region on the dynamics of wormhole propagation. In particular, focusing of the flow is shown to take place not only within the wormhole but also significantly (>5mm) into the porous region past the wormhole tip. These "virtual channels" link the tip with the neighboring regions of high porosity. Several such virtual channels can exist, indicating potential paths of further growth, and demonstrate the strong coupling of flow and geometry evolution. Additionally, we observe a dramatic dependence of the dissolution patterns on the initial pore structure, in particular the total initial porosity, distribution of pore sizes and connectivity of the pore space. In pore spaces with poor connectivity and low porosity the wormholes tend to be very tortuous and thin. Such wormholes advance through rapid, almost discontinuous jumps, guided by the above-described pre-focusing mechanism. On the other hand, the advancement of a wormhole in a well-connected rock is much more diffuse, controlled by merging between neighboring pore spaces.

Subsurface activities, such as energy production or geo-storage, affect the natural equilibrium of the reservoir and surrounding geological system. Fluid production from porous sandstones, for example, is often associated with reservoir compaction and induced seismicity, such as seen in the Groningen Gas Field. Production-induced stress changes lead to compaction by elastic and inelastic mechanisms. Partitioning between elastic and inelastic processes control the energy budget available for driving seismogenic events. To predict the amount of inelastic strain, it is key to identify the microscopic mechanisms controlling it. One of the current hypotheses is that micro-strains are accommodated by localized compaction of inter-granular clay films. In contrast to sandstones, claystones offer potential both as source rocks for shale gas and containment for the storage of radioactive waste and CO2. It is known that fluid flow in intact and fractured claystones is slow due to pore throats below 10 nm. However, it is unclear whether fractured shales contain a hierarchy of multi-scale highways and byways for fluid transport that is either poorly connected or more easily cross-linked and stable under in-situ conditions. Depending on how fractures change due to in-situ conditions, the shales may have a high potential as barriers in geo-storage systems, or they are of interest in relation to energy production.This leads to two widely different research questions:How do sandstones compact due to changing stress conditions? How do fractures influence fluid flow in shales under in-situ stress conditions? Despite the distance between these research questions, both can be addressed using in-situ imaging. We have developed a compaction cell and a fluid flow cell to perform experiments at the D50/NeXT beamline of the Institut Laue-Langevin in Grenoble, France. Here, combined X-ray and neutron imaging is possible.With the compaction cell, sandstone samples from the Groningen gas field were uniaxially compacted to axial stresses of 45 MPa. At different intervals, 3D neutron and X-ray computed tomography scans were taken. As such, 4D representations (3D volumetric + time) of the in-situ changes were obtained using both neutron and X-ray tomography. The X-ray imaging allows a thorough inspection of the grain-scale deformation of the sample, while the neutron imaging highlights the changes in porosity and gives an indication of the role of clay films.With the fluid flow cell, fractured samples of the Whitby mudstone were subjected to fluid flow under different hydrostatic pressures. The flow path evolution within the sample was visualized using neutron radiography, giving an indication of the differences between fracture and matrix permeability.In this contribution, we will show preliminary results of four experiments performed at the D50/NeXT beamline in October 2019. We will discuss the applicability of using neutron imaging to study grain-scale processes occurring in compacting sandstone, as well as for understanding the fluid pathways in clay-rich shales, with direct implications for energy production and geo-storage.

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.