Catastrophic failure of brittle rocks is important in managing risk associated with system‐sized material failure. Such failure is caused by nucleation, growth, and coalescence of microcracks that spontaneously self‐organize along localized damage zones under compressive stress. Here we present X‐ray microtomography observations that elucidate the in situ micron‐scale processes, obtained from novel tri‐axial compression experiments conducted in a synchrotron. We examine the effect of microstructural heterogeneity in the starting material (Ailsa Craig microgranite; known for being virtually crack‐free) on crack network evolution and localization. To control for heterogeneity, we introduced a random nanoscale crack network into one sample by thermal stressing, leaving a second sample as‐received. By assessing the time‐dependent statistics of crack size and spatial distribution, we test the hypothesis that the degree of starting heterogeneity influences the order and predictability of the phase transition between intact and failed states. We show that this is indeed the case at the system‐scale. The initially more heterogeneous (heat‐treated) sample showed clear evidence for a second‐order transition: inverse power law acceleration in correlation length with a well‐defined singularity near failure and distinct changes in the scaling exponents. The more homogeneous (untreated) sample showed evidence for a first‐order transition: exponential increase in correlation length associated with distributed damage and unstable crack nucleation ahead of abrupt failure. In both cases, anisotropy in the initial porosity dictated the fault orientation, and system‐sized failure occurred when the correlation length approached the grain size. These results have significant implications for the predictability of catastrophic failure in different materials.

An X-ray transparent experimental triaxial rock deformation apparatus, here named `Mjölnir', enables investigations of brittle-style rock deformation and failure, as well as coupled thermal, chemical and mechanical processes relevant to a range of Earth subsurface environments. Designed to operate with cylindrical samples up to 3.2 mm outside-diameter and up to 10 mm length, Mjölnir can attain up to 50 MPa confining pressure and in excess of 600 MPa axial load. The addition of heaters extends the experimental range to temperatures up to 140°C. Deployment of Mjolnir on synchrotron beamlines indicates that full 3D datasets may be acquired in a few seconds to a few minutes, meaning full 4D investigations of deformation processes can be undertaken. Mjölnir is constructed from readily available materials and components and complete technical drawings are included in the supporting information.

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In many geoscientific, material science, and engineering applications it is of importance to estimate a representative bulk seismic velocity of materials or to locate the source of recorded seismic or acoustic waves. Such estimates are necessary in order to interpret industrial seismic and earthquake seismological data, for example, in nondestructive evaluation and monitoring of structural materials, and as an input to rock physics models that predict other parameters of interest. Bulk velocity is commonly estimated in laboratories from the time of flight of the first‐arriving wave between a source and a receiver, assuming a linear raypath. In heterogeneous media, that method provides biased estimates of the bulk velocity, and of derived parameters such as temporal velocity changes or the locations of acoustic emissions. We show that coda wave interferometry (CWI) characterizes changes in the bulk properties of scattering media far more effectively on the scale of laboratory rock samples. Compared to conventional methods, CWI provides significant improvements in both accuracy and precision of estimates of velocity changes, and distances between pairs of acoustic sources, remaining accurate in the presence of background noise, and when source location and velocity perturbations occur simultaneously. CWI also allows 3‐D relative locations of clusters of acoustic emissions to be estimated using only a single sensor. We present a method to use CWI to infer changes in both P and S wave velocities individually. These innovations represent significant improvements in our ability to characterize the evolution of properties of media for a variety of applications.

Catastrophic failure in brittle, porous materials initiates when smaller-scale fractures localise along an emergent fault zone in a transition from stable crack growth to dynamic rupture. Due to the rapid nature of this critical transition, the precise micro-mechanisms involved are poorly understood and difficult to image directly. Here, we observe these micro-mechanisms directly by controlling the microcracking rate to slow down the transition in a unique rock deformation experiment that combines acoustic monitoring (sound) with contemporaneous in-situ x-ray imaging (vision) of the microstructure. We find seismic amplitude is not always correlated with local imaged strain; large local strain often occurs with small acoustic emissions, and vice versa. Local strain is predominantly aseismic, explained in part by grain/crack rotation along an emergent shear zone, and the shear fracture energy calculated from local dilation and shear strain on the fault is half of that inferred from the bulk deformation.