Quantifying the precursors to brittle failure in rocks using synchrotron imaging and machine learning

Author(s):  
Francois Renard ◽  
Jessica McBeck ◽  
Benoît Cordonnier

<p>Predicting the onset of system-size failure in rocks represents a fundamental goal in assessing earthquake hazard. On the field, seismological, geodetic and other monitoring data may record precursors to earthquakes. In laboratory experiments, such precursors often rely on monitoring acoustic emissions and this technique has some limitations in terms of spatial resolution and the lack of detection of aseismic strain. To overcome these challenges, we have performed a series of forty rock deformation experiments where we imaged, using synchrotron X-ray microtomography, rock samples as they deformed until brittle failure, at in situ conditions of pressure, high spatial micrometer spatial resolution, and through time. On the one hand, direct processing of the X-ray tomograms allow visualizing how precursory microfractures nucleate, grow, and coalesce until failure. From these data, we propose to characterize brittle failure as a critical phase transition, with evidence of several power-laws that characterize fracture growth. On the other hand, digital volume correlation techniques quantify the evolution of the local strain field inside each sample. We analysed the statistical properties of these strain fields using several machine learning techniques to predict the main parameters that control fracture growth (length, volume, shape, distance to the nearest fracture), and the features of the strain field that best predict the distance to failure. Our rock deformation experimental results show that, under laboratory conditions, precursors to brittle deformation exist. These precursors show predictable evolution when approaching system-size brittle deformation and we demonstrate that specific components of the strain field characterize this evolution to failure.</p>

2004 ◽  
Vol 126 (1) ◽  
pp. 18-24 ◽  
Author(s):  
Wenwu Zhang ◽  
Y. Lawrence Yao ◽  
I. C. Noyan

Microscale Laser Shock Peening (LSP) is a technique that can be potentially applied to manipulate the residual stress distributions in metal film structures and thus improve the reliability of micro-devices. This paper reports high-spatial-resolution characterization of shock treated copper thin films on single-crystal silicon substrates, where scanning x-ray microtopography is used to map the relative variation of the stress/strain field with micron spatial resolution, and instrumented nanoindentation is applied to measure the distribution of hardness and deduce the sign of the stress/strain field. The measurement results are also compared with 3-D simulation results. The general trends in simulations agree with those from experimental measurements. Simulations and experiments show that there is a near linear correlation between strain energy density at the film-substrate interface and the X-ray diffraction intensity contrast.


Author(s):  
Neelima Kandula ◽  
Jessica McBeck ◽  
Benoît Cordonnier ◽  
Jérôme Weiss ◽  
Dag Kristian Dysthe ◽  
...  

AbstractUnderstanding the mechanisms of strain localization leading to brittle failure in reservoir rocks can shed light on geomechanical processes such as porosity and permeability evolution during rock deformation, induced seismicity, fracturing, and subsidence in geological reservoirs. We perform triaxial compression tests on three types of porous reservoir rocks to reveal the local deformation mechanisms that control system-size failure. We deformed cylindrical samples of Adamswiller sandstone (23% porosity), Bentheim sandstone (23% porosity), and Anstrude limestone (20% porosity), using an X-ray transparent triaxial deformation apparatus. This apparatus enables the acquisition of three-dimensional synchrotron X-ray images, under in situ stress conditions. Analysis of the tomograms provide 3D distributions of the microfractures and dilatant pores from which we calculated the evolving macroporosity. Digital volume correlation analysis reveals the dominant strain localization mechanisms by providing the incremental strain components of pairs of tomograms. In the three rock types, damage localized as a single shear band or by the formation of conjugate bands at failure. The porosity evolution closely matches the evolution of the incremental strain components of dilation, contraction, and shear. With increasing confinement, the dominant strain in the sandstones shifts from dilative strain (Bentheim sandstone) to contractive strain (Adamswiller sandstone). Our study also links the formation of compactive shear bands with porosity variations in Anstrude limestone, which is characterized by a complex pore geometry. Scanning electron microscopy images indicate that the microscale mechanisms guiding strain localization are pore collapse and grain crushing in sandstones, and pore collapse, pore-emanated fractures and cataclasis in limestones. Our dynamic X-ray microtomography data brings unique insights on the correlation between the evolutions of rock microstructure, porosity evolution, and macroscopic strain during the approach to brittle failure in reservoir rocks.


Author(s):  
R. Hutchings ◽  
I.P. Jones ◽  
M.H. Loretto ◽  
R.E. Smallman

There is increasing interest in X-ray microanalysis of thin specimens and the present paper attempts to define some of the factors which govern the spatial resolution of this type of microanalysis. One of these factors is the spreading of the electron probe as it is transmitted through the specimen. There will always be some beam-spreading with small electron probes, because of the inevitable beam divergence associated with small, high current probes; a lower limit to the spatial resolution is thus 2αst where 2αs is the beam divergence and t the specimen thickness.In addition there will of course be beam spreading caused by elastic and inelastic interaction between the electron beam and the specimen. The angle through which electrons are scattered by the various scattering processes can vary from zero to 180° and it is clearly a very complex calculation to determine the effective size of the beam as it propagates through the specimen.


Author(s):  
J. R. Michael

X-ray microanalysis in the analytical electron microscope (AEM) refers to a technique by which chemical composition can be determined on spatial scales of less than 10 nm. There are many factors that influence the quality of x-ray microanalysis. The minimum probe size with sufficient current for microanalysis that can be generated determines the ultimate spatial resolution of each individual microanalysis. However, it is also necessary to collect efficiently the x-rays generated. Modern high brightness field emission gun equipped AEMs can now generate probes that are less than 1 nm in diameter with high probe currents. Improving the x-ray collection solid angle of the solid state energy dispersive spectrometer (EDS) results in more efficient collection of x-ray generated by the interaction of the electron probe with the specimen, thus reducing the minimum detectability limit. The combination of decreased interaction volume due to smaller electron probe size and the increased collection efficiency due to larger solid angle of x-ray collection should enhance our ability to study interfacial segregation.


Author(s):  
Brian Cross

A relatively new entry, in the field of microscopy, is the Scanning X-Ray Fluorescence Microscope (SXRFM). Using this type of instrument (e.g. Kevex Omicron X-ray Microprobe), one can obtain multiple elemental x-ray images, from the analysis of materials which show heterogeneity. The SXRFM obtains images by collimating an x-ray beam (e.g. 100 μm diameter), and then scanning the sample with a high-speed x-y stage. To speed up the image acquisition, data is acquired "on-the-fly" by slew-scanning the stage along the x-axis, like a TV or SEM scan. To reduce the overhead from "fly-back," the images can be acquired by bi-directional scanning of the x-axis. This results in very little overhead with the re-positioning of the sample stage. The image acquisition rate is dominated by the x-ray acquisition rate. Therefore, the total x-ray image acquisition rate, using the SXRFM, is very comparable to an SEM. Although the x-ray spatial resolution of the SXRFM is worse than an SEM (say 100 vs. 2 μm), there are several other advantages.


Author(s):  
J. Zhang ◽  
D.B. Williams ◽  
J.I. Goldstein

Analytical sensitivity and spatial resolution are important and closely related factors in x-ray microanalysis using the AEM. Analytical sensitivity is the ability to distinguish, for a given element under given conditions, between two concentrations that are nearly equal. The analytical sensitivity is directly related to the number of x-ray counts collected and, therefore, to the probe current, specimen thickness and counting time. The spatial resolution in AEM analysis is determined by the probe size and beam broadening in the specimen. A finer probe and a thinner specimen give a higher spatial resolution. However, the resulting lower beam current and smaller X-ray excitation volume degrade analytical sensitivity. A compromise must be made between high spatial resolution and an acceptable analytical sensitivity. In this paper, we show the necessity of evaluating these two parameters in order to determine the low temperature Fe-Ni phase diagram.A Phillips EM400T AEM with an EDAX/TN2000 EDS/MCA system and a VG HB501 FEG STEM with a LINK AN10 EDS/MCA system were used.


Author(s):  
Matthew T. Johnson ◽  
Ian M. Anderson ◽  
Jim Bentley ◽  
C. Barry Carter

Energy-dispersive X-ray spectrometry (EDS) performed at low (≤ 5 kV) accelerating voltages in the SEM has the potential for providing quantitative microanalytical information with a spatial resolution of ∼100 nm. In the present work, EDS analyses were performed on magnesium ferrite spinel [(MgxFe1−x)Fe2O4] dendrites embedded in a MgO matrix, as shown in Fig. 1. spatial resolution of X-ray microanalysis at conventional accelerating voltages is insufficient for the quantitative analysis of these dendrites, which have widths of the order of a few hundred nanometers, without deconvolution of contributions from the MgO matrix. However, Monte Carlo simulations indicate that the interaction volume for MgFe2O4 is ∼150 nm at 3 kV accelerating voltage and therefore sufficient to analyze the dendrites without matrix contributions.Single-crystal {001}-oriented MgO was reacted with hematite (Fe2O3) powder for 6 h at 1450°C in air and furnace cooled. The specimen was then cleaved to expose a clean cross-section suitable for microanalysis.


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