Synchrotron tomographic quantification of strain and fracture during simulated thermal maturation of an organic‐rich shale, UK Kimmeridge Clay

Analyzing the development of fracture networks in shale is important to understand both hydrocarbon migration pathways within and from source rocks and the effectiveness of hydraulic stimulation upon shale reservoirs. Here we use time-resolved synchrotron X-ray tomography to quantify in four dimensions (3-D plus time) the development of fractures during the accelerated maturation of an organic-rich mudstone (the UK Kimmeridge Clay), with the aim of determining the nature and timing of crack initiation. Electron microscopy (EM, both scanning backscattered and energy dispersive) was used to correlatively characterize the microstructure of the sample preheating and postheating. The tomographic data were analyzed by using digital volume correlation (DVC) to measure the three-dimensional displacements between subsequent time/heating steps allowing the strain fields surrounding each crack to be calculated, enabling crack opening modes to be determined. Quantification of the strain eigenvectors just before crack propagation suggests that the main mode driving crack initiation is the opening displacement perpendicular to the bedding, mode I. Further, detailed investigation of the DVC measured strain evolution revealed the complex interaction of the laminar clay matrix and the maximum principal strain on incipient crack nucleation. Full field DVC also allowed accurate calculation of the coefficients of thermal expansion (8 × 10−5/°C perpendicular and 6.2 × 10−5/°C parallel to the bedding plane). These results demonstrate how correlative imaging (using synchrotron tomography, DVC, and EM) can be used to elucidate the influence of shale microstructure on its anisotropic mechanical behavior.

[1]  G. Lash,et al.  Marcellus Shale Play ’ s Vast Resource Potential Creating Stir In Appalachia , 2008 .

[2]  Changes in microstructure and mineralogy of organic-rich shales caused by heating , 2015 .

[3]  Pascal Wallisch,et al.  MATLAB for Neuroscientists: An Introduction to Scientific Computing in MATLAB , 2008 .

[4]  David H. Eberly,et al.  Geometric Tools for Computer Graphics , 2002 .

[5]  Stefan Schouten,et al.  Preservation of carbohydrates through sulfurization in a Jurassic euxinic shelf sea: Examination of the Blackstone Band TOC cycle in the Kimmeridge Clay Formation, UK , 2006 .

[6]  Zdeněk P. Baažant Finite strain generalization of smallstrain constitutive relations for any finite strain tensor and additive volumetric-deviatoric split , 1996 .

[7]  T. Engelder,et al.  Preferential jointing of Upper Devonian black shale, Appalachian Plateau, USA: evidence supporting hydrocarbon generation as a joint-driving mechanism , 2004, Geological Society, London, Special Publications.

[8]  M. G. Teixeira,et al.  Microfracturing during primary migration in shales , 2017 .

[9]  Jon E. Olson,et al.  Predicting fracture swarms — the influence of subcritical crack growth and the crack-tip process zone on joint spacing in rock , 2004, Geological Society, London, Special Publications.

[10]  4D imaging of fracturing in organic-rich shales during heating , 2011, 1101.2295.

[11]  A. Desprairies,et al.  Clay diagenesis in organic-rich cycles from the Kimmeridge Clay Formation of Yorshire (G.B.): implication for palaeoclimatic interpretations , 1995 .

[12]  Peter D. Lee,et al.  Quantifying the Evolution of Soil Fabric during Shearing using Directional Parameters , 2013 .

[13]  Brian K. Bay,et al.  Methods and applications of digital volume correlation , 2008 .

[14]  R. Tyson Variation in marine total organic carbon through the type Kimmeridge Clay Formation (Late Jurassic), Dorset, UK , 2004, Journal of the Geological Society.

[15]  Paul C. Hackley,et al.  The nature of porosity in organic-rich mudstones of the Upper Jurassic Kimmeridge Clay Formation, North Sea, offshore United Kingdom , 2012 .

[16]  A. Doré,et al.  Correlation of the offshore sequences referred to the Kimmeridge Clay Formation—relevance to the Norwegian sector , 1985 .

[17]  P. Landais,et al.  Effects of pressure on organic matter maturation during confined pyrolysis of Woodford kerogen , 1994 .

[18]  J. Disnar,et al.  Primary control of paleoproduction on organic matter preservation and accumulation in the Kimmeridge rocks of Yorkshire (UK) , 1994 .

[19]  I. Ozkaya A simple analysis of oil-induced fracturing in sedimentary rocks , 1988 .

[20]  G. Team,et al.  Map of assessed shale gas in the United States, 2012 , 2013 .

[21]  C. Packard,et al.  Effect of thermal maturity on elastic properties of kerogen , 2016 .

[22]  Stéphane Roux,et al.  Digital volume correlation analyses of synchrotron tomographic images , 2011 .

[23]  Stefan Schouten,et al.  Controls on the molecular and carbon isotopic composition of organic matter deposited in a Kimmeridgian euxinic shelf sea: Evidence for preservation of carbohydrates through sulfurisation , 1998 .

[24]  Z.-H. Jin,et al.  Subcritical propagation and coalescence of oil‐filled cracks: Getting the oil out of low‐permeability source rocks , 2010 .

[25]  J. Hunt,et al.  Hydrogen porosity in directional solidified aluminium-copper alloys:in situ observation , 1997 .

[26]  A. Coe,et al.  Integrated stratigraphy of the Kimmeridge Clay Formation (Upper Jurassic) based on exposures and boreholes in south Dorset, UK , 2001, Geological Magazine.

[27]  B. Bay,et al.  Digital volume correlation: Three-dimensional strain mapping using X-ray tomography , 1999 .

[28]  P J Withers,et al.  Region‐of‐interest tomography using filtered backprojection: assessing the practical limits , 2011, Journal of microscopy.

[29]  Andreas K. Kronenberg,et al.  Experimental deformation of shale: mechanical properties and microstructural indicators of mechanisms , 1993 .

[30]  S. Derenne,et al.  Electron microscopy and pyrolysis of kerogens from the Kimmeridge Clay Formation, UK: Source organisms, preservation processes, and origin of microcycles , 1995 .

[31]  Peter D. Lee,et al.  Synchrotron Tomographic Characterization of Damage Evolution During Aluminum Alloy Solidification , 2013, Metallurgical and Materials Transactions A.

[32]  J. Olson,et al.  Experimental determination of subcritical crack growth parameters in sedimentary rock , 2001 .

[33]  S. Hergarten,et al.  A model for propagation and concentration of microcracks , 2000 .

[34]  Marco Stampanoni,et al.  A comparative study of X-ray tomographic microscopy on shales at different synchrotron facilities: ALS, APS and SLS , 2012, Journal of synchrotron radiation.

[35]  Andre Phillion,et al.  Quantitative 3D Characterization of Solidification Structure and Defect Evolution in Al Alloys , 2012 .

[36]  Paul Meakin,et al.  A 4D Synchrotron X-Ray-Tomography Study of the Formation of Hydrocarbon- Migration Pathways in Heated Organic-Rich Shale , 2013 .

[37]  C. Gourlay,et al.  Revealing the micromechanisms behind semi-solid metal deformation with time-resolved X-ray tomography , 2014, Nature Communications.

[38]  T. Engelder,et al.  An analysis of horizontal microcracking during catagenesis: Example from the Catskill delta complex , 2005 .

[39]  Christopher Martin,et al.  Regularization methods for inverse problems in x-ray tomography , 2010, Optical Engineering + Applications.

[40]  W. Oschmann Kimmeridge clay sedimentation — A new cyclic model , 1988 .

[41]  E. Faber,et al.  Geochemical Surface Exploration for Hydrocarbons in North Sea , 1984 .

[42]  K. M. Kareh,et al.  Transgranular liquation cracking of grains in the semi-solid state , 2015, Nature Communications.

[43]  Francois Barthelat,et al.  A Novel “Subset Splitting” Procedure for Digital Image Correlation on Discontinuous Displacement Fields , 2010 .

[44]  M. Lebedev,et al.  Microstructural characterisation of organic-rich shale before and after pyrolysis , 2014 .