BIB-SEM characterization of pore space morphology and distribution in postmature to overmature samples from the Haynesville and Bossier Shales

Abstract Four Haynesville Shale and four Bossier Shale samples were investigated using a combination of Scanning Electron Microscopy (SEM) and Broad Ion Beam (BIB) polishing. This approach enables the microstructure and porosity to be studied down to the mesopore size ( r in the Haynesville Shale to 1.79–2.26 VR r in the Bossier Shale. This variety within the samples enabled us to study controls on the porosity distribution in these shales. Visible pores exist as intraparticle pores mainly in carbonate grains and pyrite framboids and as interparticle pores, mainly in the clay-rich matrix. Pores in organic matter show a characteristic porosity with respect to the type of organic matter, which mainly consists of mixtures of amorphous organic matter and minerals, organic laminae and discrete macerals. A clear positive trend of organic-matter porosity with maturity was found. Pore sizes are power law distributed in the range of 4.4 μm to at least 36 nm in equivalent diameter. The differences in power law exponents suggest that a more grain supported, coarse-grained matrix may prevent pores from mechanical compaction. Porosities measured in the BIB cross-sections were significantly lower in comparison to porosities obtained by Mercury Intrusion Porosimetry (MIP). This difference is mainly attributed to the different resolution achieved with BIB-SEM and MIP and type of pore network. Extrapolation of pore size distributions (PSDs) enables the BIB-SEM porosity to be estimated down to the resolution of the MIP and thus to upscale microstructural observation at the confined space of the BIB-SEM method to bulk porosity measurement. These inferred porosities are in good agreement with the MIP determined porosities, which underpins the assumption that pores segmented in BIB-SEM mosaics are representative of the MIP methodology.

[1]  M. D. Rudnicki,et al.  Organic matter–hosted pore system, Marcellus Formation (Devonian), Pennsylvania , 2013 .

[2]  E. W. Washburn Note on a Method of Determining the Distribution of Pore Sizes in a Porous Material. , 1921, Proceedings of the National Academy of Sciences of the United States of America.

[3]  Daniel M. Jarvie,et al.  Shale Resource Systems for Oil and Gas: Part 1—Shale-gas Resource Systems , 2012 .

[4]  Jason E. Heath,et al.  Pore networks in continental and marine mudstones: Characteristics and controls on sealing behavior , 2011 .

[5]  János Urai,et al.  High-resolution 3D fabric and porosity model in a tight gas sandstone reservoir:A new approach to investigate microstructures from mm- to nm-scale combining argon beam cross-sectioning and SEM imaging , 2011 .

[6]  R. Marc Bustin,et al.  Characterization of gas shale pore systems by porosimetry, pycnometry, surface area, and field emission scanning electron microscopy/transmission electron microscopy image analyses: Examples from the Barnett, Woodford, Haynesville, Marcellus, and Doig units , 2012 .

[7]  János Urai,et al.  BIB-SEM study of the pore space morphology in early mature Posidonia Shale from the Hils area, Germany , 2012 .

[8]  L. Esteban,et al.  Pore network geometry in low permeability argillites from magnetic fabric data and oriented mercury injections , 2006 .

[9]  William J. Bosl,et al.  Permeability-porosity transforms from small sandstone fragments , 2006 .

[10]  D. Jarvie,et al.  Unconventional shale-gas systems: The Mississippian Barnett Shale of north-central Texas as one model for thermogenic shale-gas assessment , 2007 .

[11]  F. J. Pearson What is the porosity of a mudrock? , 1999, Geological Society, London, Special Publications.

[12]  Roger Wepf,et al.  On the application of focused ion beam nanotomography in characterizing the 3D pore space geometry of Opalinus clay , 2011 .

[13]  F. Pérez-Willard,et al.  Argon broad ion beam tomography in a cryogenic scanning electron microscope: a novel tool for the investigation of representative microstructures in sedimentary rocks containing pore fluid , 2013, Journal of microscopy.

[14]  K. Spikes,et al.  Estimation of reservoir properties of the Haynesville Shale by using rock-physics modelling and grid searching , 2013 .

[15]  G. Frébourg,et al.  Haynesville and Bossier mudrocks: A facies and sequence stratigraphic investigation, East Texas and Louisiana, USA , 2012 .

[16]  R. Littke,et al.  Reflectance of dispersed vitrinite in Palaeozoic rocks with and without cleavage: Implications for burial and thermal history modeling in the Devonian of Rursee area, northern Rhenish Massif, Germany , 2012 .

[17]  Marco Herwegh,et al.  Quantitative analysis of crystal/grain sizes and their distributions in 2D and 3D , 2011 .

[18]  J. Urai,et al.  Pore morphology and distribution in the Shaly facies of Opalinus Clay (Mont Terri, Switzerland): Insights from representative 2D BIB–SEM investigations on mm to nm scale , 2013 .

[19]  Ryan McLin,et al.  Imaging Texture and Porosity in Mudstones and Shales: Comparison of Secondary and Ion-Milled Backscatter SEM Methods , 2010 .

[20]  R. Loucks,et al.  Morphology, Genesis, and Distribution of Nanometer-Scale Pores in Siliceous Mudstones of the Mississippian Barnett Shale , 2009 .

[21]  J. Urai,et al.  In situ characterization of the microstructure and porosity of Opalinus Clay (Mont Terri Rock Laboratory, Switzerland) , 2013 .

[22]  Christopher R. Clarkson,et al.  Pore structure characterization of North American shale gas reservoirs using USANS/SANS, gas adsorption, and mercury intrusion , 2013 .

[23]  J. Schieber,et al.  Common Themes in the Formation and Preservation of Intrinsic Porosity in Shales and Mudstones - Illustrated with Examples Across the Phanerozoic , 2010 .

[24]  Carl H. Sondergeld,et al.  New Pore-scale Considerations for Shale Gas in Place Calculations , 2010 .

[25]  M. Curtis,et al.  Development of organic porosity in the Woodford Shale with increasing thermal maturity , 2012 .

[26]  J. Urai,et al.  A comparative study of representative 2D microstructures in Shaly and Sandy facies of Opalinus Clay (Mont Terri, Switzerland) inferred form BIB-SEM and MIP methods , 2014 .

[27]  B. Horsfield,et al.  Formation of nanoporous pyrobitumen residues during maturation of the Barnett Shale (Fort Worth Basin) , 2012 .

[28]  Bruce E. Herbert,et al.  Permeability of illite-bearing shale: 1. Anisotropy and effects of clay content and loading , 2004 .

[29]  R. Loucks,et al.  Preliminary Classification of Matrix Pores in Mudrocks , 2010 .

[30]  Stephen C. Ruppel,et al.  Spectrum of pore types and networks in mudrocks and a descriptive classification for matrix-related mudrock pores , 2012 .

[31]  B Münch,et al.  Three‐dimensional analysis of porous BaTiO3 ceramics using FIB nanotomography , 2004, Journal of microscopy.

[32]  R. Littke,et al.  Polyphase thermal evolution in the Infra-Cambrian Ara Group (South Oman Salt Basin) as deduced by maturity of solid reservoir bitumen , 2007 .

[33]  M. Curtis,et al.  Transmission and Scanning Electron Microscopy Investigation of Pore Connectivity of Gas Shales on the Nanoscale , 2011 .

[34]  János Urai,et al.  Morphology of the pore space in claystones - evidence from BIB/FIB ion beam sectioning and cryo-SEM observations , 2009 .

[35]  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 .

[36]  P. Flemings,et al.  Insights into pore-scale controls on mudstone permeability through resedimentation experiments , 2011 .

[37]  Lorenz Holzer,et al.  Contradicting Geometrical Concepts in Pore Size Analysis Attained with Electron Microscopy and Mercury Intrusion , 2008 .

[38]  A. Hildenbrand,et al.  Investigation of the morphology of pore space in mudstones—first results , 2003 .

[39]  Daniel J. Soeder,et al.  Porosity and Permeability of Eastern Devonian Gas Shale , 1988 .

[40]  Christopher R. Clarkson,et al.  Reservoir Engineering for Unconventional Reservoirs: What Do We Have to Consider? , 2011 .

[41]  Dmitriy Silin,et al.  Analysis of Chalk Petrophysical Properties by Means of Submicron-Scale Pore Imaging and Modeling , 2007 .

[42]  J. Urai,et al.  Variations in the morphology of porosity in the Boom Clay Formation: insights from 2D high resolution BIB-SEM imaging and Mercury injection Porosimetry , 2013, Netherlands Journal of Geosciences - Geologie en Mijnbouw.

[43]  M. Curtis,et al.  Structural Characterization of Gas Shales on the Micro- and Nano-Scales , 2010 .

[44]  Thomas E. Ewing,et al.  Geologic analysis of the Upper Jurassic Haynesville Shale in east Texas and west Louisiana , 2011 .

[45]  M. Curtis,et al.  Microstructural investigation of gas shales in two and three dimensions using nanometer-scale resolution imaging , 2012 .

[46]  M. Curtis,et al.  Investigation of the Relationship Between Organic Porosity and Thermal Maturity in The Marcellus Shale , 2011 .