FIB-SEM and TEM investigations of an organic-rich shale maturation series from the lower toarcian posidonia shale, Germany: Nanoscale pore system and fluid-rock interactions

AAPG Memoir

Volumn , Issue 102, 2013, Pages 53-66

  Bernard, Sylvain ^a   Brown, Leon ^b   Wirth, Richard ^c   Schreiber, Anja ^c   Schulz, Hans Martin ^c   Horsfield, Brian ^c   Aplin, Andrew C ^d   Mathia, Eliza J ^d  

^a UNIVERSITÉ PIERRE ET MARIE CURIE   (France)

^b DURHAM UNIVERSITY   (United Kingdom)

^c GFZ GERMAN RESEARCH CENTRE FOR GEOSCIENCES   (Germany)

^d NEWCASTLE UNIVERSITY   (United Kingdom)

Author keywords

[No Author keywords available]

Indexed keywords

EXSOLUTION; HYDROCARBON GENERATION; MATURATION; MINERALOGY; POROSITY; SCANNING ELECTRON MICROSCOPY; SHALE; THERMAL MATURITY; TOARCIAN; TRANSMISSION ELECTRON MICROSCOPY;

GERMANY;

POSIDONIA;

EID: 84902128628     PISSN: 02718529     EISSN: None     Source Type: Journal    
DOI: 10.1306/13391705M1023583     Document Type: Article

References (88)

1. Ambrose, R. J., R. C. Hartman, M. Diaz-Campos, I. Y. Akkutlu, and C. H. Sondergeld, 2010, New pore-scale considerations for shale gas in place calculations: Proceedings of the North American Unconventional Gas Conference and Exhibition, Society of Petroleum Engineers, SPE Paper 131772,17 p., doi: 10.2118/131772-MS.
2. Bassim, N. D., B. T. de Gregorio, A. L. D. Kylcoyne, K. Scott, T. Chou, S. Wirick, G. D. Cody, and R. M. Stroud, 2012, Minimizing damage during FIB sample preparation of soft materials: Journal of Microscopy, v. 245, no. 3, p. 288-301.
3. Benzerara, K., N. Menguy, F. Guyot, and C. Vanni, 2005, TEM study of a silicate-carbonate-microbe interface prepared by focused ion beam milling: Geochimica et Cosmochimica Acta, v. 69, p. 1413-1422.
4. Bera, B., M. K. Sushanta, and V. Douglas, 2011, Understanding the micro structure of Berea Sandstone by the simultaneous use of micro-computed tomography (micro-CT) and focused ion beam-scanning electron microscopy (FIB-SEM): Micron, v. 42, no. 5, p. 412-418.
5. Bernard, S., K. Benzerara, O. Beyssac, N. Menguy, F. Guyot, G. E. Brown Jr., and B. Goffe, 2007, Exceptional preservation of plant fossils in high-pressure metamorphic rocks: Earth and Planetary Science Letters, v. 262, no. 1-2, p. 257-272.
6. Bernard, S., K. Benzerara, O. Beyssac, G. E. Brown Jr., L. G. Stamm, and P. Duringer, 2009, Ultrastructural and chemical study of modern and fossil sporoderms by scanning transmission x-ray microscopy (STXM): Review of Palaeobotany and Palynology, v. 156, no. 1-2, p. 248-261.
7. Bernard, S., K. Benzerara, O. Beyssac, and G. E. Brown Jr., 2010a, Multiscale characterization of pyritized plant tissues in blueschist fades metamorphic rocks: Geochimica et Cosmochimica Acta, v. 74, p. 5054-5068.
8. Bernard, S., B. Horsfield, H. M. Schulz, A. Schreiber, R. Wirth, T. T. A. Vu, F. Perssen, S. Konitzer, H. Volk, N. Sherwood, and D. Fuentes, 2010b, Multi-scale detection of organic and inorganic signatures provides insights into gas shale properties and evolution: Chemie der Erde-Geochemistry, v. 70, no. 53, p. 119-133.
9. Bernard, S., B. Horsfield, H. M. Schulz, R. Wirth, A. Schreiber, and N. Sherwood, 2012a, Geochemical evolution of organic-rich shales with increasing maturity: A STXM and TEM study of the Posidonia Shale (Lower Toarcian, northern Germany): Marine and Petroleum Geology, v. 31, no. 1, p. 70-89.
10. Bernard, S., R. Wirth, A. Schreiber, H. M. Schulz, and B. Horsfield, 2012b, Formation of nanoporous pyrobi-tumen residues during maturation of the Barnett Shale (Fort Worth Basin): International Journal of Coal Geology, v. 103, p. 3-11.
11. Berner, R. A., 1968, Calcium carbonate concretions formed by the decomposition of organic matter: Science, v. 159, p. 195-197.
12. Berner, R. A., 1984, Sedimentary pyrite formation: An update: Geochimica et Cosmochimica Acta, v. 48, no. 4, p. 605-615.
13. Brock, E, R. J. Parkes, and D. E. G. Briggs, 2006, Experimental pyrite formation associated with decay of plant material: Palaios, v. 21, no. 5, p. 499-506.
14. Curtis, J. B., 2002, Fractured shale-gas systems: AAPG Bulletin, v. 86, no. 11, p. 1921-1938.
15. Curtis, M. E., C. H. Sondergeld, R. J. Ambrose, and C. S. Rai, 2010, Structural characterization of gas shales on the micro- and nano-scales: Proceedings of the Canadian Unconventional Resources and International Petroleum Conference, 'Society of Petroleum Engineers', SPE Paper 137693,15 p., doi: 10.2118/137693-MS.
16. Curtis, M. E., R. J. Ambrose, C. H. Sondergeld, and C. S. Rai, 2011a, Investigation of the relationship between organic porosity and thermal maturity in the Marcellus Shale: Proceedings of the North American Unconventional Gas Conference and Exhibition, Society of Petroleum Engineers, SPE Paper 144370, 4 p., doi:10.2118/144370-MS.
17. Curtis, M. E., R. J. Ambrose, C. H. Sondergeld, and C. S. Rai, 2011b, Transmission and scanning electron microscopy investigation of pore connectivity of gas shales on the nanoscale: Proceedings of the North American Unconventional Gas Conference and Exhibition, Society of Petroleum Engineers, SPE Paper 144391, 10 p., doi:10.2118/144391-MS.
18. Curtis, M. E., R. J. Ambrose, C. H. Sondergeld, and C. S. Rai, 2012, Microstructural investigation of gas shales in two and three dimensions using nanometer-scale resolution imaging: AAPG Bulletin, v. 96, no. 4, p. 665-677.
19. Davis, W. J., Q. Gall, C. W. lefferson, and R. H. Rainbird, 2011, Fluorapatite in the Paleoproterozoic Thelon Basin: Structural-stratigraphic context, in situ ion microprobe U-Pb ages, and fluid-flow history: GSA Bulletin, v. 123, no. 5-6, p. 1056-1073.
20. Desbois, G., J. L. Urai, and P. A. Kukla, 2009, Morphology of the pore space in claystones-evidence from BIB/FIB ion beam sectioning and cryo-SEM observations: Earth Discussion, v. 4, p. 1-19.
21. Desbois, G., J. L. Urai, M. E. Houben, and Y. Sholokhova, 2010, Typology, morphology and connectivity of pore space in claystones from reference site for research using BIB, FIB and cryo-SEM methods: EPJ Web of Conferences, doi: 10.1051/epjconf/20100622005.
22. Dewhurst, D. N., Y. Yang, and A. C. Aplin, 1999, Permeability and fluid flow in natural mudstones: GSL, Special Publications, v. 158, p. 23-43.
23. De Winter, D. A. M., C. T. W. M. Schneijdenberg, M. N. Lebbink, B. Lich, A. J. Verkleij, M. R. Drury, and B. M. Humbel, 2009, Tomography of insulating biological and geological materials using focused ion beam (FIB) sectioning and low-kV BSE imaging: lournal of Microscopy, v. 233, no. 3, p. 372-383.
24. Dieckmann, V., H. J. Schenk, B. Horsfield, and D. H. Welte, 1998, Kinetics of petroleum generation and cracking by programmed-temperature closed-system pyrolysis of Toarcian Shales: Fuel, v. 77, no. 1-2, p. 23-31.
25. Drobne, D., M. Milani, V. Leser, and F. Tatti, 2007, Surface damage induced by FIB milling and imaging of biological samples is controllable: Microscopy Research and Technique, v. 70, no. 10, p. 895-903.
26. Drobne, D., M. Milani, V. Leser, F. Tatti, A. Zrimec, N. Znidarsic, R. Kostanjsek, and J. Strus, 2008, Imaging of intracellular spherical lamellar structures and tissue gross morphology by a focused ion beam/scanning electron microscope (FIB/SEM): Ultramicroscopy, v. 108, no. 7, p. 663-670.
27. Elgmati, M., H. Zhang, B. Bai, and R. Flori, 2011a, Submicron-pore characterization of shale gas plays: Proceedings of the North American Unconventional Gas Conference and Exhibition, Society of Petroleum Engineers, SPE Paper 144050,19 p., doi: 10.2118/144050-MS
28. Elgmati, M., M. Zobaa, H. Zhang, B. Bai, and F. Oboh-Ikuenobe, 2011b, Palynofacies analysis and submicron-pore modeling of shale-gas plays: Proceedings of the North American Unconventional Gas Conference and Exhibition, Society of Petroleum Engineers, SPE Paper 144267,10 p., doi: 10.2118/144267-MS.
29. Ghazban, R, and I. S. Al-Aasm, 2010, Hydrocarbon-induced diagenetic dolomite and pyrite formation associated with the Hormoz Island Salt Dome, Offshore Iran: lournal of Petroleum Geology, v. 33, no. 2, p. 183-196.
30. Goldstein, T. P., and Z. Aizenshtat, 1994, Thermochemical sulfate reduction-A Review: Journal of Thermal Analysis, v. 42, no. 1, p. 241-290.
31. Haswell, R., U. Zeile, and K. Mensch, 2008, Van Gogh's painting grounds: An examination of barium sulphate extender using analytical electron microscopy-SEM/ FIB/TEM/EDX: Microchimica Acta, v. 161, no. 3-4, p.363-369.
32. Heaney, P. J., E. P. Vicenzi, L. A. Giannuzzi, and K. J. T. Livi, 2001, Focused ion beam milling: A method of site-specific sample extraction for microanalysis of earth and planetary materials: American Mineralogist, v. 86, no. 9, p. 1094-1099.
33. Heath, J. E., T. A. Dewers, B. J. O. L. McPherson, R. Petrusak, T. C. Chidsey, A. J. Rinehart, and P. S. Mozley, 2011, Pore networks in continental and marine mud-stones: Characteristics and controls on sealing behavior: Geosphere, v. 7, no. 2, p. 429-454.
34. Hekking, L. H. P., M. N. Lebbink, D. A. M. De Winter, C. T. W. M. Schneijdenberg, C. M. Brand, B. M. Humbel, A. J. Verkleij, and J. A. Post, 2009, Focused ion beam-scanningelectron microscope: Exploring large volumes of atherosclerotic tissue: Journal of Microscopy, v. 235, no. 3, p. 336-347.
35. Hildenbrand, A., and J. L. Urai, 2003, Investigation of the morphology of pore space in mudstones-first results: Marine and Petroleum Geology, v. 20, no. 10, p. 1185-1200.
36. Ishitani, T., K. Umemura, T. Ohnishi, T. Yaguchi, and T. Kamino, 2004, Improvements in performance of focused ion beam cross-sectioning: Aspects of ion-sample interaction: Journal of Electron Microscopy, v. 53, no. 5, p. 443-449.
37. Javadpour, E, 2009, Nanopores and apparent permeability of gas flow in mudrocks (shales and siltstone): Journal of Canadian Petroleum Technology, v. 48, no. 8, p. 16-21.
38. Jenkins, C, and C. Boyer, 2008, Coalbed and shale-gas reservoirs: Journal of Petroleum Technology, v. 60, no. 2, p. 92-99.
39. Jochum, J., G. Friedrich, D. Leythaeuser, R. Littke, and B. Ropertz, 1995, Hydrocarbon-bearing fluid inclusions in calcite-filled horizontal fractures from mature Posidonia Shale (Hils syncline, NW Germany): Ore Geology Reviews, v. 9, p. 363-370.
40. Kastner, M., and R. Siever, 1979, Low temperature feldspars in sedimentary rocks: American Journal of Science, v. 279, no. 4, p. 435-79.
41. Kelemen, S. R., C. C. Walters, P. J. Kwiatek, H. Freund, M. Afeworki, M. Sansone, W. A. Lamberti, R. J. Pottrof, H. G. Machel, K. E. Peters, and T. Bolin, 2010, Characterization of solid bitumens originating from thermal chemical alteration and thermochemical sulfate reduction: Geochimica et Cosmochimica Acta, v. 74, p. 5305-5332.
42. Kim, J. W., W. R. Bryant, J. S. Watkins, and T. T. Tieh, 1999, Electron microscopic observations of shale diagenesis, offshore Louisiana, USA, Gulf of Mexico: Geo-marine Letters, v. 18, no. 3, p. 234-240.
43. Krouse, H. R., C. A. Viau, L. S. Eliuk, A. Ueda, and S. Halas, 1988, Chemical and isotopic evidence of thermochemical sulfate reduction by light-hydrocarbon gases in deep carbonate reservoirs: Nature, v. 333, no. 6172, p. 415-419.
44. Krueger, R., 1999, Dual-column (FIB-SEM) wafer applications: Micron, v. 30, no. 3, p. 221-226.
45. Langford, R.M., 2006, Focused ion beams techniques for nanomaterials characterization: Microscopy Research and Technique, v. 69, no. 7, p. 538-549.
46. Lash, G., S. Loewy, and T. Engelder, 2004, Preferential jointing of Upper Devonian black shale, Appalachian Plateau, USA: Evidence supporting hydrocarbon generation as a joint-driving mechanism, in J. W. Cosgrove and T. Engelder, eds., The initiation, propagation, and arrest of joints and other fractures: GSL Special Publications, v. 231, p. 129-151.
47. Leser, V., M. Milani, F. Tatti, Z. P. Tkalec, J. Strus, and D. Drobne, 2010, Focused ion beam (FIB)/scanning electron microscopy (SEM) in tissue structural research: Protoplasma, v. 246, no. 1-4, p. 41-8.
48. Littke, R., D. Leythaeuser, J. Rullkotter, and D. R. Baker, 1991, Keys to the depositional history of the Posidonia Shale (Toarcian) in the Hils syncline, northern Germany: GSL Special Publications, v. 58, no. 1, p. 311-333.
49. Loucks, R. G., R. M. Reed, S. C. Ruppel, and D. M. Jarvie, 2009, Morphology, genesis, and distribution of nanometer-scale pores in siliceous mudstones of the Mississippian Barnett Shale: Journal of Sedimentary Research, v. 79, no. 12, p. 848-861.
50. Loucks, R. G., R. M. Reed, S. C. Ruppel, and U. Hammes, 2010, Preliminary classification of matrix pores in mudrocks: Gulf Coast Association of Geological Societies Transactions, v. 60, p. 435-141.
51. Machel, H. G., 1987, Saddle dolomite as a by-product of chemical compaction and thermochemical sulfate reduction: Geology, v. 15, no. 10, p. 936-940.
52. Mann, U., S. Diippenbecker, A. Langen, B. Ropertz, and D. H. Welte, 1990, Pore network evolution of the lower Toarcian Posidonia Shale during petroleum generation and expulsion-A multidisciplinary approach: Zentralblatt fur Geologie und Palaontologie Teil I, v. 8, p. 1051-1071.
53. Mayer, J., L. A. Giannuzzi, T. Kamino, and J. Michael, 2007, TEM sample preparation and FIB-induced damage: MRS Bulletin, v. 32, no. 5, p. 400-407.
54. Mehmani, A., A. Tokan-Lawal, M. Prodanovic, and A. P. Sheppard, 2011, The effect of microporosity on transport properties in tight reservoirs: Proceedings of the North American Unconventional Gas Conference and Exhibition, Society of Petroleum Engineers, SPE Paper 144383,14 p., doi: 10.2118/144384-MS.
55. Meyers, S. R., 2007, Production and preservation of organic matter: The significance of Iron: Paleoceanography, v. 22, no. 4, p. PA4211.
56. Milliken, K. L., 1992, Chemical behavior of detrital feldspars in mudrocks versus sandstones, Frio Formation (Oligocene), South Texas: Journal of Sedimentary Petrology, v. 62, p. 790-801.
57. Milliken, K. L., and R. M. Reed, 2010, Multiple causes of dia-genetic fabric anisotropy in weakly consolidated mud, Nankai accretionary prism, IODP Expedition 316: Journal of Structural Geology, v. 32, p. 1887-1898.
58. Mohr, M., P. A. Kukla, J. L. Urai, and G. Bresser, 2005, Multiphase salt tectonic evolution in NW Germany: Seismic interpretation and retro-deformation: International Journal of Earth Sciences, v. 94, no. 5-6, p. 917-940.
59. Mondol, N. H., K. Bjorlykke, and J. Jahren, 2008, Experimental compaction of clays: Relationship between permeability and petrophysical properties in mudstones: Petroleum Geoscience, v. 14, no. 4, p. 319-337.
60. Moore, C. H., 1997, Carbonate diagenesis and porosity: Developments in Sedimentology 46, Elsevier, p. 1-338.
61. Nelson, P. H., 2009, Pore throat sizes in sandstones, tight sandstones, and shales: AAPG Bulletin, v. 93, p. 1-13.
62. Obst, M., P. Gasser, D. Mavrocordatos, and M. Dittrich, 2005, TEM-specimen preparation of cell/mineral interfaces by focused ion beam milling: American Mineralogist, v. 90, no. 8-9, p. 1270-1277.
63. Ohfuji, H., and D. Rickard, 2005, Experimental syntheses of framboids-a review: Earth-Science Reviews, v. 71, no. 3-4, p. 147-170.
64. Park, S. E., A. Schertel, and S. S. Han, 2010, Altered structure of synapse in a brain of the Swedish mutation which causes early-onset Alzheimer's disease: A FIB-SEMmicroscopy study: Journal of Neurogenetics, v. 24, no. 1, p. 38-39.
65. Passey, Q. R., K. M. Bohacs, W. L. Esch, R. Klimentidis, and S. Sinha, 2010, From oil-prone source rock to gas-producing shale reservoir-Geologic and petro-physical characterization of unconventional shale gas reservoirs: Proceedings of the North American Unconventional Gas Conference and Exhibition, Society of Petroleum Engineers, SPE Paper 131350, 29 p., doi: 10.2118/131350-MS.
66. Pearson, F. J., 1999, What is the porosity of a mudrock?: GSL, Special Publications, v. 158, p. 9-21.
67. Petmecky, S., L. Meier, H. Reiser, and R. Littke, 1999, High thermal maturity in the Lower Saxony Basin: Intrusion or deep burial?: Tectonophysics, v. 304, no. 4, p. 317-344.
68. Rapp, J. R, S. Klemme, I. B. Butler, and S. L. Harley, 2010, Extremely high solubility of rutile in chloride and fluoride-bearing metamorphic fluids: An experimental investigation: Geology, v. 38, no. 4, p. 323-326.
69. Ross, D. J., and R. M. Bustin, 2009, The importance of shale composition and pore structure upon gas storage potential of shale gas reservoirs: Marine and Petroleum Geology, v. 26, no. 6, p. 916-927.
70. Rubanov, S., and P. R. Munroe, 2004, FIB-induced damage in silicon: Journal of Microscopy, v. 214, no. 3, p. 213-221.
71. Rullkotter, J., et al., 1988, Organic matter maturation under the influence of a deep intrusive heat source: A natural experiment for quantitation of hydrocarbon generation and expulsion from a petroleum source rock (Toarcian shale, northern Germany): Organic Geochemistry, v. 13, no. 4-6, p. 847-856.
72. Ruttenberg, K. C, and R. A. Berner, 1993, Authigenic apatite formation and burial in sediments from non-upwelling, continental margin environments: Geochimica et Cosmochimica Acta, v. 57, p. 991-1007.
73. Scheck, M., U. Bayer, and B. Lewerenz, 2003, Salt movements in the Northeast German Basin and its relation to major post-Permian tectonic phases-results from 3D structural modelling, backstripping and reflection seismic data: Tectonophysics, v. 361, no. 3-4, p. 277-299.
74. Schiffbauer, J. D., and S. Xiao, 2009, Novel application of focused ion beam electron microscopy (FIB-EM) in preparation and analysis of microfossil ultrastructures: A new view of complexity in early eukaryotic organisms: Palaios, v. 24, no. 9, p. 616-626.
75. Schneider, J., P. B. Flemings, R. J. Day-Stirrat, and J. T. Germaine, 2011, Insights into pore-scale controls on mud-stone permeability through resedimentation experiments: Geology, v. 39, p. 1011-1014.
76. Sivel, V. G. M., J. Van Den Brand, W. R. Wang, H. Mohdadi, F. D. Tichelaar, P. F. A. Alkemade, and H. W. Zandbergen, 2004, Application of the dual-beam FIB/SEM to metals research: Journal of Microscopy, v. 214, no. 3, p. 237-245.
77. Slatt, R. M., and N. R. O'Brien, 2011, Pore types in the Barnett and Woodford gas shales: Contribution to understanding gas storage and migration pathways in fine-grained rocks: AAPG Bulletin, v. 95, no. 12, p. 2017-2030.
78. Smith, A. J., P. R. Munroe, T. Tran, and M.S. Wainwright, 2001, FIB preparation of a sensitive porous catalyst for TEM elemental mapping at high magnifications: Journal of Materials Science, v. 36, no. 14, p. 3519-3524.
79. Sondergeld, C. H., R. J. Ambrose, C. S. Rai, and J. Moncrieff, 2010a, Micro-structural studies of gas shales: Proceedings of the SPE Unconventional Gas Conference, Society of Petroleum Engineers, SPE Paper 131771, 17 p., doi: 10.2118/131771-MS.
80. Sondergeld, C. H., K. E. Newsham, J. T. Comiski, M. C. Rice, and C. S. Rai, 2010b, Petrophysical considerations in evaluating and producing shale gas: Proceedings of the SPE Unconventional Gas Conference, Society of Petroleum Engineers, SPE Paper 131768, 34 p., doi: 10.2118/131768-MS.
81. Spotl, C, F. J. Longstaffe, K. Ramseyer, and B. Rudinger, 1999, Authigenic albite in carbonate rocks-a tracer for deep-burial brine migration? Sedimentology, v. 46, no. 4, p. 649-666.
82. Thompson, L. E., P. M. Rice, E. Delenia, V. Y. Lee, P. J. Brock, T. P. Magbitang, G. Dubois, W. Volksen, R. D. Miller, and H. C. Kim, 2006, Imaging thin films of nanoporous low-K dielectrics: Comparison between ultramicrotomy and focused ion beam preparations for transmission electron microscopy: Microscopy and Microanalysis, v. 12, p. 156-159.
83. Tomutsa, L., D. B. Silin, and V. Radmilovic, 2007, Analysis of chalk petrophysical properties by means of submi-cron-scale pore imaging and modeling: SPE Reservoir Evaluation and Engineering, v. 10, no. 3, p. 285-293.
84. Walls, J. D., and S. W. Sinclair, 2011, Eagle Ford shale reservoir properties from digital rock physics: First Break, v. 29, p. 97-101.
85. Wirth, R., 2004, Focused ion beam (FIB): A novel technology for advanced application of micro- and nanoanalysis in geosciences and applied mineralogy: European Journal of Mineralogy, v. 16, no. 6, p. 863-876.
86. Wirth, R., 2009, Focused ion beam (FIB) combined with SEM and TEM: Advanced analytical tools for studies of chemical composition, microstructure and crystal structure in geomaterials on a nanometre scale: Chemical Geology, v. 261, no. 3-4, p. 217-229.
87. Yang, Y., and A. C. Aplin, 2010, A permeability-porosity relationship for mudstones: Marine and Petroleum Geology, v. 27, no. 8, p. 1692-1697.
88. Yao, S., K. Jiao, K. Zhang, W. X. Hu, H. Ding, M. C. Li, and W. M. Pei, 2011, An atomic force microscopy study of coal nanopore structure: Chinese Science Bulletin, v. 56, no. 25, p.2706-2712.