scholarly journals Morphology of the pore space in claystones – evidence from BIB/FIB ion beam sectioning and cryo-SEM observations

2009 ◽  
Vol 4 (1) ◽  
pp. 1-19 ◽  
Author(s):  
G. Desbois ◽  
J. L. Urai ◽  
P. A. Kukla
Keyword(s):  
2021 ◽  
Vol 9 ◽  
Author(s):  
Jia Wang ◽  
Xianfeng Tan ◽  
Jingchun Tian ◽  
Long Luo ◽  
Xuanbo Gao ◽  
...  

Diagenetic evolution is an important controlling factor of shale gas reservoirs. In this study, based on field outcrop and drilling core data, analytical techniques including X-ray diffraction (XRD), field emission scanning electron microscope combined with a focused ion beam (FIB-FESEM), and energy-dispersive spectroscopy (EDS) analyses were performed to determine the diagenetic evolution of the Longmaxi Formation shale and reveal the effect of diagenetic evolution on the shale gas exploration and development in the Sichuan Basin, Southwest China. The eodiagenesis phase was subdivided into two evolution stages, and the mesodiagenesis phase was subdivided into three evolution stages in the basin margin and center. Absorbed capacity and artificial fracturing effect of the Longmaxi Formation shale gas were related to mineral composition, which was influenced by sedimentary characteristics and diagenetic evolution. The diagenetic system in the basin margin was more open than that in the basin center due to a different burial history. The more open diagenetic system, with more micro-fractures and soluble constitute (e.g., feldspar), was in favor for the formation and preservation of secondary dissolved pores and organic pores in the basin margin. The relatively closed diagenetic system with stronger compaction resulted in deformation of pore space in the central basin.


SPE Journal ◽  
2011 ◽  
Vol 17 (01) ◽  
pp. 219-229 ◽  
Author(s):  
Ray J. Ambrose ◽  
Robert C. Hartman ◽  
Mery Diaz-Campos ◽  
I. Yucel Akkutlu ◽  
Carl H. Sondergeld

Summary Using focused-ion-beam (FIB)/scanning-electron-microscope (SEM) imaging technology, a series of 2D and 3D submicroscale investigations revealed a finely dispersed porous organic (kerogen) material embedded within an inorganic matrix. The organic material has pores and capillaries having characteristic lengths typically less than 100 nm. A significant portion of total gas in place appears to be associated with interconnected large nanopores within the organic material. Thermodynamics (phase behavior) of fluids in these pores is quite different; gas residing in a small pore or capillary is rarefied under the influence of organic pore walls and shows a different density profile. This raises serious questions related to gas-in-place calculations: Under reservoir conditions, what fraction of the pore volume of the organic material can be considered available as free gas, and what fraction is taken up by the adsorbed phase? How accurately is the shale-gas storage capacity estimated using the conventional volumetric methods? And finally, do average densities exist for the free and the adsorbed phases? We combine the Langmuir adsorption isotherm with the volumetrics for free gas and formulate a new gas-in-place equation accounting for the pore space taken up by the sorbed phase. The method yields a total-gas-in-place prediction. Molecular dynamics simulations involving methane in small carbon slit-pores of varying size and temperature predict density profiles across the pores and show that (a) the adsorbed methane forms a 0.38-nm monolayer phase and (b) the adsorbed-phase density is 1.8–2.5 times larger than that of bulk methane. These findings could be a more important consideration with larger hydrocarbons and suggest that a significant adjustment is necessary in volume calculations, especially for gas shales high in total organic content. Finally, using typical values for the parameters, calculations show a 10–25% decrease in total gas-storage capacity compared with that using the conventional approach. The role of sorbed gas is more important than previously thought. The new methodology is recommended for estimating shale gas in place.


Geophysics ◽  
2016 ◽  
Vol 81 (5) ◽  
pp. D543-D551 ◽  
Author(s):  
Lukas M. Keller

Regarding the storage of nuclear waste within clay rock formations requires fundamental understanding of elastic properties of this rock type with regard to the risk evaluation process. The influence of the pore geometry on elastic properties of Opalinus Clay is studied on the basis of realistic pore microstructure, which is reconstructed from image data acquired by focused ion beam nanotomography. These microstructures are used as input pore geometries for linear elastic finite-element modeling to determine Thomsen’s [Formula: see text], [Formula: see text], and [Formula: see text] anisotropy parameters and the effective elastic moduli related to the porous material. The presence of fully drained intergranular pores substantially increases the values of [Formula: see text] and [Formula: see text]. For the investigated sample with an expected porosity of approximately 10 vol.%, the anisotropic pore space contributes similarly to the anisotropy parameters when compared with the contribution related to the preferred orientation of minerals. On the other hand, if the pore space is undrained, the effect of pores is smaller and the anisotropy is largely controlled by the preferred orientation of minerals. It is revealed that the value of [Formula: see text] is most sensitive to changes in water saturation. In case water is drained from the pores, the vertical Young’s modulus [Formula: see text] reduces significantly more when compared with the horizontal modulus [Formula: see text]. Presuming that the drainable porosity corresponds to a volume fraction of 10 vol.%, [Formula: see text] reduces by approximately 15%–20%. The effect of drainage is even more pronounced for the Poisson’s ratios, whereas the shear moduli are not much affected by drainage.


2020 ◽  
Vol 6 (10) ◽  
pp. 107
Author(s):  
Iryna Reimers ◽  
Ilia Safonov ◽  
Anton Kornilov ◽  
Ivan Yakimchuk

Focused Ion Beam Scanning Electron Microscopy (FIB-SEM) tomography provides a stack of images that represent serial slices of the sample. These images are displaced relatively to each other, and an alignment procedure is required. Traditional methods for alignment of a 3D image are based on a comparison of two adjacent slices. However, such algorithms are easily confused by anisotropy in the sample structure or even experiment geometry in the case of porous media. This may lead to significant distortions in the pore space geometry, if there are no stable fiducial marks in the frame. In this paper, we propose a new method, which meaningfully extends existing alignment procedures. Our technique allows the correction of random misalignments between slices and, at the same time, preserves the overall geometrical structure of the specimen. We consider displacements produced by existing alignment algorithms as a signal and decompose it into low and high-frequency components. Final transformations exclude slow variations and contain only high frequency variations that represent random shifts that need to be corrected. The proposed algorithm can operate with not only translations but also with arbitrary affine transformations. We demonstrate the performance of our approach on a synthetic dataset and two real FIB-SEM images of natural rock.


2018 ◽  
Vol 484 (1) ◽  
pp. 205-228 ◽  
Author(s):  
D. Misch ◽  
J. Klaver ◽  
D. Gross ◽  
J. Rustamov ◽  
R. F. Sachsenhofer ◽  
...  

AbstractThis study gives valuable insights into the microstructure and pore space characteristics of 17 compositionally variable Visean shale samples from the Ukrainian Dniepr-Donets Basin (the ‘Rudov Beds’). The representative imaging area varies considerably (from 10 000 to >300 000 µm2) as a function of the mineralogy and diagenetic overprinting. The pores hosted in organic matter (OM) are restricted to secondary solid bitumen. Based on high-resolution maps from broad ion beam scanning electron microscopy combined with organic geochemical and bulk mineralogical data, we propose that the amount of OM-hosted porosity responds to the availability of pore space, enabling the accumulation of an early oil phase, which is then progressively transformed to a porous solid bitumen residue. The type of OM porosity (pendular/interface v. spongy) is reflected in the individual pore size distributions: the spongy pores are usually smaller (<50 nm) than the pendular or OM–mineral interface pores. The OM-hosted porosity coincides with differences in the composition of the extract, with high amounts of extractable OM and saturated/aromatic compound ratios indicative of abundant porous solid bitumen. The average circularity and aspect ratio of the mineral matrix pores correlate with the corresponding values for the OM-hosted pores, which show a preferred bedding-parallel orientation, suggesting that compaction influenced both types of pore.


eEarth ◽  
2009 ◽  
Vol 4 (1) ◽  
pp. 15-22 ◽  
Author(s):  
G. Desbois ◽  
J. L. Urai ◽  
P. A. Kukla
Keyword(s):  

Author(s):  
Ilia Safonov ◽  
Anton Kornilov ◽  
Iryna Reimers

Digital rock analysis is a prospective approach to estimate properties of oil and gas reservoirs. This concept implies constructing a 3D digital twin of a rock sample. Focused Ion Beam - Scanning Electron Microscope (FIB-SEM) allows to obtain a 3D image of a sample at nanoscale. One of the main specific features of FIB-SEM images in case of porous media is pore-back (or shine-through) effect. Since pores are transparent, their back side is visible in the current slice, whereas, in fact, it locates in the following ones. A precise segmentation of pores is a challenging problem. Absence of annotated ground truth complicates fine-tuning the algorithms for processing of FIB-SEM data and prevents successful application of machine- learning-based methods, which require a huge training set. Recently, several synthetic FIB- SEM images based on stochastic structures were created. However, those images strongly differ from images of real samples. We propose fast approaches to render semisynthetic FIB- SEM images, which imply that intensities of voxels of mineral matrix in a milling plane, as well as geometry of pore space, are borrowed from an image of rock sample saturated by epoxy. Intensities of voxels in pores depend on the distance from milling plane to the given voxel along a ray directed at an angle equal to the angle between FIB and SEM columns. The proposed method allows to create very realistic FIB-SEM images of rock samples with precise ground truth. Also, it opens the door for numerical estimation of plenty of algorithms for processing FIB-SEM data.


2021 ◽  
Author(s):  
Alexander Avdonin ◽  
Mohammad Ebadi ◽  
Vladislav Krutko

Abstract Digital rock analysis has proven to be useful for the prediction of petrophysical properties of conventional reservoirs, where the pore space is captured well by a modern µCT scanner with a resolution of 1-5 µm. Nevertheless, this resolution is not enough to accurately capture the pore space of tight (low-permeable) rock samples. As a result, derived digital rock models do not reflect the real rock topology, and permeability predictions yield unreliable results. Our approach deploys high-contrast µCT scanning technique and Focused Ion Beam milling combined with Scanning Electron Microscopy to improve the quality of digital rock models and, hence, the permeability prediction. This workflow is successfully applied to a low-permeable rock sample of Achimov deposits. The computed permeability compares well to the experimental value.


SPE Journal ◽  
2021 ◽  
pp. 1-20
Author(s):  
Andrey Kazak ◽  
Kirill Simonov ◽  
Victor Kulikov

Summary The modern focused ion beam-scanning electron microscopy (FIB-SEM) allows imaging of nanoporous tight reservoir-rock samples in 3D at a resolution up to 3 nm/voxel. Correct porosity determination from FIB-SEM images requires fast and robust segmentation. However, the quality and efficient segmentation of FIB-SEM images is still a complicated and challenging task. Typically, a trained operator spends days or weeks in subjective and semimanual labeling of a single FIB-SEM data set. The presence of FIB-SEM artifacts, such as porebacks, requires developing a new methodology for efficient image segmentation. We have developed a method for simplification of multimodal segmentation of FIB-SEM data sets using machine-learning (ML)-based techniques. We study a collection of rock samples formed according to the petrophysical interpretation of well logs from a complex tight gas reservoir rock of the Berezov Formation (West Siberia, Russia). The core samples were passed through a multiscale imaging workflow for pore-space-structure upscaling from nanometer to log scale. FIB-SEM imaging resolved the finest scale using a dual-beam analytical system. Image segmentation used an architecture derived from a convolutional neural network (CNN) in the DeepUNet (Ronneberger et al. 2015) configuration. We implemented the solution in the Pytorch® (Facebook, Inc., Menlo Park, California, USA) framework in a Linux environment. Computation exploited a high-performance computing system. The acquired data included three 3D FIB-SEM data sets with a physical size of approximately 20 × 15 × 25 µm with a voxel size of 5 nm. A professional geologist manually segmented (labeled) a fraction of slices. We split the labeled slices into training, validation, and test data. We then augmented the training data to increase its size. The developed CNN delivered promising results. The model performed automatic segmentation with the following average quality indicators according to test data: accuracy of 86.66%, precision of 54.93%, recall of 83.76%, and F1 score of 55.10%. We achieved a significant boost in segmentation speed of 14.5 megapixel (MP)/min. Compared with 0.18 to 1.45 MP/min for manual labeling, this yielded an efficiency increase of at least 10 times. The presented research work improves the quality of quantitative petrophysical characterization of complex reservoir rocks using digital rock imaging. The development allows the multiphase segmentation of 3D FIB-SEM data complicated with artifacts. It delivers correct and precise pore-space segmentation, resulting in little turn-around-time saving and increased porosity-data quality. Although image segmentation using CNNs is mainstream in the modern ML world, it is an emerging novel approach for reservoir-characterizationtasks.


2012 ◽  
Vol 1421 ◽  
Author(s):  
Laxmikant V. Saraf

ABSTRACTIn this report, a method is discussed to perform successive milling on yttria-stabilized zirconia (YSZ), NiO-YSZ and Ni-alloy at the intervals of 85 nm 50 nm and 100 nm, respectively using a focused ion beam (FIB) followed by electron backscatter diffraction (EBSD) analysis on each slice. The EBSD data is then reconstructed to generate 3D volume. The 3D-EBSD band quality data is superimposed on inverse pole figure (IPF) grain orientation analysis to get a correlation with quality of band indexing. For the NiO-YSZ case, grain orientations and band quality factors were matched for grains ∼250 nm diameters producing a high resolution 3D-EBSD data. For this case, a pore space in 3D volume was visible due to nanocrystalline NiO-YSZ grain network. The advantages of 3D EBSD are discussed in the context of its applications to SOFC research community.


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