scholarly journals Imaging and quantification of the pore microstructure of gas shales using X-ray microtomography

2017 ◽  
Author(s):  
Mozhdeh Mehrabi ◽  
Mehrdad Pasha ◽  
Ali Hassanpour ◽  
Paul W. J. Glover ◽  
Xiaodong Jia

Abstract. Optimisation of gas production from shale gas reservoirs depends critically upon a good understanding of the porosity and pore microstructure of the shale. Conventionally surface area measurements or mercury porosimetry have been used to measure the porosity in gas shales. However, these conventional methods have limited accuracy and only provide a bulk measurement for the samples. More recently, scanning electron micrography (SEM) and Focussed Ion Beam SEM (FIB-SEM) techniques have been applied in an attempt to address these limitations. Unfortunately, these two methods destroy the samples. In this research three-dimensional x-ray micro tomography (XRMT) imaging techniques were used to capture the structure of three samples and also compared to data from mercury porisimetry. The resulting data have been segmented in order to recognize individual pores down to a resolution of about 1 µm. Distributions of pore volume, pore size, pore aspect ratio, surface area to pore volume ratios and pore orientations were calculated from the XRMT data. It was found that the porosity obtained from XRMT measurements is smaller than that obtained using mercury porisimetry, the reason for which might be displacement of kerogen by the high pressures generated in the mercury technique, but is unlikely to be due to both techniques not being able to measure pores smaller that about 900 nm. Pore volume and size distributions showed all of the shales tested in this work to be multimodal with similar major modal values for volume and pore size. The pores also have a range of pore aspect ratios and surface area to pore volumes, including values indicating the presence of significant oblate spheroidal pores where the major axis is up to 330 times bigger than the minor axis. This has implications both for the connectedness of pores and the resultant gas permeability and the effectiveness of gas desorption processes into the gas shale's pores. These high aspect ratio pores were oriented both in dip and azimuth in preferential directions making it likely that the shale gas itself has significant anisotropy both for permeability and in its mechanical properties. Permeabilities calculated from the XRMT distribution data matched very well with permeabilities obtained by scaling considerations and typical values for similar gas shales.

2019 ◽  
Vol 10 ◽  
pp. 2217-2228 ◽  
Author(s):  
B Rabindran Jermy ◽  
Vijaya Ravinayagam ◽  
Widyan A Alamoudi ◽  
Dana Almohazey ◽  
Hatim Dafalla ◽  
...  

The combination of magnetic nanoparticles with a porous silica is a composite that has attracted significant attention for potential multifunctional theranostic applications. In this study, 30 wt % CuFe2O4 was impregnated into a matrix of monodispersed spherical hydrophilic silica (HYPS) nanoparticles through a simple dry impregnation technique. The chemotherapy drug cisplatin was loaded through electrostatic equilibrium adsorption over 24 h in normal saline solution. The presence of cubic spinel CuFe2O4 on HYPS was confirmed through powder X-ray diffraction (PXRD), Fourier transform infrared spectroscopy (FTIR) and diffuse reflectance UV–vis spectroscopy (DR UV–vis) analysis. The HYPS particles showed a surface area of 170 m2/g, pore size of 8.3 nm and pore volume of 0.35 cm3/g. The cisplatin/CuFe2O4/HYPS nanoformulation showed the accumulation of copper ferrite nanoparticles on the surface and in the pores of HYPS with a surface area of 45 m2/g, pore size of 16 nm and pore volume of 0.18 cm3/g. Transmission electron microscopy (TEM) and energy dispersive X-ray (EDX) mapping analysis showed the presence of homogeneous silica particles with nanoclusters of copper ferrite distributed on the HYPS support. Vibrating sample magnetometry (VSM) analysis of CuFe2O4/HYPS showed paramagnetic behavior with a saturated magnetization value of 7.65 emu/g. DRS UV–vis analysis revealed the functionalization of cisplatin in tetrahedral and octahedral coordination in the CuFe2O4/HYPS composite. Compared to other supports such as mesocellular foam and silicalite, the release of cisplatin using the dialysis membrane technique was found to be superior when CuFe2O4/HYPS was applied as the support. An in vitro experiment was conducted to determine the potential of CuFe2O4/HYPS as an anticancer agent against the human breast cancer cell line MCF-7. The results show that the nanoparticle formulation can effectively target cancerous cells and could be an effective tumor imaging guide and drug delivery system.


2020 ◽  
Author(s):  
Mohamed Garum ◽  
Paul Glover ◽  
Piroska Lorinczi ◽  
Ali Hassanpour

<p> </p><p>Cost-effective and environmentally sensitive shale gas production requires detailed knowledge of the petrophysical characteristics of the shale from which the gas is extracted. Parameters such as the kerogen fraction, pore size distributions, porosity, permeability, the frackability of the rock and the degree to which natural fracturing already occurs are required in order to be able to estimate potential gas reserves and how easily it can be extracted. Innovative imaging techniques, including Focused Ion Beam Scanning Electron Microscopy (FIB-SEM) and Nanoscale X-Ray Tomography (nano-CT), can be used to characterise the microstructural properties of shale. Here we report using FIB-SEM serial sectioning and nano-CT on approximately cubic samples of side length about 25 µm. The resolution of the FIB-SEM scanning is approximately 20 nm, while that of the nano-CT is about 50 nm, providing between 125 and 1953 million voxels per scan. These ultra-high resolution techniques have been shown to be effective methods for the analysis and imaging of shale microstructure. Each technique can provide data over a different and separate range of scales, and with different resolutions. Results analysed so far indicate that pores which seem to be unconnected when imaged on a micrometre scale by micro-CT scanning, are connected by thin pathways when imaged at these higher resolutions. This nano-scale connectivity is responsible for the small but non-zero permeability of gas shales to gas flow, which is typically measured in the range 5 nD – 200 nD. The volume, size, aspect ratios, surface area to volume ratio and orientations have all been calculated from the scanned data as a function of scale. These data indicate an extremely complex, heterogeneous, anisotropic and multimodal pore nanostructure and microstructure for the shales, with structure at all scales contributing to both gas storage and gas flow. Further work analysing the connectivity of the microscale and nanoscale pore spaces within the rock is underway. We believe that the combination of nano-CT with FIB-SEM on the same sample has the potential for providing an enhanced understanding of shale microstructure, which is necessary for modelling elastic behaviour, gas storage, gas desorption and gas flow in gas shales.</p><p><strong>Keywords:</strong> Gas shale, FIB-SEM, nano-CT, porosity, permeability, Kerogen, pore volume, size distribution, pore aspect ratio and surface area to pore volume.</p>


2017 ◽  
Vol 79 (3) ◽  
Author(s):  
Abdu Muhammad Bello ◽  
Abdul Rahim Yacob ◽  
Kamaluddeen Suleiman Kabo

Mesoporous γ-Al2O3 with large surface area and narrow pore size was synthesized from acid-leachates of calcined kaolin in the presence of polyethylene glycol 6000 (PEG-6000) surfactant at room temperature. The synthesized alumina was characterized by X-ray diffraction (XRD), Nitrogen adsorption-desorption, Fourier transform infra-red spectroscopy (FTIR), field emission scanning electron microscopy (FESEM) with energy-dispersive X-ray analysis (EDX), and thermogravimetric-Derivative thermal analysis (TG-DTA). High-purity mesoporous γ-Al2O3 with large surface area of 365.1 m2/g, narrow pore size distribution centred at 5.3 nm and pore volume of 0.46 cm3/g was obtained at 500 oC. When the calcination temperature has increased to 700 oC, the surface area decreased to 272.9 m2/g. Crystallite size calculated using Scherer’s equation revealed the average size of 4.33 and 4.12 nm for alumina calcined at 500 and 700 oC, respectively. The excellent pore structural properties (high surface area and large pore volume) of the synthesized mesoporous γ-alumina in the present study will allow for higher loading of active catalytic phases, as such it can be used as catalyst support.  


2018 ◽  
Vol 37 (1) ◽  
pp. 194-218 ◽  
Author(s):  
Hongjie Xu ◽  
Shuxun Sang ◽  
Jingfen Yang ◽  
Jun Jin ◽  
Huihu Liu ◽  
...  

Indentifying reservoir characteristics of coals and their associated shales is very important in understanding the co-exploration and co-production potential of unconventional gases in Guizhou, China. Accordingly, comprehensive experimental results of 12 core samples from well LC-1# in the northern Guizhou were used and analyzed in this paper to better understand their vertical reservoir study. Coal and coal measured shale, in Longtan Formation, are rich in organic matter, with postmature stage of approximately 3.5% and shales of type III kerogen with dry gas generation. All-scale pore size analysis indicates that the pore size distribution of coal and shale pores is mainly less than 20 nm and 100 nm, respectively. Pore volume and area of coal samples influenced total gas content as well as desorbed gas and lost gas content. Obvious relationships were observed between residual gas and BET specific surface area and BJH total pore volume (determined by nitrogen adsorption). For shale, it is especially clear that the desorbed gas content is negatively correlated with BET specific surface area, BJH total pore volume and clay minerals. However, the relationships between desorbed gas and TOC (total organic carbon) as well as siderite are all well positive. The coals and shales were shown to have similar anoxic conditions with terrestrial organic input, which is beneficial to development of potential source rocks for gas. However, it may be better to use a low gas potential assessment for shales in coal-bearing formation because of their low S1+S2 values and high thermal evolution. Nevertheless, the coalbed methane content is at least 10 times greater than the shale gas content with low desorbed gases, indicating that the main development unconventional natural gas should be coalbed methane, or mainly coalbed methane with supplemented shale gas.


Minerals ◽  
2021 ◽  
Vol 11 (3) ◽  
pp. 298
Author(s):  
Chenlong Ding ◽  
Jinxian He ◽  
Hongchen Wu ◽  
Xiaoli Zhang

Ordos Basin is an important continental shale gas exploration site in China. The micropore structure of the shale reservoir is of great importance for shale gas evaluation. The Taiyuan Formation of the lower Permian is the main exploration interval for this area. To examine the nanometer pore structures in the Taiyuan Formation shale reservoirs in the Lin-Xing area, Northern Shaanxi, the microscopic pore structure characteristics were analyzed via nitrogen adsorption experiments. The pore structure parameters, such as specific surface area, pore volume, and aperture distribution, of shale were calculated; the significance of the pore structure for shale gas storage was analyzed; and the main controlling factors of pore development were assessed. The results indicated the surface area and hole volume of the shale sample to be 0.141–2.188 m2/g and 0.001398–0.008718 cm3/g, respectively. According to the IUPAC (International Union of Pure and Applied Chemistry) classification, mesopores and macropores were dominant in the pore structure, with the presence of a certain number of micropores. The adsorption curves were similar to the standard IV (a)-type isotherm line, and the hysteresis loop type was mainly similar to H3 and H4 types, indicating that most pores are dominated by open type pores, such as parallel plate-shaped pores and wedge-shaped slit pores. The micropores and mesopores provide the vast majority of the specific surface area, functioning as the main area for the adsorption of gas in the shale. The mesopores and macropores provide the vast majority of the pore volume, functioning as the main storage areas for the gas in the shale. Total organic carbon had no notable linear correlation with the total pore volume and the specific surface area. Vitrinite reflectance (Ro) had no notable correlation with the specific surface area, but did have a low “U” curve correlation with the total pore volume. There was no relationship between the quartz content and specific surface area and total pore volume. In addition, there was no notable correlation between the clay mineral content and total specific surface area and total pore volume.


2015 ◽  
Vol 22 (6) ◽  
Author(s):  
Nazile Ural

AbstractIn this study, the relationships between geotechnical index properties and the pore-size distribution of compacted natural silt and artificial soil mixtures, namely, silt with two different clays and three different clay percentages (10%, 20%, and 40%), were examined and compared. Atterberg’s limit tests, standard compaction tests, mercury intrusion porosimetry, X-ray diffraction, scanning electron microscopy (SEM) analysis, and Brunauer-Emmett-Teller specific surface analysis were conducted. The results show that the liquid limit, the cumulative pore volume, and specific surface area of artificially mixed soils increase with an increase in the percentage of clay. The cumulative pore volume and specific surface area with geotechnical index properties were compared. High correlation coefficients were observed between the specific areas and both the liquid limit and the plasticity index, as well as between the cumulative pore volume and both the clay percentage and the


1994 ◽  
Vol 337 ◽  
Author(s):  
Marsha Abramo ◽  
Loren Hahn

ABSTRACTFocused ion beam (FIB) technology is used to modify circuits for early-product design debug; it also has the capability to create probe points to underlying metallurgy, allowing device characterization while maintaining full functionality. These techniques provide critical feedback to designers for rapid verification of proposed design changes.Current FIB technology has its limitations because of redeposition of sputtered material; this phenomena may induce vertical electrical shorts and limit the achievable aspect ratio of a milled via to 6:1. Therefore, innovative enhancements are required to provide modification capability on planar chip technology which may utilize up to five levels of metallurgy. The ability to achieve high-aspect-ratio milling is required to access underlying circuitry. Vias with aspect ratios of 10:1 are necessary in some cases.This paper reviews a gas-assisted etching (GAE) process that enhances FIB milling by volatilizing the sputtered material, examines the results obtained from utilizing the GAE process for high-aspect-ratio milling, and discusses selectivity of semiconductor materials (silicon, aluminum, tungsten and silicon dioxide).


2018 ◽  
Vol 6 (4) ◽  
pp. T819-T833 ◽  
Author(s):  
Yang Gu ◽  
Wenlong Ding ◽  
Min Yin ◽  
Ruyue Wang ◽  
Baocheng Jiao ◽  
...  

The marine shale in South China has great gas exploration potential, and exploration in the Sichuan Basin has been successful, but the degree of exploration remains low in the Guizhou Province. We used organic geochemical analyses (total organic carbon content and kerogen type), scanning electron microscopy (SEM), field emission SEM, nuclear magnetic resonance (NMR), X-ray diffraction analysis, and low-temperature [Formula: see text] and [Formula: see text] adsorption experimental methods to study the micropore types and pore structures and their effects on the methane adsorption capacity of organic-rich shales found in the Fenggang block in northern Guizhou Province. The results indicate that the microscopic surface porosity of the lower Cambrian Niutitang Formation ranges from 2.88% to 5.34%, with an average value of 3.86%. Based on nitrogen adsorption methods, the range of the average pore size distribution is 4.6–9.491 nm, with an average value of 6.68 nm. All of the samples exhibit significant unimodal distributions. The main pore size is less than 10 nm, and these pores account for most of the mesopore volume, which is generally consistent with the NMR results. The methane adsorption capacity of the shale samples gradually increases in the range of 0–8 MPa at 30°C and reaches a maximum at approximately 10 MPa. Positive correlations were found between the gas content and specific surface area, total pore volume, and micropore volume. These strong correlations indicate that the Niutitang Shale has a high specific surface area, a high pore volume, and narrow-diameter pores, demonstrating that it has a high gas adsorption capacity. The results of this study provide valuable information regarding the adsorption characteristics of marine shales and the factors that affect those characteristics.


2011 ◽  
Vol 239-242 ◽  
pp. 2274-2279 ◽  
Author(s):  
Ying Chun Wang ◽  
Wen Hai Huang ◽  
Ai Hua Yao ◽  
De Ping Wang

A simple method to prepare hollow hydroxyapatite (HAP) microspheres with mespores on the surfaces is performed using a precipitation method assisted with Li2O-CaO-B2O3(LCB) glass fabrication process. This research is concerned with the effect of sintering temperature on the microstructure evolution, phase purity, surface morphology, specific surface area, and porosity after sintering process. The microspheres were sintered in air atmosphere at temperatures ranging from 500 to 900 °C. The starting hollow HAP microspheres and the sintered specimens were characterized by scanning electron microscope, X-ray diffractometer, specific surface area analyzer, and Hg porosimetry, respectively. The as-prepared microspheres consisted of calcium deficient hydroxyapatite. The results showed that the as-prepared hollow HAP microspheres had the highest specific surface areas, and the biggest total pore volume. The pore size distribution of the as-prepared hollow HAP microspheres were mainly the mesopores in the range of 2~40 nm. The specific surface area and total pore volume of hollow HAP microspheres decreased with increasing sintering temperature. Whereas the mean pore size increased with increasing sintering temperature. It showed that at 700°C, Ca-dHAP decomposes into a biphasic mixture of HAP and β-calcium phosphate(TCP).


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