BIB-SEM pore characterization of mature and post mature Posidonia Shale samples from the Hils area, Germany

Klaver, Jop; Desbois, Guillaume; Littke, Ralf; Urai, János L.

doi:10.1016/j.coal.2016.03.003

Cited by 134 publications

(55 citation statements)

References 45 publications

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“…If we compare these values to the total porosity determined by who worked on exactly the same samples we find that only 10 % for WIC (or 24 % for HAD respectively) of the total porosity can be resolved using FIB-SEM. These differences are also similar to the results of Klaver et al (2012Klaver et al ( , 2016 and Mathia et al (2016). However, no trends towards higher porosities in one or the other sample were observed, likely due to spatial inhomogeneity.…”

Section: Porosity and Pore Size Distributionsupporting

confidence: 78%

“…With increasing maturity TOC contents decrease from 7.2-14.8 % (WIC) to 5.0-10.5 % (HAD). The porosity trends cannot be confirmed by direct observations performed with micro computed tomography (µ-CT) or scanning electron microscopy (SEM) in combination with focused-or broad-ion-beam polishing (FIB or BIB) as demonstrated by Klaver et al (2012Klaver et al ( , 2016, and Mathia et al (2016). Observed image porosities (0.2-3.0 %) were significantly lower due to a lack of resolution.…”

Section: Introductionmentioning

confidence: 93%

“…However, Kuila et al (2014) state that in organic-rich shales 10-70 % of the total porosity might not even be detectable with methods like field emission scanning electron microscopy, due to overly small pore sizes (< 5 nm) within organic matter and clays. Additionally, the type of organic matter controls its porosity with increasing maturity (e.g., Klaver et al, 2016). Although we did not classify the type of organic matter it is very likely that the observed matrix-filling OM in both samples is solid bitumen which becomes mesoporous by gasification processes at gaswindow maturities (Mathia et al, 2016).…”

Section: Porositymentioning

confidence: 99%

“…Recent data on the porosity, permeability and total organic carbon determination of Posidonia shale samples are compiled in Table 1. The total porosities are reported by Gasparik et al (2014), Rexer et al (2014), Ghanizadeh et al (2014), Mohnhoff et al (2015), , Klaver et al (2012Klaver et al ( , 2016 and Mathia et al (2016) vary between 9.8-17.8 % for WIC and 9.3-16 % for HAD. All studies reported consistently that the total porosity decreases from a maximum in the early mature sample WIC to a minimum in oil mature material to than rise again to an intermediate level in overmature gas window samples (HAD).…”

Section: Introductionmentioning

confidence: 99%

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Porosity and permeability determination of organic-rich Posidonia shales based on 3-D analyses by FIB-SEM microscopy

et al. 2016

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Abstract. The goal of this study is to better understand the porosity and permeability in shales to improve modelling fluid and gas flow related to shale diagenesis. Two samples (WIC and HAD) were investigated, both mid-Jurassic organic-rich Posidonia shales from Hils area, central Germany of different maturity (WIC R 0 0.53 % and HAD R 0 1.45 %). The method for image collection was focused ion beam (FIB) microscopy coupled with scanning electron microscopy (SEM). For image and data analysis Avizo and GeoDict was used. Porosity was calculated from segmented 3-D FIB based images and permeability was simulated by a Navier Stokes-Brinkman solver in the segmented images.Results show that the quantity and distribution of pore clusters and pores (≥ 40 nm) are similar. The largest pores are located within carbonates and clay minerals, whereas the smallest pores are within the matured organic matter. Orientation of the pores calculated as pore paths showed minor directional differences between the samples. Both samples have no continuous connectivity of pore clusters along the axes in the x, y, and z direction on the scale of 10 to 20 of micrometer, but do show connectivity on the micrometer scale. The volume of organic matter in the studied volume is representative of the total organic carbon (TOC) in the samples. Organic matter does show axis connectivity in the x, y, and z directions. With increasing maturity the porosity in organic matter increases from close to 0 to more than 5 %. These pores are small and in the large organic particles have little connection to the mineral matrix. Continuous pore size distributions are compared with mercury intrusion porosimetry (MIP) data. Differences between both methods are caused by resolution limits of the FIB-SEM and by the development of small pores during the maturation of the organic matter. Calculations show no permeability when only considering visible pores due to the lack of axis connectivity. Adding the organic matter with a background permeability of 1×10 −21 m 2 to the calculations, the total permeability increased by up to 1 order of magnitude for the low mature and decreases slightly for the overmature sample from the gas window. Anisotropy of permeability was observed. Permeability coefficients increase by 1 order of magnitude if simulations are performed parallel to the bedding. Our results compare well with experimental data from the literature suggesting that upscaling may be possible in the future as soon as maturity dependent organic matter permeability coefficients can be determined.

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Section: Porosity and Pore Size Distributionsupporting

confidence: 78%

Section: Introductionmentioning

confidence: 93%

Section: Porositymentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

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Porosity and permeability determination of organic-rich Posidonia shales based on 3-D analyses by FIB-SEM microscopy

et al. 2016

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“…The pore structure characterization methods can be divided into two categories: (1) Direct method. To directly observe and obtain image by means of optical microscope, transmission electron microscope (TEM), scanning electron microscope (SEM), and other micro zone observation technologies in order to get the size, shape and distribution of pores and other qualitative informations in shales (Chalmers et al, 2012;Curtis et al, 2012;Loucks et al, 2012;Gu et al, 2015;Klaver et al, 2015Klaver et al, , 2016Li et al, 2015b;Tang et al, 2016;; (2) Indirect method. Mainly by means of probe gas adsorption techniques to quantitatively characterize the pore size and pore structure, including neutron scattering, high pressure mercury intrusion, low pressure gas adsorption and so on (Mastalerz et al, 2012(Mastalerz et al, , 2013Clarkson et al, 2013;Cao et al, 2015;Hu et al, 2015).…”

Section: Introductionmentioning

confidence: 99%

Quantitative characterization of micropore structure for organic-rich Lower Silurian shale in the Upper Yangtze Platform, South China: Implications for shale gas adsorption capacity

Chen

Jiang

Liu

et al. 2017

Adv. Geo-Energ. Res.

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The pores in shales are mainly of nanometer-scale, and their pore size distribution is very important for shale gas storage and adsorption capacity, especially micropores having widths less than 2 nm, which contribute to the main occurrence space for gas adsorption. This study is focused on the organic-rich Lower Silurian black shale from four wells in the Upper Yangtze Platform, and their total organic carbon (TOC), mineralogical composition and micropore characterization were investigated. Low pressure CO2 adsorption measurement was conducted at 273.15 K in the relative pressure range of 0.0001-0.03, and the micropore structure was characterized by Dubinin-Radushkevich (DR) equation and density functional theory (DFT) method and then the relationship between micropore structure and shale gas adsorption capacity was discussed. The results indicated that (1) The Lower Silurian shale have high TOC content in the range of 0.92-4.96%, high quartz content in the range of 30.6-69.5%, and high clays content in the range of 24.1-51.2%. The TOC content shows a strong positive relationship with the quartz content which suggests that the quartz is mainly biogenic in origin. (2) The micropore volume varies from 0.12 cm 3 /100 g to 0.44 cm 3 /100 g and micropore surface area varies from 4.97 m 2 /g to 17.94 m 2 /g. Both of them increase with increasing TOC content, indicating TOC is the key factor to control the micropore structure of the Lower Silurian shale. (3) Low pressure CO2 adsorption measurement provides the most suitable detection range (0.3-1.5 nm) and has high reliability and accuracy for micropore structure characterization. (4) The TOC content is the key factor to control gas adsorption capacity of the Lower Silurian shale in the Upper Yangtze Platform.

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Review on Organic Porosity in Shale Reservoirs

Singh¹,

Hazra²,

Singh³

et al. 2022

Handbook of Petroleum Geoscience

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BIB-SEM pore characterization of mature and post mature Posidonia Shale samples from the Hils area, Germany

Cited by 134 publications

References 45 publications

Porosity and permeability determination of organic-rich Posidonia shales based on 3-D analyses by FIB-SEM microscopy

Porosity and permeability determination of organic-rich Posidonia shales based on 3-D analyses by FIB-SEM microscopy

Quantitative characterization of micropore structure for organic-rich Lower Silurian shale in the Upper Yangtze Platform, South China: Implications for shale gas adsorption capacity

Review on Organic Porosity in Shale Reservoirs

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