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Pore Volume Characteristics of Clay-Rich Shale: Critical Insight into the Role of Clay Types, Aluminum and Silicon Concentration

  • Research Article-Petroleum Engineering
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Abstract

Shale resources contain a significant quantity of clay minerals and organic matter. These material components influence the evolution of intra- and inter-granular pore features. This study investigates the role of clay’s elemental concentration, purity and types on its pore attributes. Four samples; illite, chlorite, montmorillonite, and kaolinite-rich clay samples were studied. Clay elemental composition, purity, pore shape, and structural parameters were determined. X-ray fluorescence and diffraction techniques were used to compute the elemental and mineralogical compositions of clay samples, respectively. Rock surfaces were mapped using the energy dispersive x-ray spectroscopy and scanning electron microscopy to confirm the distribution of elements and clay homogeneity, respectively in the four phyllosilicate materials. Total organic content analysis confirms the quantity of organic matter. N2 adsorption/desorption experiment at 77 K and over a relative pressure range up to 0.995 was executed with a surface area and porosity analyzer, to extract information regarding the pore shape, and determine the pore volume and specific surface area. The interrelation of the purity and computed pore structure properties was established. Mineralogy and elemental analyses showed that the studied samples with clay purities of 60–98% have a combined 80–96 wt.% of Aluminum (Al), Silicon (Si), and Iron (Fe). The adsorption–desorption curve at \( p/p^{o} < 0.04\) and carbon content analysis indicate that clays accommodate negligible micropores. The type III and IV isotherms combined with H1, H2, and H3 hysteresis loop implied that clay had connected complex pores with plate-like, uniform cylindrical, and inkbottle shapes. Capillary condensation and evaporation curves revealed more mesopores and macropores of 2-50 nm and > 50 nm, respectively. The pore distribution plateaued around an average of 100 nm, which confirmed the suitability of the Barrett-Joyner-Halenda technique to characterize clay mesopores. Kaolinite has the highest capacity (74.43 \({\text{cm}}^{{3}} {\text{/g}}\)) to host N2 gas at a standard temperature and pressure followed by montmorillonite (65.08 \({\text{cm}}^{{3}} {\text{/g}}\)), chlorite (21.01 \({\text{cm}}^{{3}} {\text{/g}}\)) and illite (16.59 \({\text{cm}}^{{3}} {\text{/g}}\)) in that order. The capacity of the pores to store fluid and their average size follow a similar pattern and increase with aluminum and clay contents. A specific surface area of the non-micropores is directly related to silicon concentration. The study provides an insight regarding the potential of kaolinite (with the highest aluminum concentration of 39.5 wt.%) as a good catalytic material required to speed up the esterification reaction. In addition, it can serve as a waste repository and a material for the treatment of phosphorus-containing contaminants in polluted areas. This research confirms that montmorillonite with the largest specific surface area in non-micropores and silicon content of 63.9 wt.% promotes reactivity and cation exchange interaction. However, this high basal spacing attribute of the material means that swelling will occur in the presence of water.

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Abbreviations

\(A_{{\text{m}}} = 0.162\;{\text{ nm}}^{{2}}\) :

Is nitrogen molecule surface area at 77 K

\(c_{{{\text{BET}}}}\) :

BET isotherm fitting constant

\(N_{{\text{A}}}\) :

Avogadro’s number \(\left( {6.022 \times 10^{22} \frac{{{\text{number}}}}{{{\text{mol}}}}} \right)\)

\(p^{o}\) :

Standard pressure of \({\text{N}}_{2} {\text{ gas}}\) \(\sim 1.02{\text{ bar at }}77.4{\text{ K}}\)

\(p/p^{o}\) :

Relative pressure of \({\text{N}}_{2} {\text{ gas}}\) between 0.001 and 0.995 and 77.4 K

\(r\) :

Pore radius (m)

\(R = 8.314{\text{ J}}/{\text{Kmol}}\) :

Is universal gas constant

\(s_{{{\text{BET}}}} \) :

Total specific surface area (m2/g)

\(S_{{{\text{ext}}}} { }\) :

Non-micropores specific surface area

\(S_{{{\text{mic}}}}\) :

Micropores specific surface area

\(t_{{{\text{ads}}}}\) :

Statistical thickness of adsorbed layer (Å)

\(T\) :

Temperature (\(K\))

\({\text{V}}_{{{\text{ads}}}} { }\) :

Total volume of adsorbed N2 gas at p⁄po = 0.001–0.995 and 77.4 K (m3/kg)

\(V_{{\text{m}}}\) :

Monolayer adsorption capacity (cm3/g)

\(V_{{{\text{mic}}}}\) :

Micropore filling volume

\(V_{{{\text{mol}}}}\) :

Molar volume (m3/mol)

\(\alpha\) :

Shape factor of the gas/liquid interface during adsorption

\(\Delta H_{{\text{m}}}\) :

Heat of gas condensation

\(\gamma\) :

Surface tension of liquid nitrogen (N/m)

AFM:

Atomic force microscopy

APM:

Areal porosity method

BET:

Brunauer, Emmett and Teller

BJH:

Barrett, Joyner and Halenda

BSE:

Backscatter electron

DRIFTs:

Diffuse reflectance Fourier transform infrared spectroscopy

EBSD:

Electron backscatter diffraction

EDX:

Energy-dispersive X-Ray spectroscopy

EGME:

Ethylene glycol monoethyl ether

HCPC:

Hierarchical clustering of principal components

IUPAC:

International union of pure and applied chemistry

LEED:

Low energy electron diffraction

LOD:

Limit of detection

MIP:

Mercury injection porosimetry

NDIR:

Non-destructive infrared

NMR:

Nuclei magnetic resonance

QEMSCAN:

Quantitative evaluation of minerals by scanning electron microscopy

SANS:

Small angle neutron scattering

SAXS:

Small angle X-ray scattering

SEM:

Scanning electron microscopy

SSA:

Specific Surface Area

SSM:

Solid sample measurements

STP:

Standard temperature and pressure

3D-SIMS:

Three-dimensional secondary ion mass spectroscopy

TEM:

Transmission electron microscopy

TOC:

Total organic content

XRD:

X-ray diffraction

µXRF:

Micro- X-ray fluorescence

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Acknowledgements

The authors acknowledge the provision of experimental equipment by the College of Petroleum Engineering and Geosciences (CPG) and the Research Institute at King Fahd University of Petroleum and Minerals, Dhahran, Saudi Arabia. A special appreciation to Dr. Abduljamiu Olalekan Amao, Mr. Bandar Al-Otaibi, Ms. Mashaer Alfaraj, and Mr. Nadeem Syed for their assistance in CPG laboratory analyses. The authors thank Mr. Reynante Balmes Pagcaliwagan for his cooperation in using the Surface Area and Porosity analyzer Micromeritics ASAP2020 model for the N2 adsorption experiment. The authors also thank anonymous reviewers for providing comments, which improve the manuscript’s quality.

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Authors and Affiliations

  1. Petroleum Engineering Department, College of Petroleum Engineering and Geosciences, King Fahd University of Petroleum and Minerals (Eastern Province), Dhahran, 31261, Saudi Arabia

    Clement Afagwu, Mohamed Mahmoud, Saad Alafnan, Abdullah Alqubalee & Shirish Patil

  2. Center for Integrative Petroleum Research, College of Petroleum Engineering and Geosciences, King Fahd University of Petroleum and Minerals, Dhahran, 31261, Saudi Arabia

    Abdullah Alqubalee

  3. Geosciences Department, College of Petroleum Engineering and Geosciences, King Fahd University of Petroleum and Minerals, Dhahran, 31261, Saudi Arabia

    Abdullah Alqubalee & Ammar ElHusseiny

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  1. Clement Afagwu
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Correspondence to Mohamed Mahmoud.

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Afagwu, C., Mahmoud, M., Alafnan, S. et al. Pore Volume Characteristics of Clay-Rich Shale: Critical Insight into the Role of Clay Types, Aluminum and Silicon Concentration. Arab J Sci Eng 47, 12013–12029 (2022). https://doi.org/10.1007/s13369-022-06720-w

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