Nano-scale pore structure and fractal dimension of organic-rich Wufeng-Longmaxi shale from Jiaoshiba area, Sichuan Basin: Investigations using FE-SEM, gas adsorption and helium pycnometry

• Pore structure is characterized by a combination of FE-SEM and gas adsorption.
• Fractal dimensions of nano-scale pore are calculated using fractal FHH model.
• Porosities obtained from He porosimetry and gas adsorption are comparable but higher than FE-SEM.
• Pore morphologies in high TOC and low TOC shales reflect pore genesis.
• Controlling factors for pore structure and fractal dimensions are determined.

Much attention have been recently paid to the upper Ordovician Wufeng shale (O3w) and lower Silurian Longmaxi shale (S1l) in the Jiaoshiba area of Sichuan Basin, which is now the largest producing shale gas field in China. Field emission scanning electron microscopy (FE-SEM), low pressure gas (N2 and CO2) adsorption, helium pycnometry, X-ray diffraction and geochemical analyses were performed to investigate the pore structure and fractal dimension of the pores in O3w-S1l shale formation in the Jiaoshiba area. FE-SEM images show that organic matter (OM) pores are dominant in the organic-rich samples and these pores are often irregular, bubble-like, elliptical and faveolate in shape, while in organic-poor samples, limited and isolated interparticle (interP), intraparticle (intraP) and OM pores are observed. Reversed S-shaped isotherms obtained from nitrogen adsorption are type Ⅱ, and hysteresis loops indicate that the shape of micropore in the samples is slit-or plate-like. BET surface areas and total pore volume vary from 12.2 to 27.1 m2/g and from 1.8 × 10−2 to 2.9 × 10−2 cm3/g, with an average of 19.5 m2/g and 2.3 × 10−2 cm3/g, respectively. Adsorption volume from both N2 and CO2 adsorption increases with respect to TOC contents. Porosities obtained from helium porosimetry are comparable with these from gas (CO2 and N2) adsorption in O3w-S1l shale. However, porosity determined by quantitative FE-SEM analysis is much smaller, which is mainly related to limited resolution and the small areas of investigation.Based on the Frenkel-Halsey-Hill (FHH) model of low-pressure N2 adsorption, fractal dimensions of the pores varied from 2.737 to 2.823. Relationships between pore structure parameters and TOC content, mineral composition and fractal dimension reveal that the fractal dimension is mainly associated with micropores. Samples with higher TOC content, higher quartz content and lower clay content tend to contain more heterogeneous micropores, resulting in higher fractal dimensions and more complicated pore structure in shales. Therefore, fractal dimension is an effective parameter to reflect the complexity of pore structure and the degree of micropore development in O3w-S1l shale.