How to avoid multiple scattering in strongly scattering SANS and USANS samples

With the rapid development of unconventional oil and gas, the pore structure characterization of shale reservoirs has attracted an increasing attention. High pressure mercury intrusion porosimetry (HPMIP) has been widely used to quantitatively characterize the pore structure of tight shales. However, the pore structure obtained from HPMIP could be significantly affected by the sample particle size used for the analyses. This study mainly investigates the influence of shale sample particle size on the pore structure obtained from HPMIP, using Mississippian-aged Barnett Shale samples. The results show that the porosity of Barnett Shale samples with different particle sizes obtained from HPMIP has an exponentially increasing relation with the particle size, which is mainly caused by the new pores or fractures created during shale crushing process as well as the increasing exposure of blind or closed pores. The amount and proportion of mercury retention during mercury extrusion process increase with the decrease of shale particle size, which is closely related to the increased ink-bottle effect in shale sample with smaller particle size. In addition, the fractal dimension of Barnett Shale is positively related to the particle size, which indicates that the heterogeneity of pore structure is stronger in shale sample with larger particle size. Furthermore, the skeletal density of shale sample increases with the decrease of particle size, which is possibly caused by the differentiation of mineral composition during shale crushing process.

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Effect of Shale Sample Particle Size on Pore Structure Obtained from High Pressure Mercury Intrusion Porosimetry

Comparative characterization of sandstone microstructure affected by cyclic wetting-drying process

The Influence of Analytical Particle Size on the Pore System Measured by CO2, N2, and Ar Adsorption Experiments for Shales

The pore connectivity of shale directly affects the migration and distribution of oil and gas within shale reservoirs and controls the adsorption state of shale gas by determining the accessible pore spaces for methane molecules. However, previous studies mostly focused on the surficial properties, pore size, and specific surface area, ignoring the significant impact of pore connectivity on the adsorption state of shale gas. Accordingly, taking the continental shale of the Jurassic Ziliujing Formation from the northeastern Sichuan Basin as the research object, this study mainly investigates the effects of shale pore connectivity on the adsorption state of shale gas by conducting methane adsorption and field emission scanning electron microscopy experiments together with image processing software. The results show that the methane adsorption capacity per unit specific surface area of type III kerogen is higher than that of type II2 kerogen, indicating type III kerogen has a stronger affinity to methane. However, the total methane adsorption capacity of type II2 kerogen in Ziliujing Formation shale samples is about four times that of type III kerogen, which is due to the much higher specific surface area, providing more methane adsorption sites. The development of OM and clay minerals in the shale of the Ziliujing Formation has a certain orientation and promotes the pore connectivity of the shale. Furthermore, a better pore connectivity of shale samples, which is usually accompanied by more developed microfractures of OM and clay minerals, higher roughness of pore surface, and stronger randomness of pore arrangement, results in a stronger methane adsorption capacity. Based on the close relationship between pore connectivity and methane adsorption capacity, a new pore connectivity index is proposed, considering the difference between the actual and the theoretical methane adsorption capacity of shale samples. Finally, a shale methane adsorption model is established based on pore connectivity. 

Controlling Effect of Shale Pore Connectivity on the Adsorption State of Shale Gas: A Case Study of Continental Shale of Jurassic Ziliujing Formation, Sichuan Basin

The sample size or particle size of shale plays a significant role in the characterization of pores by various techniques. To systematically investigate the influence of particle size on pore characteristics and the optimum sample size for different methods, we conducted complementary tests on two overmature marine shale samples with different sample sizes. The tests included small-angle neutron scattering (SANS), gas (N2, CO2, and H2O) adsorption, mercury injection capillary pressure (MICP), and field emission-scanning electron microscopy (FE-SEM) imaging. The results indicate that artificial pores and fractures may occur on the surface or interior of the particles during the pulverization process, and some isolated pores may be exposed to the particle surface or connected by new fractures, thus improving the pore connectivity of the shale. By comparing the results of different approaches, we established a hypothetical model to analyze how the crushing process affects the pore structure of overmature shales. Our results imply that intact wafers with a thickness of 0.15–0.5 mm and cubic samples (~1 cm3) are optimal for performing SANS and MICP analyses. Meanwhile, the 35–80 mesh particle size fraction provides reliable data for various gas physisorption tests in overmature shale. Due to the intrinsic heterogeneity of shale, future research on pore characteristics in shales needs a multidisciplinary approach to obtain a more comprehensive, larger scale, and more reliable understanding.

Effect of Particle Size on Pore Characteristics of Organic-Rich Shales: Investigations from Small-Angle Neutron Scattering (SANS) and Fluid Intrusion Techniques

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Effect of Particle Size on Pore Characteristics of Organic-Rich Shales: Investigations from Small-Angle Neutron Scattering (SANS) and Fluid Intrusion Techniques