Integration of Multiscale Imaging of Nanoscale Pore Microstructures in Gas Shales

Quantification of the microstructures of shales is difficult due to their complexity which extends across many orders of magnitude of scale. Nevertheless, shale microstructures are extremely important, not only as shale gas resources but also as cap rocks in CCS resources, in geothermal reservoirs, and as a host to the long-term storage of radioactive materials. In this work, we have performed ultrahigh-resolution CT imaging (nano-CT), mercury injection porosimetry (MIP), and nitrogen adsorption experiments on a sample of gas shale for which we already have focused ion beam scanning electron microscopy (FIB-SEM) and high-resolution CT (micro-CT) data sets. The combination of these data sets has allowed us to examine the microstructure of the shale in unprecedented depth across a wide range of scales (from about 20 nm to 0.5 mm). Overall, the sample shows a porosity of 0.67 +/- 0.009% from the nano-CT data, 0.0235 +/- 0.003% from nitrogen adsorption, and 0.60 +/- 0.07% from MIP, which compare with 0.10 +/- 0.01%, 0.52 +/- 0.05%, and 0.94 +/- 0.09% from three FIB-SEM measurements and 0.06 +/- 0.008% from one micro-CT measurement. The data vary due to the different scales at which each technique interrogates the rock and whether the pores are openly accessible (especially in the case of the nitrogen adsorption value). The measured kerogen fraction is 32.4 +/- 1.45% from nano-CT compared with 34.8 +/- 1.74%, 38.2 +/- 1.91%, 41.4 +/- 2.07%, and 44.5 +/- 2.22% for three FIB-SEM and one micro-CT measurement. The pore size imaged by nano-CT ranged between 100 and 5000 nm, while the corresponding ranges were between 3 and 2000 nm for MIP analysis and between 2 and 90 nm for N-2 adsorption. The distribution of pore aspect ratio and scale-invariant pore surface area to volume ratio (sigma) as well as the calculated permeability shows the sample to have a high shale gas potential. Aspect ratios indicate that most of the pores that contribute significantly to pore volume are oblate, which is confirmed by the range of s (3-13). Oblate pores have greater potential for interacting with other pores compared to equant and needle-shaped prolate pores as well optimizing surface area for gas to desorb from the kerogen into the pores. Permeability essays provide 2.61 +/- 0.42 nD from the nano-CT data, 2.65 +/- 0.45 nD from MIP, and (5.07 +/- 0.02) x 10(-4) nD from nitrogen adsorption, which are consistent with expectations for generic gas shales (i.e., tens of nD) and the measurements made previously on the same sample using FIB-SEM and micro-CT imaging techniques.

Automated summary

Quantification of shale microstructures across a wide range of scales is challenging due to the complexity of the material. This study employed various techniques such as nano-CT, MIP, and nitrogen adsorption to analyze the microstructure of a gas shale sample, revealing differences in porosity and kerogen fraction measurements. The results suggest high shale gas potential based on pore size distribution, aspect ratio, and permeability assessments.