Pore structure properties in shales, such as pore volume,
specific
surface area, pore size distribution (PSD), and pore connectivity,
are important factors to impact petroleum generation, storage, and
migration. However, research on changes in pore structure during thermal
maturation of shales from transitional deposition environments is
still limited. In this work, a series of hydrous pyrolysis experiments
at temperatures from 250–550 °C were carried out on a
source rock sample from the Lower Permian-aged Shanxi Formation in
the northern Ordos Basin of China. (Ultra)small-angle neutron scattering
[(U)SANS] and low-pressure gas (N2/CO2) adsorption
(LNA/LCA) methods, over a measurable range of 0.35–1000 nm
in pore diameters, were used to analyze the pore properties of the
resultant solids from the pyrolysis experiments, providing data on
the evolution of gas-accessible and gas-inaccessible pores. Both pore
volumes and specific surface areas decreased initially, then increased,
and finally decreased with increasing maturity, reaching their peaks
at 340 and 500 °C, respectively. The ratio of gas-inaccessible
mesopores (2–50 nm in diameter), defined as (SANS-measured
– LNA-measured/SANS-measured mesopores), initially increases,
then decreases, and finally increases again. In shale samples subjected
to the temperatures of 250–340 and 340–380 °C,
the abundance of inaccessible pores 2–18 and 2–50 nm
in diameter increase due to a possible filling of bitumen and generated
oil; in addition, the inaccessible pore percentage at 9–50
nm is decreased at 380–460 °C. A multifractal analysis
was used to interpret (U)SANS PSD data to characterize the heterogeneity
of pore structures at different thermal evolution stages, and the
singularity index α0 and its widths could be considered
as major parameters to distinguish nanopore evolution and heterogeneity
of PSDs from immature to overmature shales.