Determination of the Thickness and Fracture Toughness of Shale Interfacial Transition Zone Near Various Micromineral Aggregates Using Nano-Scratch Tests

Heterogeneously distributed micromineral aggregates (MMAs) are common in shale reservoirs. The interfaces between these MMAs and the surrounding minerals significantly affect fracture propagation behaviors during shale oil exploitation. In this paper, the concept of interfacial transition zone (ITZ) between the MMAs (e.g., striped barite, pyrite, calcite, apatite blocks, and bedding plane) and the surrounding mineral in shale is introduced. Due to the small thickness of the ITZ, its thickness and mechanical properties are very difficult to determine by traditional standard methods. To address this issue, this paper proposes a method combining nano-scratch tests, scanning electron microscopy (SEM), and quantitative evaluation of minerals by SEM (QEMSCAN) techniques to investigate the thickness and fracture toughness of the ITZ near typical MMAs. The results show that the thickness of the ITZ determined by the transverse force FT and scratch depth (-d2) varies from 3.2 μm to 17.3 μm. In addition, the fracture toughness of both MMAs and ITZs is characterized by high heterogeneity ranging from 0.1 MPa·m0.5 to 2.1 MPa·m0.5. Moreover, a formula evaluating the fracture toughness of the ITZ is proposed taking into account the type and content of minerals in the ITZ. A strong linear relationship is observed between the thickness of the ITZ and the average fracture toughness ratio. In addition, a relationship is established between the fracture toughness of the ITZ and MMAs, and an evaluation equation is derived. This study is helpful for understanding the characteristics (i.e., mainly thickness and fracture toughness) of the ITZ within shales.