Nano-scale experimental investigation of in-situ wettability and spontaneous imbibition in ultra-tight reservoir rocks

We investigated spontaneous imbibition behavior, three-dimensional fluid occupancy maps, and in-situ wettability at the nano scale in five ultra-tight and shale reservoir rock samples. For this purpose, we developed a novel technique by integrating a custom-built in-situ miniature fluid-injection module with a non-destructive high-resolution X-ray imaging system. Small cylindrical core samples (15-60 mu m in diameter) were prepared from reservoir rocks using Focused-Ion Beam (FIB) milling technique. The pore network inside the samples were first characterized using ultra-high resolution three-dimensional images obtained at initial state by X-ray nano-tomography (Nano-CT) and FIB-Scanning Electron Microscopy (FIB-SEM) techniques at the nano scale. The petrophysical parameters, including porosity, permeability, poresize distribution, and organic content were computed for each sample using image analysis. We then performed series of imbibition experiments using brine, oil, and surfactant solutions on each core sample. We observed that both oil and brine phases spontaneously imbibe into the pore network of the rock samples at various quantities. We also, for the first time, examined fluid distribution in individual pores and found a complex wettability behavior at the pore scale in the reservoir rock samples. Three pore types were identified with water-wet, oil-wet, and fractionally-wet behaviors. This work opens a new path to developing an improved understanding of the pore-level physics involved in multi-phase flow and transport not only in tight rock samples but also in other nanoporous material used in different science and engineering applications. Published by Elsevier Ltd.