Effective production of oil from carbonate reservoirs often requires the application of improved oil recovery technologies such as waterflooding. However, conventional waterflooding in carbonates usually results in low hydrocarbon recovery as most of these formations exhibit a complex pore throats structure and are mostly oil-wet. Therefore, improved insight into the causes of hydrophobic wetting behavior of such reservoirs is important for understanding the fluid distribution, displacement and enhancing recovery processes. The characterization of fluid-rock interactions is, however, challenging with existing laboratory methods, which are typically based on macroscale (mm) observations. In this experimental study, an advanced imaging technique, namely environmental scanning electron microscope, was applied for the comprehensive investigation of microscale (µm) wettability variations in carbonate rocks covered with organic layers. For the first time, the presence of organic layers on the sample was proved using energy dispersive X-ray mapping. Furthermore, the chemical bond of this layer and carbonate rock surfaces was determined using the transmission electron microscopy and electron energy-loss spectroscopy. The thickness of layer was estimated by using image processing software. These findings show that the application of combined microscopic techniques reveals important details about the reason of hydrophobic wetting properties of real carbonate rocks.

More than a half of world's hydrocarbon reserves is presented in carbonate reservoirs. Conventional waterflooding leads to inefficient oil recovery from these reservoirs, because majority of them have mixed or oil-wet wetting properties. It is well documented in literature, that the main reason of oil wetness of carbonate rocks is adsorbed components from crude oil. Although progress has been made in determination of oil components, which have a tendency to react with carbonates, carbonate reservoirs development still remains challenging. Hence, in this study we investigated the distribution of adsorbed oil components on rock surfaces in order to define their influence on fluids flow through porous carbonate samples. This work presents the results for several carbonate core samples taken from the oil zone of an oil reservoir, which mostly consist of calcite with the small impurities of magnesite and quartz. The work provides the standard study of pore structure of samples to assess the solvents influence on pore network of samples using μCT; the method of evaluation of the amount of organic matter adsorbed on calcite using Rock - Eval pyrolysis; the visualization of such matter distribution through samples; and also the results of kinetics experiments in order to evaluate the bond disruption energy between organic matter and surface. Studies have shown that combination of pyrolysis and μCT provides comprehensive and improved data about organic matter.

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Wettability of sedimentary rock surface is an essential parameter that defines oil recovery and production rates of a reservoir. The discovery of wettability alteration in reservoirs, as well as complications that occur in analysis of heterogeneous sample, such as shale, for instance, have prompted scientists to look for the methods of wettability assessment at nanoscale. At the same time, bulk techniques, which are commonly applied, such as USBM (United States Bureau of Mines) or Amott tests, are not sensitive enough in cases with mixed wettability of rocks as they provide average wettability values of a core plug. Atomic Force Microscopy (AFM) has been identified as one of the methods that allow for measurement of adhesion forces between cantilever and sample surface in an exact location at nanoscale. These adhesion forces can be used to estimate wettability locally. Current research, however, shows that the correlation is not trivial. Moreover, adhesion force measurement via AFM has not been used extensively in studies with geological samples yet. In this study, the adhesion force values of the cantilever tip interaction with quartz inclusion on the shale sample surface, have been measured using the AFM technique. The adhesion force measured in this particular case was equal to the capillary force of water meniscus, formed between the sample surface and the cantilever tip. Experiments were conducted with a SiconG cantilever with (tip radius of 5 nm). The adhesion forces between quartz grain and cantilever tip were equal to 56.5 ± 5 nN. Assuming the surface of interaction to be half spherical, the adhesion force per area was 0.36 ± 0.03 nN/nm2. These measurements and results acquired at nano-scale will thus create a path towards much higher accuracy-wettability measurements and consequently better reservoir-scale predictions and improved underground operations.

The theoretical principles of the laboratory methods for studying the wettability of unconventional oil formation rocks are discussed and examples of their practical implementation are presented. The comparative analysis of the advantages and disadvantages of each method is presented. It is shown that despite the recent progress in the development of methods for determining the wettability of rocks, they still need to be improved. Examples of their possible improvements are discussed.

The wettability of a reservoir rock is one of the most essential parameters in oil and gas recovery applications and gas storage schemes. However, bulk techniques, which are commonly used to analyse rock wettability, for example the United States Bureau of Mines test, are not sensitive enough to probe mixed-wettability scenarios. Furthermore, these measurements are conducted at millimetre–centimetre scale, while wettability is determined at the atomic scale, and some rocks (e.g. shale) have a very fine structure even at nanoscale. Additionally, in the case of shale rocks, standard wettability measurements cannot be applied due to their extremely low permeability. To overcome these limitations, wettability can be directly measured at the nanoscale with advanced analytical methods, such as scanning electron microscopy (SEM) and atomic force microscopy (AFM). While such techniques are well-established in various disciplines, there exists no standard procedure for rock wettability analysis at nanoscale. Thus, this study elaborates on the optimal methods that can be used for the preparation of an AFM-cantilever-rock grain sample, with which the rock wettability can be measured at atomic scale. Therefore, this work aids in the wider-scale implementation of AFM as a rock wettability measurement tool.