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Journal of the Australian Petroleum Production & Exploration Association (APPEA)
RESEARCH ARTICLE

Sample preparation for rock wettability studies via atomic force microscopy

Nikolai A. Mitiurev A D , Michael Verrall B , Anastasia A. Ivanova C , Alireza Keshavarz A and Stefan Iglauer A
+ Author Affiliations
- Author Affiliations

A Edith Cowan University, 270 Joondalup Drive, Joondalup, WA 6027, Australia.

B Commonwealth Scientific and Industrial Research Organisation, 26 Dick Perry Avenue, Kensington, WA 6151, Australia.

C Skolkovo Institute of Science and Technology, Moscow, 121205, Russia.

D Corresponding author. Email: nmitiurev@gmail.com

The APPEA Journal 61(1) 216-223 https://doi.org/10.1071/AJ20083
Submitted: 13 January 2021  Accepted: 11 February 2021   Published: 2 July 2021

Abstract

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.

Keywords: wettability, atomic force microscopy, scanning electron microscopy, AFM, SEM, tipless cantilever, methodology, pitfalls, micromanipulators, hydrocarbon production, oil recovery.

Nikolai A. Mitiurev graduated from the Moscow State University, Chemistry department, in 2015 with specialisation in Petroleum Chemistry. After that, he was involved in several industrial research projects of Russian oil companies (Gaspromneft, Permnipineft, Lukoil, Vniineft, Zarubezhneft). During this time, he worked on projects related to the study of kerogen chemical properties and structure using Rock-Eval, solid-state nuclear magnetic resonance spectrometry and X-ray photoelectron spectroscopy and to the study of crude oil composition using Fourier transform–ion cyclotron resonance mass spectrometry. The last project was devoted to the study of a film of organic matter adsorbed on carbonate surface, which altered the wettability of rock. He is currently enrolled in a PhD candidature in Edith Cowan University (ECU), School of Engineering in 2020, with his thesis relating to the investigation of the impact of adsorbed organic matter on the surface wettability of using AFM and SEM.

Michael Verrall is a Senior Research Scientist and Manager of the Electron Beam and X-ray Laboratories at the Australian Resource Research Centre for CSIRO. The laboratories provide researchers with access to state-of-the-art equipment for characterisation of materials of interest to resource sector and relighted industries. His interests are in scientific instrumentation and developing SEM and X-ray based techniques for automated mineralogy. Michael has a degree in physics and previous experience working in the mining industry. He also works as a Radiation Safety Officer for CSIRO.

Anastasia A. Ivanova is a Research Scientist in the Skolkovo Institute of Science and Technology. She was enrolled in the joint PhD program between Curtin University, Perth, Australia and the Skolkovo Institute of Science and Technology, Moscow, Russia in 2020 and defended her thesis, ‘Dynamic Modelling and Experimental Evaluation of Nanoparticles Application in Surfactant Enhanced Oil Recovery’, in 2020. Her research focuses on micro- and macro-wettability of rocks, interfacial phenomenon, surfactant flooding and nanoparticles augmented surfactant flooding. Her research combines both experimental and dynamic modelling approaches. She collaborated in more than five projects as a Research Fellow at the Skolkovo Institute of Science and Technology, funded by industrial companies. The results of her research were published in five internationally respected journals and in more than 10 abstracts in international conferences.

Alireza Keshavarz has completed PhD degree in Petroleum Engineering from the University of Adelaide, Australia, in 2015. He has completed his MSc in Reservoir Engineering from the University of Tehran, Iran, in 2007 and a BSc in Chemical-Petroleum Engineering from Petroleum University of Technology, Iran, in 2002. He is currently working as a Senior Lecturer at the School of Engineering, ECU, Australia, since October 2016. His research interests focus on enhanced oil and gas recovery from conventional and unconventional reservoirs, drilling fluids rheology, CO2 and hydrogen storage, liquid nitrogen fracturing in coal cleat network and nano-energy applications.

Stefan Iglauer received his Diplom-Chemiker degree from Paderborn University in 1998 and his PhD in Engineering from Oxford Brookes University in 2002. Afterward, he joined the California Institute of Technology and subsequently the Imperial College London as a Research Fellow. In 2011, he moved to Australia as an academic where he first joined Curtin University, and since February 2018 ECU, where he is now a Professor of Petroleum Engineering. His research focuses on nano-energy applications, CO2 and hydrogen storage, flow through porous media, general energy production and climate change mitigation.


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