Microstructure and PORES

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1 Ready to start? contact phone Lochnerstraße Aachen Germany Microstructure and PORES cooled with liquid nitrogen DOWN TO -160 C We are a team of professionals for multi-scale gigapixel material analysis METHODS We offer highly accurate multi-scale microstructural investigations of challenging geological, chemical and biological samples down to nanometer resolution. Our analyses combine cutting-edge preparation methodologies with automated processing of the Gigapixel image maps in the cm- to nm-scale for porosity, 3D pore connectivity, pore fluid and microstructural assessment. s PORE IMAGING LIQUID METAL INJECTION WHY US Our offering includes unique in-situ analysis of extremely sensitive materials including pore fluids, possible through experience in handling challenging geological, chemical and biological materials. Our highly automated post-processing suite enables generating representative data at a range of scales with high accuracy and resolution. MaP combines twenty years of experience in a wide area of applications of nano- and microstructural research. CRYO PREPARATION & IMAGING 7 GIGAPIXEL IMAGE PROCESSING

2 Equipment The unique combination of a multi-scale Gigapixel workflow consisting of our Virtual Polarised Microscope (ViP), Argon Cryo Broad Ion Beam polishers, state-of-the-art Field Emission Cryo Scanning Electron Microscope and Liquid Metal Injection technology and researchers having over twenty years of experience makes our lab one-of-a-kind in the world. We developed the first and only fully integrated Cryo- BIB-M workflow on the market today. Our second generation, state-of-the-art facilities enable standardized sample analysis and high-quality image processing at gigapixel resolution. We are experts in our fields, engaging in cutting-edge research and regularly publishing in top peer-reviewed journals. Our knowledge is ahead of the curve and enables us to focus on only the most promising methods and to invest in the best equipment. Equipment which is not available yet off-the-shelf is developed in close cooperation with vendors and the engineering institutes of the RWTH Aachen University. Our network and customer-oriented approach give us the ability to deliver custom solutions for demanding projects even within a short time-frame. Virtual polarizing microscope Broad Ion Beam Polisher -160 C CRYO Broad Ion Beam POLISHER Cryo FE-M -160 C Liquid METAL INJECTION Gigapixel IMAGE PROCESSING

3 Microstructure and Pore analysis How Combining Broad Ion Beam (BIB) sputtering with Scanning Electron Microscopy (M) imaging including topography-, phase-, and chemical- mapping using Secondary Electrons (), Backscattered Electrons () and Energy Dispersive X-ray Spectroscopy (EDS). The argon ion sputtered surface allows Gigapixel imaging at nano-scale resolution of the polished microstructure followed by image processing and analysis. Applications High-resolution microstructural analysis of heterogeneous materials such as tight rock samples from core plugs and cuttings at a representative scale. Products Gigapixel image maps Pore Map Fabric Map Element Map Pore analyses Visible porosity Pore size distributions Pore shape and orientation Surface area Surface roughness Quantified mineralogy Grain size distributions Mineral fabric Organic-matter fraction/ distributions Advanced analyses Organic-matter porosity Mineral phase porosity Inter-/intraparticle porosity Inferred porosity and permeability Diagenesis s PORE IMAGING BEFORE AFTER 10 μm 10 μm BROKEN CLAY Surface Ion-PolishED clay SURFACE 15 μm 300 nm GIGAPIXEL image of pores in carbonate Carbonate Porosity at Pore-Scale

4 Microstructure and pore analysis Materials Our microstructure and pore analyses are applied particularly on heterogeneous and fine-grained geological materials such as shales or tight sands. With the processing power of our software suite it is possible to analyse representative gigapixel sample cross sections at multi-scale resolution. All materials with microstructural properties such as cements for construction, conductive coatings and membranes for filtration applications are also investigated using our BIB-M methodology. This friction-free argon ion sample preparation method is especially well-suited for delicate samples. 1 μm preparation of delicate samples s PORE IMAGING 10,000 s of pores 5 μm gigapixel pore-, Fabric-, and Element maps Processed-EDS Porosity 3,0% Matrix pores 2,5% Organic-matter pores 2,0% 1,5% 1,0% 0,5% 0,0% Pore diameter [nm] Visible porosity Frequency [-] Micro-cracks Organic-matter pores Matrix pores Equivalent pore diameter [nm] Pore size distributions

5 MaP LIQUID METAL INJECTION Injection pressure [MPa] How During Liquid Metal Injection (LMI) the fusible alloy intrudes into and fills the connected pore network. The degree of percolation depends on the critical pore throat diameter in the porous medium. The minimum pore throat diameter which can be filled depends on the injection pressure, following the Washburn equation. After the desired injection pressure is reached, the sample is cooled down under pressure and the metal solidifies in the pore space. The subsequent microstructure and pore investigation allows identifying the connected pore space and interrogating the 3D pore network Intrusion Ø Pressure Intrusion pore throat diameter [nm] Pore connectivity analysis 0 Time Injection pressure vs. Pore throat Applications Characterization of the connected pore network at nanometer resolution on a representative sample scale. 5 μm connected pore network revealed by LMI-BIB-M m 10 n 3 mm 100 nm LM-filled samples LM-filled Nano-pore throat

6 Pore connectivity analysis Products Using our liquid metal injection method we provide, next to the standard microstructure and pore analysis the following: LIQUID METAL INJECTION Pore connectivity analyses Effective porosity 3D Pore connectivity Percolation threshold Porosity and permeability assessment LMI supersedes the conventional Mercury Intrusion Porosimetry (MIP) and therefore we can evaluate MIP data as we visualize what part of the pore space is actually being filled with the liquid metal. Moreover, we can investigate the pore space in cracks and correct for potential core damage. Permeability estimation can be obtained by using the capillary tube model, based on the effective porosity and the percolation threshold gained from the image data. Materials This LMI followed by BIB-M methodology can be applied on any fine-grained geological material or nano-material with sub-millimeter pore throats. Connected porosity 10 μm Injected Pores in soft clay 3% 2% 1% 0% Pore diameter [nm] Connected porosity vs. pore size 2 μm 5 μm segmented Metal-Injected Pores in Shale with DETAIL SHOWING INJECTED FOSSIL

7 Pore fluid analyses How Combining Cryo-Broad Ion Beam sputtering with Cryo- Scanning Electron Microscopy and chemical analysis using EDS we are able to image and analyze Cryo-preserved fluids inside pore networks and micro cracks. The Cryo-loading station with Cryo-saw allows performing sample preparation for the Cryo-BIB under LN2 conditions. Applications High-resolution microstructural characterization of wet or soft materials, like oil/brine-filled reservoir rocks, oil shales, tissue, biological materials, polymers, membranes. Products Our unique cutting-edge Cryo-BIB-M method allows the imaging and investigation of the fluid-filled pores and measuring through a FluidMap the direct in-situ: Fluid Chemistry Wettability Fluid Distribution Fluid Saturation CRYO PREPARATION & IMAGING This cutting-edge technology opens new fields of research such as EOR screening or core and formation damage evaluation on fresh samples, such as cuttings. 1 μm Fluid Map: In-Situ Fluid Distribution and EOR Screening EDS 5 μm 3.5 μm Freeze Fracturing Phase Mapping

8 CRYO-BIB-m Materials Cryo-BIB-M microstructural investigations are applied particularly on wet heterogeneous and fine-grained geological materials like clays or reservoir rocks. Other wet and soft materials such as tissue, cements and medical/biological preparations can also be investigated using our Cryo-BIB- M methodology. Cryo-Saw with Load Lock Cryo-Vacuum-Transfer CRYO PREPARATION & IMAGING Cryo Preparation GMENTED 25 µm Saturation Map in Carbonate Reservoir Number Frequency 25% 20% 15% 10% 5% 0% μm nm Nanoscale Contact Angle Contact angle [o] Statistical Analysis Quartz Oil Droplet size [µm 2 ] EDS Feldspar water (blue) water (blue) Cement Cement 15 µm Cryo-Stabilized Cement Paste - Element Map

9 VIP - Virtual POLARISING MICROSCOPy How This system displays mosaic images of thin-sections with 10 nm accuracy at all settings of a conventional polarizing microscope from a highly compressed Gigapixel image file. Using multi-scale automated petrographic analyses we are able to segment fracture networks, minerals, pores and mineral overgrowths. Regions of interest can be selected for enhanced analyses like ion-polishing preparation followed by BIB-M. Applications Multi-scale, quantitative analysis of petrophysical attributes, automated analysis of sections, digital library. digital viewer s PORE IMAGING Multi-Task OpticaL microscopy integrated pha segmentation Analyze and Annotate Your Samples

10 s MaP PORE IMAGING VIP - Virtual POLARISING MICROSCOPy Pore analysis Visible porosity Pore size distributions Pore shape and orientation Surface area and roughness EDS Autom. quantified mineralogy Grain size distributions Mineral fabric Olivine Anhydrite Data storage Digital thin section libraries Interpretation stored with thin section Halite 300 μm Integrated VIP-M-EDS Analysis Customer value Added value of the VIP over conventional optical microscopy is the online expert consultation and rapid analyses. The knowledge-based system enables standardized and transparent reporting. Integrated studies using the combination of the VIP with BIB-M investigations allow assessment of diagenentic relations and multi-scale evaluation of porosity and permeability as well as pore connectivity even offline and remotely, without being physically present in the lab Frequency [-] Products Image data Transmitted light maps Polarized light maps Reflected light maps Pore area [µm2] Pore size distribution VIP 0.5 mm Carbonate thin section: more than pores classified, 16.4 % porosity 1 μm cm- to nm-scale Integrated Multi-scale imaging and Quantitative Analysis

11 Customer Service All tools are complemented by our sophisticated image processing algorithms for high-quality pore segmentation and classification. All analysis results and image data can be accessed and archived with our web-based storage facility. Our analyses are employed in pore characteristics modeling and quality check of basic measurements. Up-scaling is possible based on the multi-scale investigations. FIB-M and MicroCT are complementary to our methods and are integrated depending on the requirements. Additional petrophysical and petrographic measurements are carried out by our partners. Send us your samples for a quick-scan or a multi-scale integrated imaging project. s PORE IMAGING CRYO PREPARATION & IMAGING METAL INJECTION ANALYSIS 7 GIGAPIXEL IMAGE PROCESSING current research New developments are focused on the integration of our imaging tools with various 3D methods to generate Digital Rock models. New developments in Liquid Metal Injection experiments offer a new type in pore connectivity analyses. Cryo-BIB-M extends the basic standard methods in SCAL (Special Core Analysis). 2D 3D We are a team of professionals for multi-scale gigapixel material analysis OUR TEAM Dr. Joyce Schmatz Geologist Microstructures in wet rocks Cryo-BIB-M Microanalytics Microscopy Dr. Jop Klaver Geologist Microstructures of organic-rich shales BIB-M Metal injection methods Mingze Jiang, MSc. Algorithm Engineer Image analysis and Software development Business Economist Sales and Business Development Prof. Dr. Janos L. Urai Chair of Structural Geology, Tectonics and Geomechanics, Geological Institute, RWTH Aachen University Advisor From 2007 onwards the Structural Geology, Tectonics and Geomechanics group of the RWTH Aachen University developed a range of world class methods to characterize the in-situ microstructure of wet and fine-grained rocks. These developments are crucial for a comprehensive understanding of fragile and tight materials such as clays, rock salt, oil reservoir sandstone, mudstones, shales and tight sands.

12 Reference projects Research projects, carried out using our BIB-M, LMI-BIB-M, and Cryo-BIB-M methods were succesfully used in the fields of hydrocarbon exploration and production and the evaluation of salt and clays for long-term storage of nuclear waste, as well as analysis of subsurface integrity for energy storage. These projects comprise pore-scale imaging studies in: Reservoirs and seals Posidonia Shale, Germany; Haynesville and Bossier Shale, USA; Cherts and Carbonates, Middle East; Oil-filled reservoir sandstone; Lacustrine Shales, USA; Niobrara Oil Shale, USA; Rock Salt, Middle East; Tight Gas Sandstone, Germany; Dnieper- Donets Basin Shales, Ukraine; Host rocks Ypresian and Boom Clay, Belgium; Callovian-Oxfordian Clay, France; Opalinus Clay, Switzerland. Network Find all of our publications at m-a-p.expert selected Publications Schmatz, J., Urai, J.L., Berg, S., Ott, H., Nano-scale imaging of pore-scale fluid-fluid-solid contacts in sandstone. Geophysical Research Letters, 2015GL Klaver, J., Hemes, S., Houben, M., Desbois, G., Radi, Z., Urai, J.L., The connectivity of pore space in mudstones: insights from high-pressure Wood s metal injection, BIB-M imaging, and mercury intrusion porosimetry. Geofluids, 15, Hemes, S., Desbois, G., Urai, J.L., Schröppel, B., Schwarz, J.-O., Multi-scale characterization of porosity in Boom Clay (HADES-level, Mol, Belgium) using a combination of X-ray μ-ct, 2D BIB-M and FIB-M tomography. Microporous and Mesoporous Materials 208, Klaver, J., Desbois, G., Littke, R., Urai, J.L., BIB-M characterization of pore space morphology and distribution in postmature to overmature samples from the Haynesville and Bossier Shales. Marine and Petroleum Geology 59, Desbois, G., Urai, J.L., Pérez-Willard, F., Radi, Z., Offern, S., Burkart, I., Kukla, P.A., Wollenberg, U., Argon broad ion beam tomography in a cryogenic scanning electron microscope: a novel tool for the investigation of representative microstructures in sedimentary rocks containing pore fluid. Journal of Microscopy 249, Giffin, S., Littke, R., Klaver, J., Urai, J.L., Application of BIB M technology to characterize macropore morphology in coal. International Journal of Coal Geolology 114, Houben, M.E., Desbois, G., Urai, J.L., Pore morphology and distribution in the Shaly facies of Opalinus Clay (Mont Terri, Switzerland): Insights from representative 2D BIB M investigations on mm to nm scale. Applied Clay Science 71, Klaver, J., Desbois, G., Urai, J.L., Littke, R., BIB-M study of the pore space morphology in early mature Posidonia Shale from the Hils area, Germany. International Journal of Coal Geolology 103, Desbois, G., Urai, J.L., Kukla, P.A., Konstanty, J., Baerle, C., High-resolution 3D fabric and porosity model in a tight gas sandstone reservoir:a new approach to investigate microstructures from mm- to nm-scale combining argon beam crosssectioning and M imaging. Journal of Petroleum Science and Engineering 78, Desbois, G., Urai, J.L., Kukla, P.A., Morphology of the pore space in claystones - evidence from BIB/FIB ion beam sectioning and cryo-m observations. eearth 4, 8.