MaPM i c r o s t r u c t u r e a n d P o r e s

MaPMicrostructure and Pores GmbH

Microstructure

and

PORES

We are a team of professionals for multi-scale gigapixel material analyses

METHODSWe offer highly accurate multi-scale microstructural

investigations of challenging geological, chemical and biological samples down to nanometer resolution. Our analyses combine cutting-edge preparation method-

ologies with automated processing of the Gigapixel image maps in the cm- to nm-scale for porosity,

3D pore connectivity, pore fluid and

microstructural assessment.

WHY USOur 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-pro-

cessing 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.

Ready to start?

contactinfo@m-a-p.expert

MaP - Microstructure and Pores GmbH phone +49 241 8098445

Lochnerstraße 4-20 52064 Aachen

Germany

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PORE IMAGING

LIQUID METAL INJECTION

CRYO PREPARATION

& IMAGING

7

GIGAPIXEL IMAGE

PROCESSING

cooled with

liquid nitrogen

DOWN TO

-160°C

Find all of our publications at m-a-p.expert

Research projects, carried out using our BIB-SEM, LMI-BIB-SEM, and Cryo-BIB-SEM 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:

Reference projects

selected PublicationsSchmatz, J., Urai, J.L., Berg, S., Ott, H., 2015. Nano-scale imaging of pore-scale fluid-fluid-solid contacts in sandstone. Geo-

physical Research Letters, 2015GL063354.

Klaver, J., Hemes, S., Houben, M., Desbois, G., Radi, Z., Urai, J.L., 2015. The connectivity of pore space in mudstones: insights from high-pressure Wood’s metal injection, BIB-SEM imaging, and mercury intrusion porosimetry. Geofluids, 15, 577-591.

Hemes, S., Desbois, G., Urai, J.L., Schröppel, B., Schwarz, J.-O., 2015. Multi-scale characterization of porosity in Boom Clay (HADES-level, Mol, Belgium) using a combination of X-ray μ-CT, 2D BIB-SEM and FIB-SEM tomography. Microporous and Mesoporous Materials 208, 1-20.

Klaver, J., Desbois, G., Littke, R., Urai, J.L., 2015. BIB-SEM characterization of pore space morphology and distribution in post-mature to overmature samples from the Haynesville and Bossier Shales. Marine and Petroleum Geology 59, 451-466.

Desbois, G., Urai, J.L., Pérez-Willard, F., Radi, Z., Offern, S., Burkart, I., Kukla, P.A., Wollenberg, U., 2013. Argon broad ion beam tomography in a cryogenic scanning electron microscope: a novel tool for the investigation of representative microstruc-tures in sedimentary rocks containing pore fluid. Journal of Microscopy 249, 215-235.

Giffin, S., Littke, R., Klaver, J., Urai, J.L., 2013. Application of BIB–SEM technology to characterize macropore morphology in coal. International Journal of Coal Geolology 114, 85-95.

Houben, M.E., Desbois, G., Urai, J.L., 2013. Pore morphology and distribution in the Shaly facies of Opalinus Clay (Mont Terri, Switzerland): Insights from representative 2D BIB–SEM investigations on mm to nm scale. Applied Clay Science 71, 82-97.

Klaver, J., Desbois, G., Urai, J.L., Littke, R., 2012. BIB-SEM study of the pore space morphology in early mature Posidonia Shale from the Hils area, Germany. International Journal of Coal Geolology 103, 12-25.

Desbois, G., Urai, J.L., Kukla, P.A., Konstanty, J., Baerle, C., 2011. 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 cross-sectioning and SEM imaging. Journal of Petroleum Science and Engineering 78, 243-257.

Desbois, G., Urai, J.L., Kukla, P.A., 2009. Morphology of the pore space in claystones - evidence from BIB/FIB ion beam sec-tioning and cryo-SEM observations. eEarth 4, 8.

Network

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.

MaP - Microstructure and Pores GmbH · +49 241 80 98445 · info@m-a-p.expert · www.m-a-p.expert Amtsgericht Aachen · HRB 20536 · USt-ID-Nr. DE306972825 · Geschäftsführung: Dr. Joyce Schmatz, Dr. Johannes Klaver

MaP MaPM i c r o s t r u c t u r e a n d P o r e s M i c r o s t r u c t u r e a n d P o r e s

Cryo FE-SEM

Broad Ion Beam Polisher

CRYO Broad Ion Beam POLISHER

Liquid METAL INJECTION

Virtual polariZing microscope

Gigapixel IMAGE PROCESSING

2D 3D

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 Emis-

sion 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-SEM workflow on the market today. Our second genera-

tion, state-of-the-art facilities enable standardized sample analysis and high-quality image processing at gigapixel resolution.

EquipmentWe 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 avail-able 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.

-160°C

-160°C

Customer ServiceAll 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 model-ing and quality check of basic measurements. Up-scaling is possible based on the multi-scale investigations. FIB-SEM and MicroCT are complementary to our methods and are integrated depending on the requirements. Additional pet-rophysical and petrographic measurements are carried out by our partners.

Send us your samples for a quick-scan or a multi-scale inte-

grated imaging project.

We are a team of professionals for multi-scale gigapixel material analyses

OUR TEAM

Dr. Joyce Schmatz

Geologist

Microstructures in wet rocks

Cryo-BIB-SEM

Microanalytics

Microscopy

Mingze Jiang, MSc.

Algorithm Engineer

Image analysis and

Software development

Dr. Jop Klaver

Geologist

Microstructures of organic-rich shales

BIB-SEM

Metal injection methods

From 2007 onwards the Structural Geology, Tectonics and Geomechanics group of the RWTH Aachen University de-

veloped 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 understand-

ing of fragile and tight materials such as clays, rock salt, oil reservoir sandstone, mudstones, shales and tight sands.

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PORE IMAGING

METAL INJECTION ANALYSIS

CRYO PREPARATION

& IMAGING

7

GIGAPIXEL IMAGE

PROCESSING

current researchNew 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-SEM extends the basic standard methods in SCAL (Special Core Analysis).

Prof. Dr. Janos L. Urai

Chair of Structural Geology, Tectonics

and Geomechanics, Geological Institute,

RWTH Aachen University

Advisor

Business Economist

Sales and

Business Development

MaP MaPM i c r o s t r u c t u r e a n d P o r e s M i c r o s t r u c t u r e a n d P o r e s

gigapixel pore-, Fabric-, and Element mapS

preparation of delicate samples

1 μm

BROKEN CLAY Surface

SESE

How

Combining Broad Ion Beam (BIB) sputtering with Scanning Electron Microscopy (SEM) imaging including topography-, phase-, and chemical- mapping using Secondary Electrons (SE), Backscattered Electrons (BSE) 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.

Microstructure and Pore analysis

s

PORE IMAGING

10 μm10 μm

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

GIGAPIXEL image of pores in carbonate

15 μm 300 nm

Carbonate Porosity at Pore-Scale

Ion-PolishED clay SURFACE

BEFORE AFTER

Microstructure and pore analysisMaterials

Our microstructure and pore analyses are applied particu-

larly on heterogeneous and fine-grained geological materi-als 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-SEM methodology. This friction-free argon ion sample preparation method is especially well-suited for delicate samples.

SE

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PORE IMAGING

1

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13 18 26 36 51 72 102

144

204

289

409

578

817

1155

1634

2311

3268

4622

6536

Freq

uenc

y [-]

Equivalent pore diameter [nm]

Micro-cracksOrganic-matter poresMatrix pores

0,0%

0,5%

1,0%

1,5%

2,0%

2,5%

3,0%

10 100 1000 10000

Poro

sity

Pore diameter [nm]

Matrix poresOrganic-matter pores

Visible porosity

BSE

5 μm

SE BSE

Processed-EDS

10,000’s of pores

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1000

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13 18 26 36 51 72 102

144

204

289

409

578

817

1155

1634

2311

3268

4622

6536

Freq

uenc

y [-]

Equivalent pore diameter [nm]

Micro-cracksOrganic-matter poresMatrix pores

0,0%

0,5%

1,0%

1,5%

2,0%

2,5%

3,0%

10 100 1000 10000

Poro

sity

Pore diameter [nm]

Matrix poresOrganic-matter pores

Pore size distributions

MaP MaPM i c r o s t r u c t u r e a n d P o r e s M i c r o s t r u c t u r e a n d P o r e s

Injection pressure vs. Pore throat ∅

LM-filled Nano-pore throatLM-filled samples

connected pore network revealed by LMI-BIB-SEM

0

80

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Inje

cti

on

pre

ssu

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Pa]

Time →

Intr

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ore

th

roat

dia

mete

r [n

m]

Intrusion Ø

Pressure

10 nm

5 μm

100 nm

LIQUID METAL INJECTION

3 mm

Connected porosity vs. pore size

Injected Pores in soft clay

12,76615 3,2E-2318,05407 3,4E-2325,53231 5,5E-2336,10813 1,8E-2251,06461 5,9E-2272,21627 2,1E-21102,1292 7,0E-21144,4325 2,0E-20204,2584 5,5E-20288,8651 1,1E-19408,5169 2,1E-19577,7301 2,4E-19817,0338 2,3E-191155,46 1,6E-19

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Inje

ctio

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essu

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Pa]

Time →

Intr

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re t

hroa

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diam

eter

[nm

]

Intrusion Ø

Pressure0%

1%

2%

3%

10 100 1000 10000

Conn

ecte

d po

rosi

ty

Pore diameter [nm]

1,E-25

1,E-23

1,E-21

1,E-19

1,E-17

1,E-15

10 100 1000 10000

Esti

mat

ed p

erm

eabi

lity

[m2 ]

Pore diameter [nm]

<- Effective pore throat diameter

segmented Metal-Injected Pores in Shale with DETAIL SHOWING INJECTED FOSSIL

5 μm

BSE

LIQUID METAL INJECTION

10 μm

BSE

2 μm

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 diam-

eter which can be filled depends on the injection pressure, following the Washburn equation. After the desired injec-tion 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.

Applications

Characterization of the connected pore network at nanome-

ter resolution on a representative sample scale.

Pore connectivity analysis

BSE

BSE

Products

Using our liquid metal injection method we provide, next to the standard microstructure and pore analysis the follow-

ing:

Pore connectivity analyses

Effective porosity

3D Pore connectivity

Percolation threshold

Porosity and permeability assessment

LMI supersedes the conventional Mercury Intrusion Poro-

simetry (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 capil-lary tube model, based on the effective porosity and the percolation threshold gained from the image data.

Materials

This LMI followed by BIB-SEM methodology can be applied on any fine-grained geological material or nano-material with sub-millimeter pore throats.

Pore connectivity analysis

MaP MaPM i c r o s t r u c t u r e a n d P o r e s M i c r o s t r u c t u r e a n d P o r e s

Fluid Map: In-Situ Fluid Distribution and EOR Screening

1 μm

BSE

Freeze Fracturing

5 μm

SE EDS

BSE

SE

3.5 μm

Phase Mapping

Nanoscale Contact Angle

25 μm

BSE

0%

5%

10%

15%

20%

25%

Fre

qu

en

cy

Oil Droplet size [µm2]

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100

150

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18

36

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72

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Nu

mb

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Contact angle [o]

Statistical Analysis

SEGMENTED

BSE

EDS

15 µm

25 µm

500 nm

Quartz

Feldspar

Cement

water (blue)

water (blue) Cement

Pore fluid analysEsHow

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 prepara-

tion 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.

CRYO PREPARATION

& IMAGING

Products

Our unique cutting-edge Cryo-BIB-SEM method allows the imaging and investigation of the fluid-filled pores and mea-

suring through a FluidMap the direct in-situ:

Fluid Chemistry

Wettability

Fluid Distribution

Fluid Saturation

This cutting-edge technology opens new fields of research such as EOR screening or core and formation damage evalu-

ation on fresh samples, such as cuttings.

CRYO-BIB-SEm

CRYO PREPARATION

& IMAGING

Materials

Cryo-BIB-SEM microstructural investigations are applied particularly on wet heterogeneous and fine-grained geologi-cal 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-SEM methodology.

Cryo Preparation

Cryo-Vacuum-TransferCryo-Saw with Load Lock

Saturation Map in Carbonate Reservoir

Cryo-Stabilized Cement Paste - Element Map

MaP MaPM i c r o s t r u c t u r e a n d P o r e s M i c r o s t r u c t u r e a n d P o r e s

Pore size distribution

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Pore area [µm2]

Integrated Multi-scale imaging and Quantitative Analysis

cm- to nm-scale

Integrated VIP-SEM-EDS Analysis

300 μm

0.5 mm

1 μm

VIP - Virtual POLARISING MICROSCOPyProducts

Image data

Transmitted light maps

Polarized light maps

Reflected light maps

Pore analysis

Visible porosity

Pore size distributions

Pore shape and orientation

Surface area and roughness

Autom. quantified mineralogy

Grain size distributions

Mineral fabric

Data storage

Digital thin section libraries

Interpretation stored with

thin section

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 trans-

parent reporting. Integrated studies using the combination of the VIP with BIB-SEM 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.

Carbonate thin section:more than 200.000 pores classified, 16.4 % porosity

EDS

SEVIP

Multi-Task OpticaL mICROSCOPY

Analyze and Annotate Your Samples

dIGITAL vIEWER

iNTEGRATED pHASE sEGMENTATION

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-SEM. Applications

Multi-scale, quantitative analysis of petrophysical attributes, automated analysis of sections, digital library.

VIP - Virtual POLARISING MICROSCOPy

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PORE IMAGING

Halite

Olivine

Anhydrite

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PORE IMAGING