map - microstructure and pores gmbh microstructure...from 2007 onwards the structural geology,...
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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?
MaP - Microstructure and Pores GmbH phone +49 241 8098445
Lochnerstraße 4-20 52064 Aachen
Germany
s
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 · [email protected] · 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.
s
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
s
PORE IMAGING
1
10
100
1000
10000
100000
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
1
10
100
1000
10000
100000
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
160
240
320
0
20
40
60
Inje
cti
on
pre
ssu
re [M
Pa]
Time →
Intr
usio
n p
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
0
80
160
240
320
0
20
40
60
Inje
ctio
n pr
essu
re [M
Pa]
Time →
Intr
usio
n po
re t
hroa
t
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]
0
50
100
150
200
250
300
350
400
450
500
0
18
36
54
72
90
10
8
12
6
14
4
16
2
18
0
Nu
mb
er
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
1
10
100
1000
10000
100000
1000000
Fre
qu
en
cy [-]
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
s
PORE IMAGING
Halite
Olivine
Anhydrite
s
PORE IMAGING