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HIGH RESOLUTION IMAGING OF POROUS

GEOMATERIALS AND GEOLOGICAL CORES WITH
MICRO COMPUTED X-RAY TOMOGRAPHY

F.H. Kim
1
, D. Penumadu
1
, A. Gu
2
, S. Yun
2
, and J. Gelb
2

1
Civil and Environmental Engineering, University of Tennessee Knoxville, TN 37996
2
Xradia Inc. Pleasanton, CA

This paper was prepared for presentation at the International Symposium of the Society
of Core Analysts held in Aberdeen, Scotland, UK, 27-30 August, 2012

ABSTRACT
High resolution X-ray tomography results of dry and partially water saturated silica sand
specimens compacted to target density are presented. The concept of multi-
resolution/FOV is demonstrated by using two different magnifications (1X and 10X) on
the same specimen. This resulted in high contrast of the water phase compared to the
silica and air phases without using a contrast agent, thus highly desirable for studying
samples from the environment. Direct Numerical Simulations (DNS) using the
tomography data was used to predict capillary pressure versus saturation/suction curve
using full morphology method. An estimation of the capillary pressure of the partially
saturated compacted sand specimen used in the tomography measurements from DNS is
also included.

INTRODUCTION
Geo-materials (sand, silt, clays, and rock cores) are natural materials with complex
properties resulting from three-phases composed of solid (silica), gas (air), and liquid
(water and/or oil) phases. The solid phase is composed of discrete particles (sand or silt
grains or clay platelets), and the interactions between solid particles affect the
deformation behavior of the soil mass. The geometric arrangement of the three phases
can significantly affect the total porosity, pore size distribution, fluid transport, and
reservoir/storage capacity of target liquids and gases. The distribution of the liquid phase
in partially saturated geo-materials also strongly affects its shear strength and
permeability/hydraulic conductivity. Understanding fluid transport properties in
geological samples is of increasing importance in recent years for applications such as
carbon sequestration, understanding Fracking effects on ground water, transport of
contaminants through ground water, and for optimizing the hydraulic fracturing schemes
for oil recovery.

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X-ray micro computed tomography techniques have previously been explored for
imaging geo-materials [1, 2]. However, the low attenuation of water relative to the rocks
silica phase typically produces low contrast in which water and air are difficult to
distinguish using conventional X-ray imaging. It is necessary to add a contrast agent to
the water in order to distinguish water phase more precisely [3]. However, the addition of
contrast agent will affect the contact behavior of the liquid and solid phases, thus
affecting the measured transport properties not representative of in situ conditions.
Recently, the first two authors of this paper have performed a dual modality (neutron and
X-ray) imaging to overcome the limitation of visualizing low contrast phase of water in
compacted silica sand specimen using X-rays [4]. The microstructures of geo-materials
obtained from X-ray tomography have also been used to perform fluid flow simulation [5,
6]. X-ray tomography can provide actual microstructure of the pore geometry, and pore
scale simulation can thus be performed using such data sets.

In this paper, we demonstrate the results of using a novel laboratory X-ray microscopy
platform, which uses a unique high dynamic range detector system, capable of imaging
unstained water, air, silica sand in a custom specimen holder specifically designed to
compact the granular material at target bulk density to mimic natural system. Very
detailed quantitative information on the three phases was obtained from X-ray
tomography in three dimensions. Direct numerical simulations (DNS) using actual
microstructure obtained from reconstructed tomography data was used to generate
capillary pressure saturation curves. High resolution three-phase tomography imaging
data can be used to predict fluid flow properties of partially saturated system. This
approach shows tremendous potential to offer new insight on developing next generation
predictive property based geo-materials and advanced material characterization tools for
applications such as carbon sequestration, and understanding the deformation behavior of
granular materials, heat transfer through porous systems, and related fluid flow behavior.

PROCEDURE
Specimen Description
A compacted dry Ottawa sand (20/40 Oil Frac, 99.98% silica phase) and a partially
saturated specimens were prepared under controlled conditions using a custom designed
mold suitable for tomography and known compaction effort. The compaction mold had
inner dimension of approximately 10.21 mm dia. 10.21 mm height as shown in Figure
1(a). Dry or partially saturated sand (12% gravimetric water content) are compacted in
the mold using three compaction layers. The dry or wet sand (mixed to 12% water
content) was placed in the compaction mold to about 1/3 height and compacted by
dropping a tamping rod 25 times. The process is repeated for the next two layers. The
average grains size of the sand grain is approximately 700 m.

X-ray Tomography
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Xradia microXCT-400 high resolution X-ray microscope system was used to image the
specimens. The system consists of a microfocus X-ray source (150kV), multiple imaging
optics to switch between different resolution modes and a CCD camera (2048 2048).
Variable sizes of lens can be selected to change the size of field of view (FOV) and
spatial resolution. The system can image specimen size from 100 mm to 50 m and
spatial resolution from 50 m to 500 nm. In this research, the 1X and 10X magnification
lens were used to change the size of FOV. For the wet sand specimen, 10X magnification
imaging was performed at top, middle and bottom of the specimen corresponding to top,
middle and bottom compaction layers as shown in Figure1b. For the dry sand specimen,
only the top area was selected form 10X magnification imaging. Imaging parameters are
shown in Table 1. A good contrast of silica, air and water phase is obtained in partially
saturated sand specimen. Due to a stable microfocus X-ray source and novel imaging
optics, high resolution and high contrast imaging was achieved. The data was
reconstructed with filtered backprojection algorithm. The reconstructed slices were first
smoothened by median 3D filter, and then non-local mean filter was applied. The data
was thresholded for phase quantification. The image processing was performed with
Avizo (version 7.0).

RESULTS
Multi-resolution Imaging of Identical Specimen
Example tomography slices of partially saturated sand specimen are shown in Figure 1c
and 1d for 1X and 10X magnification respectively. Approximately the same region inside
of the red circle shown in Figure 1c is magnified in Figure 1d with much higher
resolution. The water (dark gray), sand (light gray) and air (black) phases are shown very
clearly with a good contrast without the use of a contrast agent. Three dimensional
images of dry and wet specimen at 10X magnification are shown in Figure 2. The
porosity and saturation values of the 1X magnification data obtained from image analysis
are shown in Table 2. The 1X magnification image resolution (22 m/voxel) was high
enough to quantify sand grain phase with much higher size (~700 m) relatively well, but
it was not high enough to quantify the water phase below the resolution limit accurately.
Some error is expected with the saturation value of the wet sand due to partial volume
effects.

Direct Numerical Simulation
Full morphology model [7, 8] is used to simulate the quasi-static drainage simulation of
liquid in the porous media. The stationary distribution of wetting phase (WP) and non-
wetting phase (NWP) for an arbitrary capillary pressure (p
c
) can be determined. The
simulations presented here run the full morphology method as implemented in the
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GeoDict code (www.geodict.com). Pore size is the main factor determining the drainage
at a given capillary pressure. Morphological opening is used to determine the pore size
distribution as shown in Eq. (1) where X represents the pore space and B is the structuring
element. O
B
represents the morphologically opened pores space, and it also means the
pore space where the structuring element fits in.
} { ) ( X B B X O
B
(1)
A spherical structuring element with radius r is used, and a spherical interface is assumed
between WP and NWP. It is assumed that one end of the dataset is connected to the WP
reservoir and the other end is connected to the NWP reservoir. The pore space is assumed
to be fully saturated with the WP, and the capillary pressure is zero. The pore space is
eroded by spheres with r starting from the smallest radius. Based on the radius r, the
capillary pressure is computed based on Young Laplace equation as shown in Eq. (2)
where is the contact angle between WP and solid, and is the surface tension between
NWP and WP.

r
p
c
cos 2
(2)
The pore space is filled with NWP if the erosion of the pore space has a continuous
connection to the NWP reservoir. The leftover eroded set is dilated to complete the
opening process. The volume fractions of NWP and WP are determined for the given
capillary pressure. The process is repeated for the next structuring element with larger
radius r.

An example capillary pressure saturation curve for drainage is generated based on the
microstructure of partially saturated sand (1X magnification) by using the full
morphology method as shown in Figure 3. Fully wetting condition was assumed, and
contact angle of water on silica was chosen as 0. The surface tension of water was
assumed to be 72.75 mN/m. Example simulated two phase distributions obtained from
the full morphology simulation are shown in a, b, c of Figure 3 and compared to the
actual experimental result shown in Figure 3d. Based on the simulated capillary pressure
saturation curve, the capillary pressure of the given partially saturated sand specimen is
estimated as 1.35 kPa.

CONCLUSION
Multi-resolution and high contrast X-ray tomography imaging of dry and partially
saturated geomaterial were presented. High contrast of water phase was obtained without
using a contrast agent. Multi-resolution capability provides option to zoom into more
details at the region of interest without moving the specimen or experimental equipment.
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Direct numerical simulation was applied on the actual microstructure obtained from X-
ray tomography, and a capillary pressure saturation curve was obtained. Predictive
measurement of capillary pressure of the partially saturated sand specimen was obtained
based on the simulated capillary pressure saturation curve.

ACKNOWLEDGEMENTS
The authors would like to thank Dr. Volker Schulz at Baden-Wuerttemberg Cooperative
State University Mannheim, Germany and Dr. Andreas Wiegmann at Fraunhofer ITWM,
Kaiserlautern, Germany for the continued collaboration with DNS research and support
related to the GeoDict software license for collaborative research.

REFERENCES
1. Wellington, S. L. and H. J. Vinegar, "X-Ray Computerized Tomography," Journal of
Petroleum Technology, (1987) 39, 8, 885-898
2. Sallier, B. and G. Hamon, Micritic limestones of the middle east: influence of wettability,
pore network and experimental technique on drainage capillary pressure curve, 2005
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Liquid Morphology in Natural Porous Media Using Synchrotron X-ray
Microtomography," Environmental Science & Technology, (2005) 39, 21, 8403-8410
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neutron and X-ray imaging of granular materials, Under Review," Journal of
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(2001) 28, 17, 3361-3364
7. Hilpert, M. and C. T. Miller, "Pore-morphology-based simulation of drainage in totally
wetting porous media," Advances in Water Resources, (2001) 24, 3-4, 243-255
8. Schulz, V. P., J. Becker, A. Wiegmann, P. P. Mukherjee and C.-Y. Wang, "Modeling of
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Table 1: High resolution X-ray imaging parameters

Magnification Voltage
(kV)
Current
(W)
FOV
(mm)
Voxel size
(m)
Number of
projection
Exposure
Time (s)
1X 70 10 14 22 1500 10
10X 80 10 2.05 2.04 3000 15

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Table 2: Porosity and saturation values obtained from image analysis of 1X magnification data

Dry 1X Wet 1X
Porosity (%) 36.1 32.9
Saturation (%) 0 39.0


Figure 1: Picture of the partially saturated sand specimen (a), radiography of partially saturated sand
specimen showing 1X and 10X magnification FOV size and location (b), tomography slice of partially
saturated sand specimen at 1X magnification (c), and tomography slice of partially saturated sand specimen
at 10X magnification (d)

Figure 2: Three dimensional visualization (1mm
3
) of dry (a) and partially saturated (b) sand specimen at
10X magnification

Figure 3: Simulated capillary pressure saturation curve of drainage and example two phase distributions
from simulation (a, b, c) and experiment (d)