Artigo - Cnudde (2011) - 3D Characterization of Sandstone by Means of X-Ray Computed Tomography
Artigo - Cnudde (2011) - 3D Characterization of Sandstone by Means of X-Ray Computed Tomography
Geosphere
Geosphere 2011;7;54-61
doi: 10.1130/GES00563.1
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Notes
ABSTRACT (Russ, 2002). In order to overcome this problem, Although statistical and process-based models
several orthogonal sections or serial sectioning have their advantages, X-ray microtomography
Due to technological development, state- coupled with digital image analysis to construct (micro-CT) can also be applied in the study of
of-the-art high-resolution X-ray computed a three-dimensional image of the microstructure internal structures of geomaterials. Micro-CT
tomography (CT) systems can be developed, can be necessary to reveal 3D mineral structures has improved enormously in recent years thanks
enabling the internal visualization of geo- (Lin and Cohen, 1982; Holt et al., 1996). to rapid technological developments and is more
materials in three dimensions. However, in Many research topics in geology concern widely available now, with a constantly improv-
order to obtain structural information one the study of internal structures of geomaterials ing resolution and image quality. This technique
also needs proper three-dimensional (3D) on a pore-scale level in order to estimate enables rapid, nondestructive, 2D and 3D exam-
analysis software. In this paper, the potential their macroscopic behavior (Bakke and Øren, ination and analysis of almost any kind of mate-
for petrographic purposes of high-resolution 1997). In order to compute properties such as rial, including rock and soil (Carlson, 2006).
X-ray CT in combination with the 3D analy- permeability and electrical conductivity, there Tomography-based methods rebuild the inter-
sis software Morpho+ is explored for a Bel- is a need for an adequate description of the nal structural information within an object by
gian sandstone sample. The advantage of the complex internal microstructure. Bakke and mathematically reconstructing it from a series
CT technique is the fact that it is an ideal tool Øren (1997) developed a process-based recon- of projections (Russ, 2002). All transmission
to characterize the internal structure of a struction procedure that incorporates grain- tomography devices are based on the same prin-
rock in three dimensions in a nondestructive size distribution and other petrographic data ciple: the object is positioned between a source
way while a limitation of this CT technique obtained from 2D thin sections to reconstruct and a detector and rotated while transmission
is that only small samples can be combined 3D sandstones. The essence of this approach images are recorded. Different kinds of probes
with a high spatial resolution and therefore was to build sandstone models that were ana- can be used for the visualization: X-rays, neu-
often many samples will need to be scanned logs of actual sandstones by stochastically trons, gamma rays, etc.
in order to obtain representative volumes. modeling the results of the main sandstone In this paper X-ray computed tomography
The relationship between sample size and forming processes: sedimentation, compac- (CT) is used. A set of 2D radiographs of the
obtained spatial resolution are discussed as tion, and diagenesis. While statistical models sample are collected at a sequence of transmis-
well as the influence on the spatial resolution based on correlation-function reconstruction sion angles, providing information on X-ray
exerted by some important technical aspects retain a similar degree of isotropy and homo- attenuation, which depends on the density and
like the used X-ray source and detector. This geneity as the experimental microstructure, atomic number of the components. By means
paper focuses in detail on the structures that they tend to significantly underestimate the of reconstruction software the radiographs are
can be determined by means of micro- and connectivity properties. Although the recon- converted into a stack of 2D cross sections that
high-resolution X-ray CT in combination struction method proposed by Bakke and Øren allow 3D renderings of the sample. Although in
with 3D algorithms. was promising, it was unclear how accurately the beginning X-ray computed tomography was
it can reproduce more heterogeneous and dia- mainly used in medicine, it soon became clear
INTRODUCTION genetically complex sandstones such as those that X-ray CT had a large potential for other
encountered in nature. Øren and Bakke (2002) applications, including palaeontology (Fourie,
Conventional microstructure analysis of rock stated that although X-ray microtomography 1974; Conroy and Vannier, 1984; Haubitz et al.,
samples is usually carried out by studying two- was extremely useful, it was still not readily 1988; Chapman et al., 2003; Hlusko et al.,
dimensional (2D) polished thin sections with available in practice and therefore information 2004), sedimentology (Kenter, 1989; Peyton
optical microscopy or scanning electron micros- about the pore structure of porous materials et al., 1992; Zeng et al., 1996; Boespflug et al.,
copy (SEM). When looking at 2D images, it is was often limited to 2D thin-section images. 1995), petrology (Van Geet et al., 2001), soil
necessary to keep in mind that the shape of min- Consequently, the attractive approach was to science (Allan et al., 2002), and fluid-flow
erals and their spatial relationships can be much reconstruct a 3D description of the pore struc- research (Wellington and Vinegar, 1987; Géraud
more complex in three dimensions. Although ture from readily available 2D images, by et al., 2003; Dunsmuir et al., 1991; Coles et al.,
there are powerful quantitative tools to interpret means of statistical models for reconstructing 1994; Spanne et al., 1994; Hazlett, 1995; Coles
data derived from 2D images for the character- 3D porous media from 2D thin-section images et al., 1996; Coker et al., 1996).
ization of three-dimensional (3D) structures, (Joshi, 1974; Adler et al., 1990; Adler et al., Industrial X-ray CT scanners proved to be
many quantitative and qualitative aspects of 1992; Adler, 1992; Hazlett, 1997; Yeong and successful for research on geomaterials but with
structures remain inaccessible from 2D images Torquato, 1998a, 1998b). a resolution of a few hundreds of μm only. To
3D characterization of sandstone
obtain (sub)micron-scale resolution, currently if the entire sample width is not imaged. Since in a heterogeneous material can be determined
two options exist: synchrotron sources and X-ray detectors have a limited number of pixels, either by a few measurements on large volumes,
laboratory high-resolution X-ray CT (HRXCT) image resolution is limited to the discretization or by measurements of many small volumes of
scanners. Synchrotron sources allow submicron of the sample width, the latter forming the main material. They conclude that the representative
resolution with a monochromatic beam of well- practical limit for computed tomography. volume element must be considered as a func-
defined energy, but prove to be inaccessible for As mentioned earlier, a small sample size tion of several parameters including the physical
daily use for most research groups. More acces- is crucial for a high spatial resolution. How- property, the contrast of properties, the volume
sible laboratory equipment includes medical ever, working with small rock samples raises fractions of components, the desired relative
and micro-CT scanners (resolutions varying the question of the representative volume. In precision for the estimation of the effective
from roughly 100 to 1 μm, respectively) using order to obtain an acceptable estimation of the property, and the number of samples associated
X-ray tubes instead of synchrotron sources. general rock properties, the samples to be ana- with computations that one is ready to carry
HRXCT systems are currently being developed lyzed should be representative of the rock body out. The primary question, however, remains:
with submicron resolution. The CT scanners itself, including its normal spatial variations. what characteristic or property does one want
with micron or submicron resolution provide an Theoretically, a sample is only representative to see in 3D by means of X-ray? Is it to deter-
alternative to synchrotron-based research. One when its analysis results are both accurate and mine overall parameters like total porosity to be
of the advantages of CT systems is that they can reproducible (Gy, 1994). Sampling accuracy used as the overall porosity value for the stone
nondestructively provide stacks of more than is achieved when a few qualitative rules are in general? Or does one want to look in detail
1000 2D cross sections of the sample under respected. Correct sampling will provide all con- at a certain volume of interest in order to solve
investigation much faster than by performing stitutive elements to be evaluated with an equal some remaining questions? In this paper we
serial sectioning. Since no system is perfect, it probability of being selected and of belonging will focus on the detail that can be detected
is important to understand the advantages and to the sample (Gy, 1994). Three major factors with high-resolution X-ray CT rather than on
limitations of this technique in order to properly influence the accuracy of sampling: the sample the porosity values or the grain-size distribution
use it to address particular geological questions. grain size, the sample volume, and the amount results as the overall properties. As an example,
An important issue when working with CT is of samples taken (Smith, 1999). All these fac- we present an analysis conducted on the Bray
the relationship between sample size and spa- tors are in relation with each other. If a rock sandstone. The Bray sandstone has already
tial resolution. In HRXCT, the best achievable type has a high internal heterogeneity, a larger been characterized in different ways (Cnudde
resolution is related to the spot size of the X-ray amount of samples should be taken. Many stud- and Jacobs, 2004; Cnudde, 2005; Cnudde et al.,
source and the magnification of the system. ies were performed on sampling by Gy (1967, 2008), so the results of these experiments can be
The magnification is limited by the diameter 1971, 1979), Goodsall and Mathews (1970), and compared with the results of the high-resolution
of the sample under investigation. The resolv- Sedman and Stanley (1990). General rules like scan presented here.
ing power of an imaging system is the smallest the one formulated by Gy (1979) predict that Several parameters play a role in the classifi-
distance between two features (point, lines) at a good estimate of the required sample size is cation of different minerals in 3D derived from
which these features can be distinguished from obtained if X-ray CT scanning: the contrast in X-ray attenua-
one another. tion between those minerals, which is dependent
The resolving power that can be achieved Ms ≥ K· d 3, (3) on the density and average atomic number of
within the image is these minerals, and the size of the minerals in
where Ms is the sample weight and d is the diam- relation to the spatial resolution. Comprehen-
d ⎛ 1⎞ eter of the largest particle (Gy, 1979). Depend- sion of the image acquisition technique based on
R= + 1 − ⎟ s, (1)
M ⎜⎝ M⎠ ing on the degree of variation in grain size, the X-ray transmission and of the methods used for
parameter K is given a certain value (Gy, 1979). extraction of 3D data from a data set is crucial
with R the achievable resolution (Equation 1) in In case of a high degree of variation in grain if one is to obtain reliable quantitative measures
the object, s the spot size of the X-ray source, d size, the sample size might have to be doubled of features of interest. 3D image analysis starts
the pixel size of the detector, and M the magni- compared to samples with a low degree of varia- with high-quality images, since this is essential
fication, which is related to the position of the tion. However, in the case of sampling rocks to to retrieve valuable and useful information from
object and the separation between the source be used as building stone, the size of the blocks the original images. The use of image analysis
and detector: produced has to be taken into account as well generally involves the implementation of com-
as an estimation of the variation between the plex image processing (Starkey and Samantaray,
M = (total source-detector distance)/ blocks themselves. Jefferson (1993) suggests 1994) and of advanced calculation algorithms
(2)
(total source-object distance). that, as the properties of a block of stone such as (Pirard, 1994). Classical image analysis consists
its durability are determined by the properties of of noise reduction, segmentation, and binary
For low magnifications, the detector pixel size its constituent parts, the size of these constituent image editing. But before performing image
is the limiting factor for the image resolution parts can be used as a guide to determining the analysis, the original images often need to be
(Equation 1). For high magnifications, the X-ray sample size. Another approach, suggested by processed. This image processing is primarily
source spot size becomes significant, resulting Kanit et al. (2003) states that the representative performed to improve the visual appearance of
in a fuzzy image. The spot size thus limits the volume element size can be associated with a the images and to prepare for measurements of
resolution of the whole setup. Furthermore, to given precision of the estimation of the wanted features and structures present. A wide range
achieve high magnification the targeted part of overall property and the number of realizations of different techniques exists for each of these
the sample must be positioned very close to of a given volume of microstructure one is able tasks. Several software packages are available
the X-ray source, which is impossible for large to consider. For example, Kanit et al. (2003) for analysis of 2D images. Software for 3D
samples. Moreover, images can contain artifacts argue that the overall volume fraction of a phase analysis, however, is less frequently available or
Cnudde et al.
sometimes not well adapted to specific needs. the roundness in thin sections, the relation of the at 300 ms exposure time in order to obtain a
Therefore the new 3D software Morpho+ various particle diameters (length, width, and high signal-to-noise ratio. The total scan time
(Vlassenbroeck et al., 2007) was developed in thickness) is calculated; specifically the degree was ~90 min. A source-to-detector distance
order to overcome the existing limitations to to which the shape of a grain approaches that of of 890 mm and a source-to-object distance of
analyze (pore) structures inside reconstructed a sphere (Bates and Jackson, 1980) is of inter- 51.8 mm resulted in a magnification of 17.2,
micro-CT images. est. In general, there is no real preferred orienta- equivalent to a voxel pitch of 7.4 μm (detector
In this paper, the potential of high-resolution tion of the grains; they are also closely packed pixel pitch of 127 μm). For the small sample,
X-ray CT in combination with the Morpho+ 3D (Fig. 1). The average open porosity of the Bray the spot size was set to its minimal size of below
analysis software for petrographic purposes is sandstone determined with water absorption 1 μm, limiting the available target current to
explored on a Belgian Bray sandstone sample. under vacuum is 14%, with a minimum of 9 μA, or ~1 W target power. A voxel pitch of
The advantages and limitations of these tech- 4% and a maximum of 24% (Cnudde, 2005; 700 nm was achieved by a source-to-detector
niques are discussed. The data obtained with Cnudde et al., 2008). The average pore diameter distance of 890 mm and a source-to-object dis-
X-ray CT is compared with results from the determined with mercury intrusion porosimetry tance of 4.9 mm, equivalent to a magnification
more conventional techniques of optical micros- (MIP) ranges from 4.7 to 20.1 μm, with an aver- of 181.6. Due to the low X-ray flux, no beam-
copy and scanning electron microscopy. age of 15.7 μm. The average threshold pressure hardening filter was applied. Four frames at an
derived from MIP was between 11 μm and exposure time of 1000 ms were averaged for each
MATERIALS 16 μm depending on the degree of cementation. of the 1500 projections, extending the total scan
The density of the Bray sandstone is on average time to nearly 3 h. The Varian PaxScan 2520V
The Bray Sandstone 2281 kg/m3 (Cnudde, 2005). (a-Si flat panel, CsI screen, 1880 horizontal by
Two different samples of the Bray sandstone 1496 vertical pixels, 127 μm pixel size) recorded
The Bray sandstone is a quartz arenite from were analyzed for this study. A large rectangular images for both samples, although its orienta-
the Thanetian (Paleocene, Paleogene). This sample with a cross section of 6.6 × 7.4 mm2 tion was changed for the different purposes. This
natural building stone has mainly been used for was scanned. Because of the size of the sample, resulted in an image width of 1496 pixels for the
monuments in Binche, Mons, and Bray (Bel- only part of the sample height could be imaged low resolution scan, and 1880 pixels to achieve
gium) and in houses (Cnudde, 2005). The Bray in order to obtain the desired resolution. The maximum resolution for the small sample. Both
sandstone is a heterogeneous accumulation of second sample is a drilling core with only 1 mm samples were reconstructed using the soft-
mostly continental deposits consisting of quartz diameter and a height of ~500 μm. Its small size ware package Octopus (http://www.inct.be).
grains with a siliceous cement. Its color varies allowed scanning at very high resolution. The software Morpho+ (Vlassenbroeck et al.,
from gray to yellowish brown, depending on the 2007) was used for the 3D analysis of the
amount of iron oxide and/or hydroxides, which METHODS pores and the grains of the Bray sandstone. In
occur as a very thin coating around the grains. 3D analysis, a volume composed of voxels is
In addition to monocrystalline quartz grains and High-Resolution X-ray CT (HRXCT) processed to extract quantitative data about the
sometimes polycrystalline quartz, feldspars, Combined with 3D Analysis by Morpho+ structural composition of the sample. The vol-
rutile, zircon, some mica, and clays can be iden- ume can be represented as a stack of images,
tified in thin sections. Some quartz grains show A flexible multifunctional high-resolution although the operations need to be performed
a typical overgrowth; in many cases the shape X-ray CT (HRXCT) scanner allowing 2D in 3D. The objective of the analysis is to obtain
of the original grain is delineated by a thin iron radiography and 3D visualization and quanti- parameters such as size, shape, and orientation
oxide and/or hydroxides or clay coating between fication on a (sub)micron scale was used. The for each object (for example, a pore or a grain)
the overgrowth and the grain itself. The presence scanner was developed at the “Centre for X-ray inside the sample. In Morpho+, the analysis
of the clay minerals in the sandstone can be very Tomography” of the Ghent University, Belgium
significant as it strongly affects rock permeabil- (Masschaele et al., 2007). The transmission tube
ity and porosity. The Bray sandstone is a fine- head was operated at a high voltage of 100 kV
grained, poorly sorted sandstone (Cnudde et al., for both samples. The large sample was scanned
2004). Grains are angular to subrounded, with at a target current of 80 μA, resulting in 8 W
an average grain size of 0.156 mm and low in target power. In this configuration, the X-ray
sphericity (Cnudde and Jacobs, 2004). Accord- spot size is ~5 μm in diameter. A 550-μm-thick
ing to the formulas of Folk and Ward (1957) aluminum plate was used as a beam-hardening
(Table 1), the grains could be defined as poorly filter. In total 1000 projections were recorded,
sorted and positively fine-skewed. To determine each projection being an average of three frames
3D characterization of sandstone
process is composed of several steps, includ- als present in the Bray sandstone, zircon has the equal to 7.4 μm are not included in this volume
ing filtering, phase segmentation or threshold- highest attenuation coefficient, while quartz has analysis since they are below the resolution.
ing, labeling, and object separation. By using an the lowest (Cnudde, 2005; Gualda and Rivers, In addition to determining porosity and over-
algorithm-based dual threshold, the original data 2006). The quartz grains can be clearly detected, all pore shapes and spatial relationships, each
was transformed into a binary data set with the as well as some dense inclusions of rutile and individual grain can be analyzed as well. There-
aim to extract structural features of the selected zircon, based on a microscopic examination fore grains are first segmented and automati-
pore volume. Dual thresholding uses two inter- of the samples prior to CT scanning. Besides cally identified by a watershed separation algo-
vals; voxels with a gray value in the first interval cross sections, 3D renderings (Fig. 4) can be rithm based on the Euclidean distance transform
are classified as foreground voxels, while voxels produced for visual interpretation of the mineral (Russ, 2002). Based on analysis of the grain
in the second interval are only defined as fore- shape and their spatial relationships. However, size in the 343 mm3 volume sample, an aver-
ground voxels if they are connected to voxels for quantitative results a 3D analysis is required. age equivalent diameter for the Bray sandstone
from the first interval. This approach reduces the Analyzing the pore-volume of the scanned sam- grains of 194 (±53) μm was found together with
sensitivity to residual image noise. One of the ple with Morpho+ revealed an average porosity an average maximum opening of 117 (±34) μm.
analyzed parameters, which is necessary for our of 18 vol% over an analyzed partial volume of In this volume, a total of 53,103 grains were
shape analysis, is the maximum opening, which 343 mm3. However, all pores smaller than or analyzed.
can be extracted from the distance transform.
The maximum opening is defined as the diam-
eter of the maximum inscribed sphere which fits
inside the object (Fig. 2). For each grain its total
volume can be determined as well as its surface. Figure 2. Two-dimensional
If a sphere with the same total volume of a grain (2D) illustration of the maxi-
is constructed, its corresponding diameter is mum opening of an object.
defined as the equivalent diameter of the grain.
Morpho+ calculates the sphericity S as the ratio
of the maximum opening over the equivalent
diameter. This parameter gives a rough approxi-
mation of the object shape since it expresses
how much an object resembles a sphere (S = 1).
S ≈ 0 typically corresponds to a large network
composed of narrow channels.
Additionally, each object can be modeled
as an equivalent ellipsoid which has the same
moments of inertia. The three-dimensional
moments of the inertia tensor are then calcu-
Figure 3. Reconstructed cross
lated and diagonalized. The corresponding rota-
section of the Bray sandstone
tion of the eigenvectors defines the orientation
scanned with a resolution of
of the object, while the eigenvalues correspond
7.4 μm.
to the lengths of the principal axes of the equiva-
lent ellipsoid. Since Morpho+ can determine the
orientation of the objects of interest such as the
grains constituting the sandstone, it is possible
to produce a stereoplot derived from the 3D
analysis of the grains. The processed volume
1000 μm
can be visualized after each step in the analysis
process. Since all analysis algorithms operate in
three dimensions, cross sections of the volume
according to the different principal planes can
be visualized.
RESULTS
Cnudde et al.
Figure 5 shows details of the 3D renderings the intergranular structure, and to identify The grain contact varies from point (grains
of the results of Morpho+, where the grains in details inside the grains (Fig. 7). Monocrystal- touch each other) to sutured contacts (mutual
the selected volume have been relabeled (color line quartz grains can easily be detected on the interpenetration of grains).
coded) based on a selected parameter, such as, reconstructed cross sections as well as mineral Volume rendering of the 2D reconstructions
e.g., their equivalent diameter. From the grain inclusions like rutile and zircon, and voids. One reveals the internal structure of the stone with
analysis performed on the micro-CT scan, the has to be very careful when identifying minerals high 3D detail (Fig. 8). Besides looking at the
largest equivalent diameter found was 375 μm on X-ray CT reconstructed images since X-ray structures themselves, it is also possible to virtu-
and the largest maximum opening 231 μm. The attenuation coefficients are a function of both ally cut the sample at any desired location and/or
average sphericity of the analyzed grains based atomic number and material density. However, angle and to make certain components transpar-
on the micro-CT scan was 0.6. This value indi- based on experience with the material most ent while rendering other features opaque.
cates that on average the grains are not perfectly probably clays and local thin iron oxide coat- When investigating the images of the high-
spherical. Figure 6 illustrates the frequency dis- ings can be detected in the reconstructions. resolution scan with Morpho+, a total volume
tribution of the grain sphericity. The frequency Since feldspars and quartz have a more similar of 0.57 mm3 was analyzed, corresponding to a
distribution shows a well-sorted curve, which attenuation coefficient, they are more difficult mass of 0.013 g. Although much more detail
corresponds with the estimation made on the to distinguish from one another. A small varia- can be detected in this high-resolution CT scan,
basis of the 2D reconstructed images. tion in attenuation coefficient toward the edge many similar samples should be examined in
of the sample can be seen on Figure 7, caused order to obtain a representative element vol-
High-Resolution CT Scan by phase-contrast. However, this feature is not ume. As the subsample volume is so small, only
(Resolution 0.7 μm) problematic for the segmentation purpose since a small amount of grains, a total of 710, could
by using dual thresholding the correct features be analyzed on their equivalent diameter, maxi-
In order to achieve a resolution on the order can still be segmented. mum opening, and sphericity. Figure 9 shows a
of 700 nm, a subsample of the Bray sandstone Based on the reconstructed 2D cross sections, 3D rendering of the results of Morpho+, where
was selected. This resolution enables one to the grains of the Bray sandstone were character- each grain has been relabeled (color coded)
clearly distinguish the different grains, to assess ized as subangular over subrounded to rounded. based on its equivalent diameter. The average
grain sphericity calculated based on the high-
resolution scan was 0.57. This value indicates
that on average the grains are not perfectly
spherical, although some grains definitely are
(sphericity value = 1).
Frequency of sphericity
25,000
20,000
Frequency
15,000
Figure 6. Sphericity distribution
of the analyzed grains obtained 10,000
by the micro-CT scan.
5000 200 μm
3D characterization of sandstone
Figure 8. Three-dimensional
(3D) rendered volume of the
Bray sandstone sample scanned
with a resolution of 700 nm.
The dense inclusions are visual-
ized in red.
Cnudde et al.
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ACKNOWLEDGMENTS science.226.4673.456.
High-resolution CT scans provide more Dunsmuir, J.H., Ferguson, S.R., D’Amico, K.L., and Stokes,
structural detail due to their higher resolution. The Fund for Scientific Research—Flanders J.P., 1991, X-ray microtomography: A new tool for
(FWO) is acknowledged for the post-doctoral grant to the characterization of porous media: Proceedings
However, since the volume examined is smaller V. Cnudde. The Institute for the Promotion of Innova- 1991 SPE Annual Technical Conference and Exhibi-
than for micro-CT scans, the amount of analyzed tion by Science and Technology in Flanders, Belgium, tion, Dallas, Oct. 6–9: Society of Petroleum Enginers,
grains is much smaller, introducing insufficient is acknowledged for the Ph.D. grant to J. Dewanckele. paper SPE 22860.
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