Multi-scale characteristics of coal structure by x-ray computed tomography (x-ray

CT), scanning electron microscope (SEM) and mercury intrusion porosimetry (MIP)
Ting-ting Cai, Zeng-chao Feng, and Dong Zhou

Citation: AIP Advances 8, 025324 (2018); doi: 10.1063/1.5021699

View online: https://doi.org/10.1063/1.5021699
View Table of Contents: http://aip.scitation.org/toc/adv/8/2
Published by the American Institute of Physics
 AIP ADVANCES 8, 025324 (2018)

Multi-scale characteristics of coal structure by x-ray

computed tomography (x-ray CT), scanning electron
microscope (SEM) and mercury intrusion
porosimetry (MIP)
Ting-ting Cai, Zeng-chao Feng,a and Dong Zhou
Key Laboratory of In-situ Property Improving Mining of Ministry of Education,
Taiyuan University of Technology, Taiyuan, Shanxi 030024, P. R. China
(Received 7 January 2018; accepted 19 February 2018; published online 28 February 2018)

It is of great benefit to study the material and structural heterogeneity of coal for bet-
ter understanding the coalbed methane (CBM) storage and enrichment. In this paper,
multi-scale X-ray computed tomography (CT), scanning electron microscope (SEM)
and mercury intrusion porosimetry (MIP) at multi scales were conducted to thoroughly
study the material distribution, heterogeneity, pore development, porosity and perme-
ability of coal. It is suitable and reasonable to divide the testing samples into three
structural categories by average density and heterogeneity degree, and the meso struc-
ture in the three categories accords with the morphology on SEM images. The pore
size distribution and pore development of each subsample cannot be correspondingly
related to their respective structure category or morphology due to different observa-
tion scales, while the macro pore size development, accumulated macro pore volume
and macro pores porosity accord with the meso structure category and morphology
information by CT and SEM at the same scale very well. Given the effect of macro
pores on permeability and the contribution of micro pores to CBM storage capacity,
reservoirs with developed micro pores and macro pores may be the most suitable coal
reservoir for CBM exploitation. © 2018 Author(s). All article content, except where
otherwise noted, is licensed under a Creative Commons Attribution (CC BY) license
(http://creativecommons.org/licenses/by/4.0/). https://doi.org/10.1063/1.5021699

I. INTRODUCTION
In recent years, coalbed methane (CBM) has become a potential alternative energy to fossil fuels
for its clean property, high calorific value and large storage in the field of energy exploitation. Coal is
a natural reservoir with great gas adsorption capacity. As a complex porous media, coal commonly
contains matrix, clay minerals, numerous pores and small fractures, showing evident material and
structural heterogeneity at meso and micro scale.1 The heterogeneity of pores and fractures ranging
from nm to mm scale has significant impact on the CBM storage and mass transport.2 Previous studies
on coal structure mainly concentrate on characteristics of pore structure, such as pore volume (PV),
pore specific surface area (PSSA), pore size distribution (PSD), fractal dimension and so on,3–7 few
of the studies have attempted to characterize the entire coal structure with coal matrix, clay minerals
and pore distribution all taken into consideration. As pores have larger gas storage capacity than coal
matrix and clay minerals,8,9 so the maceral compositions and the non-homogeneously distributed
pores both affect the inhomogeneous methane adsorption and result in regional CBM enrichment.
Early in 1990, Yu10 proposed inhomogeneous methane enrichment in coal mines, he pointed out
gas bags that coal pits with considerably higher gas pressure and gas content than their adjacent
areas existed in coal seams. Recently, by updating methods, Feng11,12 and Zhou13,14 have revealed
the inhomogeneous adsorption and deformation characteristics in coal at the experimental scale, and
they attributed the different adsorption and deformation responding to structure differences. Similarly,

a
Corresponding author Email: zc fengg@126.com

2158-3226/2018/8(2)/025324/12 8, 025324-1 © Author(s) 2018

025324-2 Cai, Feng, and Zhou AIP Advances 8, 025324 (2018)

in engineering practice, CBM production and composition from individual stacked coal seams in
a multi-zone completed gas well vary greatly.15 One of the main reasons for these inhomogeneous
phenomena lies in the non-homogeneously distributed materials and porous structure, thus adsorption
and deformation responding differences were resulted, so it is necessary to take the material and
structural heterogeneity into consideration for better understanding and further studying the CBM
enrichment.
There are many observation methods for meso and micro structure of porous media emerging
and updating, such as scanning electron microscope (SEM), mercury intrusion porosimetry (MIP),
low temperature N2 /CO2 adsorption (LTNA/LTCA), 3-D X-ray computed tomography (CT) and so
on. As X-ray CT scanning is not affected by the material shape and can visually present the internal
structure information in a nondestructive manner, it has become a simple and feasible method for
qualitative and quantitative analysis for rock materials. The 2-D CT images can reflect the density
difference of the detected material, which makes it easy for coal matrix, minerals, pores and fractures
distinction. By using X-ray CT scanning, coal skeleton deformation and pores/fractures evolving in
rock materials under different testing conditions were extensively obtained.16–19 Besides, on the basis
of threshold segmentation and 3-D reconstructions, the qualitative visualization and pore structure
quantitative characterization can be performed, too.20,21 As for scanning electron microscopy (SEM),
it works in larger magnification and can accurately shows more detailed material composition and
structural characterization information, thus it is widely used in the morphology study of rock and
soil materials.22,23 The mercury intrusion porosimetry (MIP) is also extensively used to characterize
the pore characteristics of porous media, such as PV, PSD, and PSSA.24–27 It is worth noting that
although these methods have excellent observation on meso and micro structure, there are still some
differences in their application due to respective precision and scope. By X-ray CT, 3-D scanning can
be realized, and the density or structure change within samples can be determined. However, affected
by the magnification and material size, its resolution is about 10 um ∼1 mm. The SEM scanning is
more subtle, and its main scanning scale is about 0.01∼10 um.28 But only surface scanning can be
performed, the 3-D porous structure and material distribution in the entire sample cannot be obtained
unless FIB-SEM or other destructive microscopy is used.29 The MIP testing can measure pores larger
than 1 nm, and PV, PSD and PSSA can be calculated, but the detailed morphology information cannot
be obtained (Fig. 1).
Given the limitations of these observation methods and the complexity of coal’s material and
structure, it is quite impossible to simultaneously get porous structure, morphology information, PV
and PSD by one single observation method, so multi methods are needed cooperatively. In this paper,
X-ray CT, SEM and MIP were combined at multi scales to thoroughly study the meso structure,
heterogeneity degree, pore development of coals. By X-ray CT, the avenge density, material distribu-
tion, heterogeneity degree and porosity of coal samples were obtained, and by SEM, meso structure,
pore shape and material distribution were acquired, and by MIP testing, PV, PSD and porosity were
gained. Finally, the observation results by three methods were synthesized and compared to get thor-
ough material and structural information of coal samples. Besides, the result consistency at different
scales was further discussed.

FIG. 1. Multi scale observation methods.

025324-3 Cai, Feng, and Zhou AIP Advances 8, 025324 (2018)

II. EXPERIMENTS
A. Samples preparation
The coal samples are coking coal and lean coal, from the Xishan coal field and Qinshui coal
field respectively in North China. Standard core samples with size of ϕ50 × 100mm were machined
and numbered 1# and 2# respectively. Considering the sample size limitations in SEM scanning
and MIP testing, sizeable subsamples are needed to be extracted from standard core samples. The
detailed procedures are as follow (Fig. 2). The X-ray CT scanning was conducted to standard core
samples by High-precision µ CT225kVFCB micro CT experimental system. The scanning voltage
was 110 kV, and electric current was 130 µA. The magnification was 3.8, and the resolution was
49.3 µm. 1500 CT images were obtained (Fig. 2–a). CT Image Analysis Software, developed by our
team, was used to perform 3-D reconstruction. Several reconstructions with size of 150×150×150
pixels (7.4×7.4×7.4 mm) were established (Fig. 2–b). Homogeneous reconstructions with different
average attenuation coefficients were chosen. Lastly, according to the detailed CT layer and coordinate
positioning on 2-D images, these reconstructions can be located in standard core samples (Fig. 2–c),
and then the homogeneous subsamples were extracted, thus 7.4 mm cubic subsamples were acquired,
and numbered 1-1, 1-2, 1-3, 1-4, 1-5, 2-2, 2-3, 2-4 and 2-5. Subsequently, the second X-ray CT
scanning, SEM scanning and MIP testing were conducted with these subsamples.
B. The second X-ray CT scanning
High-precision µ CT225kVFCB micro CT experimental system was used for CT scanning. The
second scanning voltage was 90 kV, and the electric current was 120 µA. The magnification was
13.3, and the resolution was 14.7 um. Then 2-D CT images of all subsamples at the same scanning
condition were acquired.
C. SEM scanning
The Quanta 250 scanning electron microscope was used in SEM scanning. In this experiment, the
entire surface area of each subsample was scanned carefully at first, and then several representative
regions were chosen and magnified for detailed and thorough scanning. In order to present the meso
and micro structure of each subsample roundly, 10∼12 regions on the surface of each subsample were
chosen and magnified, and the maximum magnification was 3000.
D. MIP testing
Pore Master 33 mercury injection apparatus was used in MIP testing. The injection mercury
pressure ranged 1.5 kPa ∼231 MPa, and pores larger than 7 nm could be measured. In the process of
mercury injection, the larger mercury injection pressure, the smaller pores where mercury injected
in, so according to the relationship between mercury injection pressure and pore diameter, PV, PSD,
PSSA and porosity could be acquired.

FIG. 2. The testing samples procedure. (a) The 600th 2-D image of 1# coal sample by CT scanning; (b) 3-D digital
reconstruction; (c) locations of subsamples in 1# coal sample.
025324-4 Cai, Feng, and Zhou AIP Advances 8, 025324 (2018)

III. MESO STRUCTURE

A. Meso structure by X-ray CT
In X-ray CT scanning, X-ray goes through the detected material, and the ray intensity decreases
in an exponential law, that is,
I = I0 × exp(−µi,j d) (1)
I 0 and I are the ray intensity before and after the scanning respectively, µi,j is the linear attenuation
coefficient of arbitrary point in the material scanned, and d is the thickness of this point.
The 2-D CT image reflects the quantitative attenuation coefficient data, which are related to the
density of the material scanned, as follows:30
µi,j = µm × ρi,j (2)
Where µi,j is the attenuation coefficient of arbitrary point on 2-D CT image, µm is the mass attenuation
coefficient, and ρi,j is the density of this point.
According to Eq. (2), the attenuation coefficient array of any horizontal cross-section in the
sample can be obtained and converted to grey image, and then the real material and structural infor-
mation inside the sample can be read from these 2-D grey images, for example, in Fig. 2–a, the bright
white areas present large attenuation coefficients, and may be dense clay minerals, the majority of the
image is gray, and this part in coal is matrix. For the black lines, or holes with the smallest attenuation
coefficients, they are pores or fractures in coal.
Fig. 3–a shows the 400th CT image of 2-3# subsample. It can be seen that on this cross section,
coal is quite homogeneous, and there is no obvious dense clay minerals or evident pore/fractures.
The attenuation coefficients of all pixels on this image were summed and their proportions were
calculated (Fig. 3–b). As can be seen, the attenuation coefficients on this image were unimodally
distributed, and mainly concentrated in 0.021 ∼ 0.042, presenting obvious heterogeneity. Similarly,
it can be predicted that heterogeneity exists in entire coal subsample, too. So, 3-D reconstruction was
conducted to these subsamples according to the second X-ray scanning images, and corresponding
average attenuation coefficients were summed and calculated by the following equation,
n
X
µ= µi,j,z /n3 (3)
i=1,j=1,z=1

µ is the average attenuation coefficient of each subsample, µi,j,z is the attenuation coefficient of any
pixel inside the reconstruction and n is the pixel number along each direction.
As the attenuation coefficient is proportional to density, so the average attenuation coefficient
reflects the average density of each subsample, and the different attenuation coefficients in subsamples
means the different density essentially, so the attenuation coefficient variance can be used to embody

FIG. 3. The 400th 2-D CT image of 2-3# (a) and the attenuation coefficient distribution on this CT image (b).
025324-5 Cai, Feng, and Zhou AIP Advances 8, 025324 (2018)

the discrete attenuation coefficients, namely, heterogeneity degree in coal. The attenuation coefficient
variance is defined as:
Xn  2
s= µi,j,z − µ /n3 (4)
i=1,j=1,z=1

By Eq. (3) and Eq. (4), the average attenuation coefficient and variance of each subsample after
the second X-ray CT scanning and 3-D reconstruction can be acquired to characterize the average
density and heterogeneity degree. The average attenuation coefficient and variance of each subsample
are shown in Table I.
It can be seen that there are small differences in the average attenuation coefficients, but there are
still distinctions in the attenuation coefficient variance, indicating the material distribution differences
in these subsamples. Once the average attenuation coefficients and variances of any two subsamples
both accord with Eq. (5) and Eq. (6), then the two subsamples are deemed as similar subsamples with
close average densities and similar heterogeneity degrees. Otherwise, the two samples are regarded
as different subsamples.
µm + µn
!
∆µ = | µm − µn | / ≤ 3% (5)
2
s + s 
m n
∆s = |sm − sn | / ≤ 10% (6)
2
Where ∆µ is the difference of the average attenuation coefficients of two subsamples, ∆s is the
difference of the attenuation coefficient variances; µm and µn are the average attenuation coefficients
of the sample m and n, and sm and sn are their attenuation coefficient variance respectively.
By the above algorithm, these subsamples can be divided into three categories preliminarily, and
large, moderate and small average attenuation coefficient and variance are used to generally describe
and analyze the probable meso structure characteristics in each category.
(a) In category A, the subsamples have small attenuation coefficient variances and moderate aver-
age attenuation coefficients. 1-2, 1-3, 2-2 and 2-3 belong to this category. The small attenuation
coefficient variances indicate that both the differences in density distribution and the hetero-
geneity degrees are small, and the moderate average attenuation coefficients mean moderate
density, so the probable meso structure may be quite dense coal matrix with lowly developed
pores.
(b) In category B, the subsamples have moderate attenuation coefficient variances and small average
attenuation coefficients. 1-4, 1-5 and 2-1 are in this category. Compared with the subsamples in
category A, the subsamples in category B have slightly larger attenuation coefficient variances
and slightly smaller average attenuation coefficients. The slightly larger attenuation coefficient
variances mean a little more heterogeneous density distribution, suggesting the probable meso
structure may be coal matrix with a little more developed pores or coal matrix with pores and
clay minerals together, however, the slightly smaller average attenuation coefficients rule out
the latter possibility. That is because the density of clay minerals is larger than that of coal
matrix, and far larger than that of pores and fractures, if clay minerals are assumed existing in

TABLE I. Average attenuation coefficient and variance of each subsample.

Category Subsample number The average attenuation coefficient The attenuation coefficient variance (10-5 )

C 1-1 0.034 188 5.722

1-2 0.033 257 3.963
A
1-3 0.033 306 3.711
1-4 0.032 160 4.888
B
1-5 0.032 542 4.570
B 2-1 0.030 091 2.963
2-2 0.030 764 2.361
A
2-3 0.030 391 2.144
C 2-4 0.031 166 5.302
025324-6 Cai, Feng, and Zhou AIP Advances 8, 025324 (2018)

subsamples, then the density will increase evidently, resulting in large attenuation coefficients,
which is opposite to the testing results. So, given the slightly smaller average attenuation coef-
ficients, the probable meso structure may be coal matrix with more developed pores. Compared
with subsamples in category A, a little more pores are in subsamples in category B, which lead
to smaller density and higher heterogeneity.
(c) In category C, the subsamples have large attenuation coefficient variances and large average
attenuation coefficients. 1-1 and 2-4 are in this category. Compared with the aforementioned
subsamples, the quite large attenuation coefficient variances show the largest heterogeneity in
material distribution. Meanwhile, the average attenuation coefficients of both subsamples are
also the largest overall. In view of the material density differences in clay minerals, coal matrix
and pores/fractures, the probable meso structure of the two subsamples may be coal matrix
mixed with developed pores and clay minerals, thus the densities and heterogeneity degrees of
subsamples in this category both are the largest.
B. Morphology by SEM
After the SEM scanning, representative SEM images were chosen from hundreds of scanning
images to exhibit the meso and micro morphology information of each subsample. The magnification
of SEM image determines the information it can reflects, such as the number and size of pores and
fracture. If the magnification is too large, the absolute size of the region scanned will be too small,
and the detailed material and structural information reflected by this single SEM image is not typical
and representative. Otherwise, if the magnification is too small, pores and fractures will be too small
on the SEM image, which makes it difficult to distinguish the pores from matrix. After several
attempts, two SEM images of the same scanning area at the same operating voltage of 30 kV, with
magnification of 100 and 1000 respectively, were chosen and illustrated to show the meso morphology
characteristics of each subsample (Fig. 4). From these SEM images, the distribution of pores and clay
minerals can be clearly observed, and the structural and material morphology of each subsample can
be fully and thorough reflected without missing any essential information.
As shown in Fig. 4, for coking coal subsamples, in 1-1, pores are developed and mainly of them
are cell pores, besides, some pores are filled with mineral crystal, and the entire morphology shows
obvious heterogeneity. As for 1-2 and 1-3, the pore development degree is quite low and only a few
pores can be detected under SEM scanning. While 1-4’s structure is quite different from others’. The
coal matrix of 1-4 is composed of orderly flake-like phyteral, whose mainly composition is fusinite.
Compared with regular dense coal matrix of vitirnite, the matrix of phyteral contains more pores and
presents larger specific surface area owing to the special structure. In 1-5, the pore development is
obvious.
For the lean coal subsamples, in 2-1, the pore development is obvious, too, and pores larger than
10 um can be clearly seen in SEM image. The meso structure of 2-2 and 2-3 is dense coal matrix with
few pores. The meso morphology of 2-4 is quite complex. The developed pores are distributing in
coal matrix, and most of the pores are induced by mineral crystal. In addition, some mineral crystals
fill in pores, and some are scattering on the matrix surface. High structural and material heterogeneity
is presented in 2-4.

C. Comparison of meso structure by X-ray CT and SEM

The X-ray CT and SEM are both scanning methods for meso structure and morphology, so in
this section, the meso structure od subsamples in different categories by X-ray CT scanning and the
directly visible meso morphology by SEM scanning are compared and analyzed.
In category A, the probable meso structure may be quite dense coal matrix with lowly developed
pores. 1-2, 1-3, 2-2 and 2-3 belong to this category. From SEM images, it can be seen that few pores
are shown in 1-2 and 1-3, and the pore development in 2-2 and 2-3 is poor. The structure of the
four subsamples is similar to each other, and is all dense coal matrixes with lowly developed pores,
which is coherent to the structure detected by X-ray CT scanning. In category B, the probable meso
structure may be coal matrix with more developed pores. 1-4, 1-5 and 2-1 are in this category. As
can be seen from SEM images, many pores can be seen clearly in 1-4 due to the special flake-like
structure, and pores highly develop in 1-5 and 2-1, macro pores can be easily detected. In category C,
025324-7 Cai, Feng, and Zhou AIP Advances 8, 025324 (2018)

FIG. 4. SEM images of subsamples.

1-1 and 2-4 belong to this category, and the probable meso structure of the two subsamples may
be coal matrix mixed with developed pores and clay minerals. According to SEM images, in 1-1,
pores are developed and mainly of them are cell pores, and some pores are filled with mineral crystal.
In 2-4, developed pores are distributing in coal matrix, besides, some mineral crystals fill in pores, and
some are scattering on the matrix surface. The structure of the two subsamples is complex, showing
high material and structural heterogeneity. In summary, the meso structure of subsamples in three
categories preliminarily divided by CT quite accords with the morphology by SEM generally, so it is
quite suitable to classify and judge the material distribution and pore development of coal samples by
the average density and heterogeneity degree, however, the more detailed pore shape and coal matrix
morphology information cannot be acquired by CT, thus SEM scanning is still needed, for example,
1-4 and 1-5 are close in average density and heterogeneity degree, and both the two subsamples’
probable meso structure may be coal matrix with high developed pores according to the preliminary
division of CT scanning. However, by contrast with SEM images, although their meso structures are
025324-8 Cai, Feng, and Zhou AIP Advances 8, 025324 (2018)

both matrixes with developed pores indeed, their morphologies are totally different to each other.
The coal matrix of 1-4 is orderly flake-like phyteral, and the pores in matrix are mainly original plant
tissue pores, which are typically layered in order with regular size of 2∼5 um, while the matrix in
1-5 is vitrinite with obvious developed pores, and the pores are mainly metamorphic pores induced
by tectonic stress.
To sum up, it is quite suitable and reasonable to classify and judge the material distribution
and the pore development of coal samples by the average attenuation coefficient and variance by
X-ray scanning, and the probable meso structure in three categories accords with the morphology by
SEM scanning quite well. However, the detailed pore shape and coal matrix morphology information
cannot be distinguished by X-ray scanning, and SEM scanning is still needed.

IV. PORE DEVELOPMENT

A. Pore size distribution
The decimal classification method of pores proposed by Xodot31 is used in this paper, namely,
micro pores (<10 nm), transition pores (10∼100 nm), meso pores (100∼1000 nm) and macro pores
(>1000 nm).
By MIP testing, the pore size distribution curve of each subsample is shown in Fig. 5. For coking
coal subsamples, in 1-1, there are two peaks in its pore size distribution curve, the micro pores at
the diameter of 7.13 nm and the macro pores at the diameter of 5.67 um are the most developed.
1-2 and 1-3 have similar unimodal pore size distribution at the diameter of 7.16 nm and 9.27 nm
respectively. In 1-4, Micro pores are the most developed, then transition pores and macro pores
follow, and the meso pores are the least developed. In 1-5, the macro pores are the most developed,
and the representative macro pore diameter is about 12.29 um, the micro pores and transition pores
are moderately developed, and the meso pores are the least developed. For lean coal subsamples,
obvious bimodal or multimodal distribution is presented. In 2-1, there are three peaks in the pore
size distribution curve, and the representative diameters are 7.12 nm, 6.28 um and 14.9 um, besides,
the macro pores are the most developed, and the micro pores and transition pores are moderately

FIG. 5. Pore size distribution curves.

025324-9 Cai, Feng, and Zhou AIP Advances 8, 025324 (2018)

developed, and the meso pores are least developed or do not develop at all. 2-2 and 2-3 have similar
pore size distribution curve, that is, the most developed micro pores, moderately developed macro
pores, then the less developed transition pores and the least developed meso pores. In 2-4, the macro
pores are the most developed, and the representative diameter is about 14.5 um. The micro pores and
transition pores are moderately developed, and the meso pores are the least developed.
Comparing the pore size distribution curve and the meso structure and morphology characteristics
of each subsample, it is found that in spite these subsamples can be divided into three categories by
their meso structure by CT and SEM scanning, while little corresponding distinction on their pore
size distribution can be related to their meso structures. It seems that there is no evident relationship
between meso structure and pore size distribution, for example, in 1# coking coal subsamples, only
1-2 and 1-3 show different pore size distribution characteristics from others, and little differences are
shown in 1-1, 1-4 and 1-5, so is the pore size distribution in 2# coking coal subsamples, there are
some differences, but not obvious. The main reason for this phenomenon lies in the different scales
of the observation methods. The resolution of CT scanning is 14.7 um, and only pores larger than
14.7 um can be detected. The main observation scale of SEM scanning is about 0.01∼100 um, while
the scale of MIP can be nano scale. As for the pores ranging from 7 nm to 14.7 um, they can be
detected by MIP, but cannot be recognized by CT and SEM totally, thus there are inconsistencies
when observation results at different scales are compared.
B. Macro pore volume
In order to analyze the pore development at the same scale with X-ray CT scanning and SEM
scanning, the volume of super macro pores (larger than 14.7 um) were summed on the basis of
the accumulated mercury injection/accumulated pore volume curve (Fig. 6). It can be seen that
the accumulated macro pore volume order of these subsamples are: 1-4>1-5>1-1>1-2>1-3, and
2-4>2-1>2-2>2-3.
As analyzed before, the probable meso structure of 1-4 is coal matrix with developed pores,
and the real coal matrix morphology under SEM scanning is flake-like phyteral with developed
macro pores. Many macro pores can be seen clearly on SEM images, which accords with the quite
developed macro pores by MIP. In 1-5, the macro pores are obvious developed according to SEM and
CT scanning, and this can also be verified by the pore size distribution curve. Similarly, in 1-1, pores
are developed, too. For 1-4, 1-5 and 1-1, many evident macro pores can be seen on their SEM images,
and their macro pores are quite developed in MIP, too, so the accumulated super macro volumes of
the three subsamples are quite large. As for 1-2 and 1-3, both meso structures are dense matrix with
lowly developed pores, and the macro pores are lowly developed on the pore size distribution curves,
so the accumulated super macro volumes of the two subsamples are small. In lean coal subsamples,
in 2-1, macro pores are evidently developed on SEM images, and the pore size distribution curve also
shows that the macro pores are the most developed. In 2-4, the SEM images show that the developed
macro pores are distributing in coal matrix, and from the pore size distribution curve, the macro pores
are the most developed, too, so the accumulated macro volumes of 2-1 and 2-4 are quite large. As for
2-2 and 2-3, few super macro pores can be seen in their SEM images, and the macro pores are not
developed as obviously as that in 2-1 and 2-4, so the accumulated super macro volumes of 2-2 and
2-3 are smaller.

FIG. 6. The accumulated pore volume of samples.

025324-10 Cai, Feng, and Zhou AIP Advances 8, 025324 (2018)

Generally, the meso structure information offered by CT and SEM scanning do not accord with
the entire pore size distribution characteristics due to different observation scales. However, once
the observation scales of the three methods are all unified to macro scale, the super macro pore size
distribution can be related to the meso structure category, the pore development and morphology
reflected by CT and SEM very well at the same scale.
C. Porosity
Both X-ray CT scanning and MIP testing can be used to calculate the porosity of samples
quantitatively. After the second CT scanning, 3-D reconstruction and threshold segmentation were
used to calculate the porosity of subsamples. In the MIP testing, the porosity is calculated by the ratio
of accumulated pore volume to sample volume. The porosity calculated by CT scanning is defined
as nCT , and the porosity measured by MIP is defined as nMIP . As limited in MIP testing, only open
pores (>7 nm) can be measured, and partial closed pores cannot be detected, which is impossible to
be avoided. In this paper, the closed pores are ignored, and the volume of open pores larger than 7 nm
is regarded as the entire pore volume of sample, so the entire porosity is the ratio of all open pores
d ≥7nm
(>7 nm) volume to coal sample volume, and is written as nMIP , the super macro pore porosity is
d ≥14.7um
the ratio of super macro pores (>14.7 um) volume to coal sample volume, and is written as nMIP .
The porosities of each subsample measured by CT and MIP were calculated and shown in Fig. 7.
d ≥14.7um
From Fig. 7, it can be seen that nCT and nMIP have similar trends in these subsamples, but
d ≥7nm
little relevance is shown between nCT and nMIP , especially in 2# lean coal subsamples. The reason
also lies in the different observation scales. The resolution of CT scanning is 14.7 um, while the scale
of MIP is nano scale. Pores larger than 14.7 um can be detected by both methods, as for pores with
diameter ranging from 7 nm to 14.7 um, they could be detected by MIP, but cannot be recognized
d ≥7nm
by CT, so the porosity nCT do not accord with porosity nMIP . The porosities measured by CT and
d ≥14.7um
MIP show that nCT and nMIP presents quite well consistence at the same observation scale, while
d ≥7nm
large difference exists between nCT and nMIP due to scale differences.
D. Permeability
A new permeability calculation method on basis of capillary pressure was put forward by Gürdal
& Yalçın.32 It is assumed that the pore system of rock material is composed of different capillaries
with different sizes, and the entire pore volume is divided into several intervals with the same volume.
The interval permeability is calculated, and then the entire permeability is obtained by adding the
interval permeability together in statistical view. The entire permeability of porous rock material can
be drawn as: f g
k = φ4/3 /8n2 r 2 1 + 3r 2 2 + 5r 2 3 + · · · + (2n − 1)r 2 n
X n  (7)
= φ4/3  (2i − 1)r 2 1  /8n2
 i=1 

FIG. 7. Porosity of samples measured by CT and MIP.

025324-11 Cai, Feng, and Zhou AIP Advances 8, 025324 (2018)

Where k is the entire permeability, φ is the porosity, n is the intervals (generally, n=10), and r i is the
corresponding pore diameter of each interval (r1 > r2 > r3 > · · · > rn ).
The contribution of each interval to the entire permeability is:
n
X
mi = (2i − 1)r 2 1 / (2i − 1)r 2 1 (8)
i=1

As indicated by Eq. (8), the larger pore diameter of the interval, the larger contribution to the entire
permeability, so the contribution of macro pores to the entire permeability is the maximum, which
has been proved by Yao & Liu24 and Wang et al.33 As we all know, highly developed macro pores are
more suitable to form seepage paths in coal reservoirs for gas transport than other pores, so the macro
pores developed subsamples, such as 2-1, 2-4, 1-4 and 1-5 may be potential suitable reservoir for
CBM exploitation. However, it is noteworthy that the coal matrix in 1-4 is orderly and shape-regular
fusinite, within many tissue pores, while the fusinite usually develops along one direction, and few
tissue pores are connected, so reservoirs with pore system like 1-4 are not suitable to be chosen for
CBM exploitation because of the low connectivity although the pores in 1-4 are the most developed.
Besides, micro and transition pores are the main places for gas adsorption and storage, and about
80∼90% coal bed methane gas is stored there, so the micro and transition pores are also important
factors to be considered for CBM reservoir choice. Comparing the pore size distribution curve of
each subsample, it can be found that, both micro pores and macro pores are much more developed in
2-1 than that in other subsamples, given the larger gas storage capacity and more seepage paths, so
porous coal reservoirs with pore system like 2-1 subsample may be the most suitable coal reservoir
for CBM exploitation.

V. CONCLUSIONS
The X-ray CT scanning, SEM scanning and MIP testing are important meso and micro observa-
tion methods for porous material, and they are different in applications due to respective precisions
and observation scopes. In this paper, multi-scale X-ray CT scanning, SEM scanning and MIP testing
were all conducted to study the material distribution, morphology information and pore development
in coals, and four important conclusions were obtained as follow:
(a) The subsamples can be divided into three different meso structural categories by average density
and heterogeneity degree. Comparing with the morphology information from SEM images, it
is quite suitable and reasonable to classy and judge the meso structure of coal samples by X-ray
CT scanning, but SEM scanning is still needed to get the further morphology information.
(b) By MIP testing, the pore size distribution and pore development of each subsample were
obtained, and there was inconsistence between pore size distribution by MIP and meso structure
by CT and SEM due to scale differences. In order to meet the observation scale of CT and SEM,
the accumulated super macro pore volumes were summed. The macro pore development and
the accumulated super macro pore volume accorded with the meso structure category and
morphology information by CT and SEM very well.
(c) The porosity of each subsample was measured by CT scanning and MIP testing at different
d ≥7nm
observation scales. Owing to the scale differences, there was inconsistence in nCT and nMIP ,
d ≥14.7um
but the nCT accorded with nMIP very well at the same observation scale.
(d) In view of the effect of macro pores on permeability and the contribution of micro pores to
CBM storage capacity, porous coal reservoirs with developed micro pores and macro pores,
like 2-1, may be the most suitable coal reservoir for CBM exploitation.

ACKNOWLEDGMENTS
Support for this work is provided by National Natural Science Foundation of China (No.
21373146) and San Jin scholars support plan by Natural Science Foundation of Shanxi Province
(2016), which are greatly acknowledged by the authors.
025324-12 Cai, Feng, and Zhou AIP Advances 8, 025324 (2018)

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