minerals

Article
Nano-Scale Pore Structure and Its Multi-Fractal
Characteristics of Tight Sandstone by N2
Adsorption/Desorption Analyses: A Case Study
of Shihezi Formation from the Sulige Gas Filed,
Ordos Basin, China
Zhelin Wang , Xuewei Jiang, Mao Pan and Yongmin Shi *
School of Earth and Space Sciences, Peking University, Beijing 100871, China; zhelin_wang@pku.edu.cn (Z.W.);
jiangxw@pku.edu.cn (X.J.); panmao@pku.edu.cn (M.P.)
* Correspondence: sym@pku.edu.cn




Received: 16 March 2020; Accepted: 20 April 2020; Published: 22 April 2020


Abstract: Fractal dimension is a critical parameter to evaluate the heterogeneity of complex pore
structure in tight sandstone gas and other low permeability reservoirs. To quantify the fractal
dimension of tight sandstone at various pore size classes and evaluate their implications on mineral
composition and nano pore structure parameters, we conducted an integrated approach of N2
adsorption/desorption experiment (N2 -GA), X-ray diffraction (X-RD), and field emission scanning
electron microscopy (FE-SEM) on Sulige tight sandstone reservoirs. By comparing the nine types of
fractal dimensions calculated from N2 adsorption data, we put forward the concept of “concentrated”
fractal dimensions and “scattered” fractal dimensions (DN2 , DN3 , DN5 , DN7 and DN8 ) for the first
time according to its concentration extent of distribute in different samples. Result shows that
mineral composition has a significant influence of a different level on specific surface area (SSA),
pore volume (PV), and fractal dimensions (DN ), respectively, where the “scattered” fractal dimension
is more sensitive to certain specific property of the reservoir, including mineral content and the
specific surface area contribution rate (Sr ) of type II mesopores (Mesopore-II: 10~50nm). In addition,
three type of hysteresis loops were distinguished corresponding to different pore shape combination
of N2 -GA isotherm curve, which reveals that pore structure heterogeneity is mainly controlled
by inkbottle-shaped pores and the volume contribution rate (V r ) of mesopores in this study area.
These findings could contribute to a better understanding of the controlling effect of pore heterogeneity
on natural gas storage and adsorption.

Keywords: tight sandstone; fractal dimension; nanopore structure; Sulige gas field; Shihezi Formation

1. Introduction
Energy sources around the world have been changing from solid (firewood and coals) and liquid
(petroleum) states to gas state (natural gas) [1], where tight sandstone reservoirs have been playing an
important role and exploited industrially in many countries as an effective storage of natural gas, which
is a complicated porous material with a highly heterogeneous nanopore structure [2–8]. Owing to the
complexity of the its pore-throat system, pore structure and its fractal characteristics analysis become
the core work of reservoir quality evaluation, which includes the research content of specific surface
area (SSA), pore volume (PV), pore size distribution (PSD), pore morphology, and anisotropy [9–11].
Due to the complicated 3D characteristics of a tight sandstone pore-throat system, it is difficult for
traditional Euclidean geometry to describe the pore morphological characteristics precisely. Fractal

Minerals 2020, 10, 377; doi:10.3390/min10040377 www.mdpi.com/journal/minerals

Minerals 2020, 10, 377 2 of 21

theory is an effective approach to evaluating the surfaces roughness and complexity of irregular pores,
which was first proposed by Benoit B. Mandelbrot in 1983 [12–17], where fractal dimension is an
essential feature parameter. It can quantitatively characterize nanoscale pore heterogeneity and make
a better understanding of the pore microstructures complexity comprehensively, with a value usually
distributed between two and three. In general, fractal dimension value often reflects the heterogeneity
of the pore-throat system including connectivity, coordination, and the complexity of pore shape,
where a higher value indicates a more complex pore-throat system [18,19]. In addition, fractal theory
also reveals that the rock surface displays a property of “self-similar regularity” at molecular scales
and exhibits a similar structure regularity over 3-4 orders of magnitude resolution scales in length
between 1 nm and 100 µm [20,21].
In recent years, with the development of pore structure characterization technology, there are four
established methods to calculate fractal dimensions based on experimental data: fluid injection
technique, gas adsorption [22,23], image analysis [18,19], and no-destructive methods through
CT scanning [24,25], where fluid injection technique includes low-field nuclear magnetic
resonance (NMR) [21,26–28] and mercury intrusion porosimetry (MIP) [29–31]. In terms of N2
absorption/desorption data, numerous studies have applied Frenkel–Halsey–Hill (FHH) model to
study the fractal characteristics of nanopore structure in different reservoir, including coal-bearing
organic shale in different facies [20,21,32–38], coal [23,39–42], or tight sandstone [29,30], which is
proven to be an efficient method to capture fractal dimensions aim at nanoscale pores (2–400 nm) [43].
Previous research usually obtained fractal dimensions by the unsegmented method, or capture two
fractal dimensions D1 (P/P0 : 0–0.5) and D2 (P/P0 : 0.5–1) represents the fractals generated by volume
irregularity and pore structures, respectively [18]. Moreover, many of them have already made a
comparative study between N2 adsorption with NMR or MIP [30,37,44], whereas the scientificity
and validity of different fractal dimensions obtained from nitrogen adsorption data have not been
distinguished, and its influence factors are still not explicit.
Therefore, in this paper, N2 adsorption/desorption experiment (N2 -GA) was utilized to accurately
characterize the nanoscale pore heterogeneity, morphology and structure parameters of 11 different
ranks of tight sandstone from the Sulige gas field. Fractal characteristics of pore throats with different
sizes were specified according to the FHH model. Furthermore, field emission scanning electron
microscopy (FE-SEM) was used to help make more explicit the pore morphology features, petrographic
characteristic and the relationship between them. In addition, we used X-ray diffraction (X-RD) to
characterize the mineral composition of all samples accurately. First, pore morphological characteristics
and mineral composition were identified by FE-SEM and X-RD. Then, based on N2 -GA data of all
11 samples, we effectively captured the PSD, SSA, and PV, and nine types of fractal dimensions
were calculated to understand the complexity of pore microstructures comprehensively, which can
clarify the effect of mineral composition and pore structure on different types of fractal dimensions,
respectively. Hence, the major aims of this study were to (1) quantitatively characterize the nanoscale
pore heterogeneity of tight sandstone in He 8 Member at different size classes and (2) clarify the effect
factor of different types of fractal dimensions, respectively.

2. Samples and Methods

2.1. Samples and Geological Setting

The tight sandstone gas field in the Sulige area is located in the northwest of Yishan slope in the
Ordos Basin, which is a typical example of tight gas in China. The Ordos Basin is the second largest
sedimentary basin in China (Figure 1a), which is located in the western part of North China Craton,
and is a large multi-cycle superimposed basin with overall uplift and simple geotectonics [45,46].
According to previous studies, the eighth member of the Middle Permian Lower Shihezi Formation
(He 8 Member) is generally considered as a set of deposits of braided river-shallow delta facies, with a
Minerals 2020, 10, 377 3 of 21
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a larger
larger variation
variation rangerange of hydrodynamic
of hydrodynamic conditions.
conditions. Under a Under a gentle
wide and wide geotectonic
and gentle background,
geotectonic
background,
the the channel
channel changes changes
and overlaps in and
variousoverlaps in forming
periods, various aperiods,
complexforming a complex
pattern structure pattern
[47].
structure [47].
Based on core observation, 11 tight sandstone samples with different physical characteristics were
Based
collected onthe
from core
Heobservation,
8 Member in11 thetight
Ordos sandstone samples
Basin, which with gas
is a main different physical
production layercharacteristics
of the Sulige
were gas
large collected from(Figure
province the He1b).
8 Member
In order in to
thedetermine
Ordos Basin, which is a mainofgas
the heterogeneity production
nanoscale porelayer of the
structure,
Sulige large gas province (Figure 1b). In order to determine the heterogeneity of nanoscale
we collected core samples from one appraisal well where the burial depth varies from 3326 m to 3358 pore
m.
structure,
Figure we collected
2 shows core samples
the generalized from onecolumns
stratigraphic appraisalofwell where the
the Shihezi burial depth
Formation and varies
samplingfrom 3326
depth
m toits3358
and m. Figure 2logging
corresponding shows profile
the generalized
and gamma (GR) curve.columns of the Shihezi Formation and
stratigraphic
sampling depth and its corresponding logging profile and gamma (GR) curve.

Figure 1.1. Location

Figure Location of
of the
the study
study area
area showing
showing in
in the
the tectonic
tectonic map
map ofof Ordos
Ordos Basin.
Basin. (a)
(a) Geographic
Geographic
location of the Ordos Basin; (b) geographic location of the study area.
location of the Ordos Basin; (b) geographic location of the study area.
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Figure 2. Schematic diagram of sampling location. (a) Generalized stratigraphic columns of the Shihezi
Figure 2. Schematic diagram of sampling location. (a) Generalized stratigraphic columns of the
Formation (modified from reference [47]); (b) sampling depth and its corresponding logging profile
Shihezi Formation (modified from reference [47]); (b) sampling depth and its corresponding logging
and gamma (GR ) curve.
profile and gamma (GR ) curve.
2.2. Experimental Methods
2.2. Experimental Methods
All 11 samples were analyzed using X-RD analysis, FE-SEM observation, and N2 -GA.
First,All 11 samples
pore were analyzed
morphological using X-RD
characteristics and analysis,
mineral FE-SEM observation,
composition and N2-GA.
were identified by First,
XRD pore
and
morphological characteristics and mineral composition were identified by XRD
FE-SEM. Then built on N2 adsorption data of all 11 samples, whicheffectively captured PSD, SSA, and FE-SEM. Then
builtPV.
and on Three
N2 adsorption data of loop
types hysteresis all 11were
samples, whicheffectively
distinguished, and ninecaptured
types ofPSD, SSA,
fractal and PV. Three
dimensions were
types hysteresis
calculated loop were
to understand thedistinguished,
complexity of and porenine types of fractal
microstructures dimensions were calculated to
comprehensively.
understand the complexity of pore
N2 adsorption/desorption microstructures
isotherms comprehensively.
were obtained using a Quantachrome QUADRAS-ORB SI
N2 adsorption/desorption
Surface Area and Pore Size Analyzer isotherms were obtainedBoynton
(Quantachrome, using a Beach,
Quantachrome
FL, USA)QUADRAS-ORB
–196.15 ◦ C, withSI a
Surface
pore sizeArea
test and
range Pore Size Analyzer
of 0.35–400 (Quantachrome,
nm. Experimental Boynton
process was Beach, FL, USA)
conducted with a–196.15
mixture°C,ofwith
blocka
pore size test range of 0.35–400 nm. Experimental process was conducted with
sample and 60–80 mesh powder samples for the purpose of eliminating the experimental error caused a mixture of block
sample
by andsize
sample 60–80 mesh powder
in accordance withsamples for thegovernment
the Chinese purpose of eliminating
standard GB/Tthe experimental
19587-2017. error caused
by sample size in accordance with the Chinese government standard
X-RD was employed as a supporting test for analyzing mineral composition, GB/T 19587-2017.using powder
X-RD was employed as a supporting test for analyzing mineral composition,using
samples that were crushed to less than 200 mesh size. The X-ray diffractometer was operated at powder
25 ◦ C
samples
and that werewith
10% humidity crushed
a steptoofless
0.01than
◦ (2θ)200 mesh size.
performed The
using X-ray diffractometer
a PANalytical was operated
X’Pert3 Powder at 25
(PANalytical,
°C and 10% humidity with a step of 0.01°(2 θ ) performed using a PANalytical
Almelo, The Netherlands), with the procedure adhering to the Chinese Oil and Gas Industry Standard X’Pert3 Powder
(PANalytical,
SY/T5163 Almelo, The Netherlands), with the procedure adhering to the Chinese Oil and Gas
(2018).
Industry Standardanalysis
The FE-SEM SY/T5163 was(2018).
completed using a FEI Quanta 650 high performance multipurpose field
The FE-SEM analysis
emission-scanning was completed
electron microscopy (FEI,using a FEIOR,
Hillsboro, Quanta
USA).650 high
Prior performancetight
to observation, multipurpose
sandstone
field emission-scanning
samples were polishing electron microscopy
by an Ar-ion milling(FEI, Hillsboro,
system, and theOR,samples
USA). Prior
were to observation,
then tight
sputter-coated
sandstone samples were polishing by an Ar-ion milling system, and the samples
with chromium for conductivity. The specifications for the high-resolution imaging and analysis of were then sputter-
coated with chromium for conductivity. The specifications for the high-resolution imaging and
Minerals 2020, 10, 377 5 of 21

the conductive samples were acceleration voltage: 200 V–30 kV; resolution: 1.4 nm at 30 kV under
environmental vacuum conditions (ESEM); and magnification: 80–6 × 1,000,000.

2.3. Fractal Model of N2 Adsorption

The FHH model has proven to be an effective model and has been widely used to obtain the
fractal dimension based on N2 adsorption data [22,48–50], which can be expressed as the following
double logarithm form:
ln(V ) = k × ln[ln(P0 /P)] + C (1)

where V is the volume of N2 adsorption capacity at equilibrium pressure in cm3 /g, P0 is the gas
saturation pressure in MPa, P is the gas equilibrium pressure in MPa, C is constant, and k is the slope
of ln(V) vs. ln(P0 /P) linear fitting plots. On this foundation, fractal dimension (DN ) based on N2
adsorption/desorption can be calculated by following equation:

DN = k + 3 (2)

3. Results

3.1. Minerals Composition

According to the X-RD result of investigated core samples, the mineral composition of the
investigated samples shown in Table 1 and Figure 3, it can be seen that He 8 Member tight sandstone
mainly consists of quartz, clay, calcite, and feldspar. Quartz abundance between 49.6% and 93.6%
averages at 81.5%. Total clay content ranges from 3.0% to 31.3% with an average value of 14.0%,
in which the content of chlorite is highest (from 19.0% to 77.0%, averages at 43.5%), followed by
kaolinite (from 11.0% to 57.0%, averages at 28.5%), illite/smectite (from 3.0% to 37.0%, averages at
16.8%), and illite (from 6.0% to 27.0%, averages at 13.8%). These clustered intercrystalline micropores
of clay minerals exist as a local enrichment form with poor connectivity, developed inside original
intergranular pores wherefore the percolation capacity of the reservoir was impaired to a certain extent
as well.

Table 1. Mineral composition based on X-ray diffraction (X-RD) analysis of the eighth member of the
Middle Permian Lower Shihezi Formation (He 8 Member) tight sandstone.

Mineral Composition (%) Clay Composition (%)

Sample ID
Q F C Clay I/S I K C
SU-1 90.6 0.2 4.2 5 5 7 57 31
SU-2 93.6 0.2 6.2 15 12 11 62
SU-3 93.3 0.2 0.4 6.1 21 15 38 26
SU-4 89.5 0.2 3.8 6.5 3 13 48 36
SU-6 87.8 0.4 1 10.8 10 13 22 55
SU-7 88.2 0.2 11.6 6 17 77
SU-9 49.6 0.4 33.5 16.5 28 16 23 33
SU-10 67.2 1.5 31.3 37 27 17 19
SU-13 73.6 0.2 1.1 25.1 11 16 35 38
SU-14 84.7 0.5 0.6 14.2 14 14 27 45
SU-15 78.8 0.6 20.6 24 13 18 45
Average 81.5 0.4 6.4 14.0 16.8 13.8 28.5 42.5
Note: Q—quartz; F—feldspar; Ca—calcite; I/S—Illite/Smectite; I—Illite; K—kaolinite; C—chlorite.
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(a) (b)
(a) (b)
Figure 3. Mineral composition bar chart of He 8 Member tight sandstone. (a) Total rock mineral
Figure
Figure 3. Mineral
Mineral
composition composition
(b) claybar
composition
bar charts; bar chart of
of He
He 88 Member
chartcomposition
mineral Member tight
tight sandstone.
bar charts. sandstone. (a)
(a) Total
Total rock
rock mineral
mineral
composition
composition bar
bar charts;
charts; (b)
(b) clay
clay mineral
mineral composition
composition bar charts.
3.2. Nanoscale Pore Geometry from N2 Adsorption/Desorption Isotherms
3.2. Nanoscale
3.2. NanoscalePorePore Geometry
Geometry from
from N N22Adsorption/Desorption
Adsorption/Desorption Isotherms
Isotherms
The N2 adsorption isotherms can be classified into six types according to the International Union
The N
The N22 adsorption
adsorption isotherms
isotherms cancan be
be classified
classified into six types
typesaccording totothe
theInternational Union of
of Pure and Applied Chemistry (IUPAC) (Figure into
4a). six
Investigatedaccording
tight sandstone International Union
samples belong to
Pure
oftype and
PureIV Applied
and AppliedChemistry
Chemistry (IUPAC)
(IUPAC)(Figure 4a).
(Figure Investigated tight sandstone samples belong to type
with a hysteresis loop, which are anti 4a).
“s” Investigated
as a whole, and tightsamples
sandstone in samples
this studybelong
area toare
IV with
type IV awith
hysteresis
asolid,loop, which
hysteresis are anti are
“s” anti
as a whole,
“s” as and samples andinsamples
this study in area
thisofare mesoporous
mesoporous whereloop, which
the hysteresis loop patterns a are
whole,
indicative of mixtures study area are
mesopores and
solid, where the
mesoporous hysteresis
solid, where loophysteresis
the patterns areloopindicative
patterns ofare
mixtures of mesopores
indicative of mixtures andofmicropores
mesopores inand
the
micropores in the samples. Furthermore, type IV N2 adsorption/desorption hysteresis loops can be
samples. Furthermore,
micropores in four
the samples.typeFurthermore,
IV N2 adsorption/desorption
type IV to hysteresis loops can
N2cylindrical
adsorption/desorption be divided
hysteresis into
loops can four
be
divided into main types, which correspond pores, inkbottle-shaped pores, parallel
main types,
divided intowhich
four correspond
main types, to cylindrical
which pores,
correspond to inkbottle-shaped
cylindrical pores, parallel platepores,shaped pores,
plate shaped pores, and wedge-/slit-shaped pores (Figure pores, inkbottle-shaped
4c) [18,40,51]. Based on the pattern parallel of
and wedge-/slit-shaped
plate shapedloops,
pores, pores (Figure 4c) [18,40,51].
poresBased on 4c)
the pattern of hysteresis onloops, the 11 He
hysteresis theand
11 Hewedge-/slit-shaped
8 Member tight sandstone (Figure
samples [18,40,51]. Basedthree
mainly exhibit the pattern
types—H1, of
H2,
8 Member loops,
hysteresis tight sandstone
the 11 Hesamples
8 Member mainly
tightexhibit
sandstonethreesamples
types—H1, H2,exhibit
mainly and H3. three types—H1, H2,
and H3.
and H3.

Figure 4. Type of adsorption isotherms and its corresponding pore types: (a) Type of adsorption
Figure 4. Type
isotherms; of adsorption
(b) specific surfaceisotherms andtested
area (SSA) its corresponding pore types: (a) Type of(BET)
range by Brunauer-Emmett-Teller adsorption
test;
Figure 4. Type
isotherms; (b) of adsorption
specific isotherms
surface area andtested
(SSA) its corresponding
range by pore types: (a) Type of(BET)
Brunauer-Emmett-Teller adsorption
test; (c)
(c) hysteresis loops and its corresponding pore shapes.
isotherms;
hysteresis(b) specific
loops surface
and its area (SSA)
corresponding tested
pore range by Brunauer-Emmett-Teller (BET) test; (c)
shapes.
hysteresis loops and its corresponding pore shapes.
Minerals 2020,
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As the result shown in Figure 5 and Table 2, type H1 including SU-6, SU-7, and SU-14 always
As the result shown in Figure 5 and Table 2, type H1 including SU-6, SU-7, and SU-14 always has
has a smaller amount N2 adsorption volume with narrow hysteresis loops, where their adsorption
a smaller amount N2 adsorption volume with narrow hysteresis loops, where their adsorption curves
curves almost completely coincide with the desorption curves and increase rapidly and
almost completely coincide with the desorption curves and increase rapidly and synchronously at a
synchronously at a P/P0 = 0.9 approaching to 1.0. This type of loop usually corresponds to the
P/P0 = 0.9 approaching to 1.0. This type of loop usually corresponds to the combination of cylindrical
combination of cylindrical pores and parallel plate shaped pores [40], the cylindrical pores often with
pores and parallel plate shaped pores [40], the cylindrical pores often with the pore size distributed in
the pore size distributed in 50–200 nm (macropores) and the parallel plate shaped pores usually with
50–200 nm (macropores) and the parallel plate shaped pores usually with the pore size varies from
the pore size varies from 5–50 nm.
5–50 nm.
Analogously, the inflection point for the rapid increase of type H3 (SU-1, SU-2, SU-3, SU-4)
Analogously, the inflection point for the rapid increase of type H3 (SU-1, SU-2, SU-3, SU-4) appears
appears around P/P0 = 0.8 with a slightly wider hysteresis loop, which is the main difference from H1
around P/P0 = 0.8 with a slightly wider hysteresis loop, which is the main difference from H1 type
type loops. This type of loop is usually related to aggregates of slit-/wedge-shaped particles giving
loops. This type of loop is usually related to aggregates of slit-/wedge-shaped particles giving rise to
rise to parallel plate shaped pore with the pore size varies from 2–50 nm (slit-/wedge-shaped) and
parallel plate shaped pore with the pore size varies from 2–50 nm (slit-/wedge-shaped) and 50–100 nm
50–100 nm (parallel plate shaped pore) [51].
(parallel plate shaped pore) [51].
For type H2 represented by SU-9, SU-10, SU-13, SU-15, the inflection point visible in the
For type H2 represented by SU-9, SU-10, SU-13, SU-15, the inflection point visible in the desorption
desorption curves appears around P/P0 = 0.5, which developed a wider hysteresis; this indicates the
curves appears around P/P0 = 0.5, which developed a wider hysteresis; this indicates the morphology of
morphology of mesopore-I present a fine bottleneck with one side almost closed or double side open
mesopore-I present a fine bottleneck with one side almost closed or double side open [18]. In addition,
[18]. In addition, parallel plate–shaped pores and cylindrical pores usually appear in combination
parallel plate–shaped pores and cylindrical pores usually appear in combination among these samples.
among these samples.

Figure 5. N2 adsorption/desorption isotherms and the corresponding pore shapes of He 8 Member

Figure 5. N2 adsorption/desorption isotherms and the corresponding pore shapes of He 8 Member
tight sandstone samples. (a1)–(a3) Samples with H1 type hysteresis loop; (b1)-(b4) samples with H2
tight sandstone samples. (a1)–(a3) Samples with H1 type hysteresis loop; (b1)-(b4) samples with H2
type hysteresis loop; (c1)–(c4) samples with H3 type hysteresis loop.
type hysteresis loop; (c1)–(c4) samples with H3 type hysteresis loop.
3.3. Specific Surface Area, Pore Volume, and Pore Size Distribution
3.3. Specific Surface Area, Pore Volume, and Pore Size Distribution
The nanopore structure parameter in this study was calculated by the BET model (SSA) [52], BJH
model The nanopore
(PV structure
of mesopores) [53],parameter
and HK-SF in model
this study
(PV was calculated by
of micropores) the on
based BETN2model (SSA) data.
adsorption [52], BJH
It is
model (PV ofthat
noteworthy mesopores)
the closed[53], andare
pores HK-SF model (PV
not included in of
themicropores) based
BET test result on N2 4b).
(Figure adsorption data. It
The nanoscale
is noteworthy
pore thatanalysis
quantitative the closed pores are of
consequence notHe
included in the
8 Member BET
tight test result
sandstone by(Figure 4b). The nanoscale
N2 adsorption-desorption
pore quantitative analysis consequence of He 8 Member tight sandstone by N2 adsorption-desorption
Minerals 2020, 10, 377 8 of 21

experiments can be seen in Table 2. The BET SSA (SBET ) ranges from 0.530–3.162 m2 /g (averages at
1.297 m2 /g). The BJH adsorption cumulative SSA (SBJH ) ranges from 0.925–3.858 m2 /g (averages at
1.641 m2 /g), where the average value is higher than SBET . The BJH adsorption cumulative volume
(V BJH ) ranges from 3.291–13.379 × 10–3 cm3 /g (averages at 6.703 × 10–3 cm3 /g) showed a good positive
relationship with SBET (R2 = 0.569) (Figure 6a) and SBJH (R2 = 0.657) (Figure 6b). The SF micropore
volume (V SF ) ranges from 1.198 ~ 0.220 ×1 0–3 cm3 /g with an average of 0.518 × 10–3 cm3 /g, which
shows a better positive relationship with SBET (R 2 = 0.988) (Figure 6c) and SBJH (R2 = 0.903) (Figure 6d),
this result indicated that micropores has a higher contribution to SSA than mesopores and macropores.
The N2 maximum absorbed amount (AM ) of 11 sample ranges from 1.950–8.266 cm3 /g (averages
at 4.155 cm3 /g), which showing an excellent positive relationship with PV (V BJH : R2 = 0.997, V SF :
R2 = 0.615) (Figure 6e,f). This result revealed that N2 maximum absorbed amount can represent
the total PV of different samples, where the mesopores have a higher contribution. In consequence,
we divided samples into three types depending on the maximum adsorption capacity, which can
reflect the reservoir quality. Class A samples including SU-13, SU-14, SU-15, AM are within the range
of 7.0–10.0 m2 /g, with an average value of 8.453 m2 /g among three samples. Class B samples including
SU-6, SU-7, SU-9 SU-10, AM are within the range of 3.0~7.0 m2 /g, with an average value of 4.148 m2 /g.
among four samples. Class C samples including SU-1, SU-2, SU-3, SU-4, AM are within the range of
0.1–3.0 m2 /g, with an average value of 4.148 m2 /g among four samples.
Among all three types samples, Class C samples only have a single form hysteresis loop type
(H3 type loop). Whereas Class B developed H1 type loop (SU-6, SU-7) and H2 type loop (SU-9, SU-10)
simultaneously. This phenomenon is related to the complex morphological features of mesopores
in samples with H2 type loop as well as a smaller volume of the micropore (V SF ) in samples with
H1 type loop. Furthermore, as listed in Table 2, the total adsorption average pore width (W T ) ranges
from 10.329–45.9839 nm with an average of 24.036 nm, where samples with H1 type loop often have a
larger total pore average width, while samples with H2 type loop always have a smaller one. Based
on the corresponding pore shapes to H2 type loops, revealed a large amount of bowl-shaped pores
in mesopores, which is the transitional form from an inkbottle-shaped pores to parallel plate shaped
pores, such as SU-9 (Figure 5b1) and SU-10 (Figure 5b2).

Table 2. Results of pores surface area, volume and pore width by N2 adsorption/desorption experiment
of He 8 Member tight sandstone.

Specific Surface Pore Volume

Sample AM Pore Width (nm) Hysteresis
Area (m2 /g) (×10–3 cm3 /g) Classfication
ID (cm3 /g) Loop Type
SBET SBJH V BJH V SF WT W BJH_ave W BJH_med W SF_med
SU-1 1.950 0.597 1.014 3.291 0.250 20.212 12.983 2.040 1.835 C H3
SU-2 2.100 0.548 0.944 3.503 0.247 23.726 14.840 2.035 1.967 C H3
SU-3 2.166 0.530 0.925 3.593 0.220 25.271 15.547 3.509 1.728 C H3
SU-4 2.217 0.594 1.044 3.725 0.334 23.104 14.271 2.801 1.718 C H3
SU-6 3.148 0.697 1.124 5.167 0.288 27.931 18.379 2.814 1.727 B H1
SU-7 3.652 0.683 1.188 5.987 0.326 33.094 20.151 2.033 1.728 B H1
SU-9 4.512 2.012 1.932 7.043 0.746 13.877 14.583 3.976 1.108 B H2
SU-10 5.279 3.162 2.862 8.147 1.198 10.329 11.387 2.099 1.067 B H2
SU-13 8.261 3.038 3.858 13.379 1.055 16.823 13.872 2.819 1.071 A H2
SU-14 8.266 1.112 1.519 13.198 0.518 45.989 34.762 2.062 1.728 A H1
SU-15 8.831 3.772 4.368 13.404 1.272 13.686 12.275 2.498 1.104 A H2
Note: AM –N2 Maximal absorbed amount; SBET —BET SSA; SBJH —BJH Adsorption cumulative SSA; V BJH —BJH
Adsorption cumulative PV; V SF —SF Micropore PV; W T —Total adsorption average pore width; W BJH_ave —BJH
Adsorption average pore width; W BJH_med —BJH Adsorption median pore width; W SF_med —SF Median pore width;
A—Class A; B—Class B; C—Class C.
Minerals 2020, 10, 377 9 of 21
Minerals 2020, 10, x FOR PEER REVIEW 9 of 22

Figure 6. Univariate linear regression analysis of pore structure parameters: (a) Relationship between
VFigure
BJH and SBET ; (b) relationship
6. Univariate between
linear regression analysis V BJH SBJH ; (c)parameters:.(a)
andstructure
of pore relationship between V SF between
Relationship and SBET ;
(d) relationship
VBJH and SBET; between V SF andbetween
(b) relationship SBJH ; (e) V
relationship between V BJH and between
BJH and SBJH; (c) relationship
AM ; (f) relationship
VSF and SBETbetween
; (d)
Vrelationship
SF , and AM .between VSF and SBJH; (e) relationship between VBJH and AM; (f) relationship between VSF,
and AM.
A further discussion of the contribution rate (V r ) among five different size ranges pores to the total
SBJH and total Vdiscussion
A further BJH is conducted from the experimental
of the contribution result
rate (Vr) among as different
five showingsize in Figure
ranges7.pores
The average
to the
Vtotal
r of micropore (<2 nm), type I mesopores (mesopore-I: 2–10 nm), type II mesopores (mesopore-II:
SBJH and total VBJH is conducted from the experimental result as showing in Figure 7. The average
10–50
Vr of nm), type I (<2
micropore macropores
nm), type(macropore-I:
I mesopores50–100 nm) and
(mesopore-I: type
2–10 II macropores
nm), (macropore-I:
type II mesopores >100 nm)
(mesopore-II:
to10–50
the total V are 0.48%, 23.21%, 37.14%, 17.63% respectively (Figure 7a). The average
BJH I macropores (macropore-I: 50–100 nm) and type II macropores (macropore-I: ＞100
nm), type contribution
rate
nm)oftomicropore,
the total Vmesopore-I,
BJH are 0.48%,mesopore-II, macropore-I
23.21%, 37.14%, 17.63%and macropore-II
respectively to the
(Figure TheSBJH
7a).total (Sr ) is
average
3.05%, 72.65%,rate
contribution 20.08%, 3.21%, and
of micropore, 1.00%, respectively
mesopore-I, (Figure
mesopore-II, 7b). To summarize,
macropore-I BJH volume
and macropore-II to the mainly
total
hinges
SBJH (Son
r) isthe number
3.05%, of mesopore-II
72.65%, (37.14%),
20.08%, 3.21%, and followed by the mesopore-II
1.00%, respectively (23.21%)
(Figure 7b). and macropore-II
To summarize, BJH
(21.54%). The pore
volume mainly typeon
hinges with
the the largest
number of contribution rate for the
mesopore-II (37.14%), total SSA
followed is also
by the mesopores,
mesopore-II with an
(23.21%)
average value of 92.73%
and macropore-II (mesopore-I:
(21.54%). 76.25%,
The pore type withmesopore-II: 20.08%).
the largest contribution rate for the total SSA is also
mesopores, with an average value of 92.73% (mesopore-I: 76.25%, mesopore-II: 20.08%).
Minerals 2020, 10, x FOR PEER REVIEW 10 of 22
Minerals 2020, 10, 377 10 of 21
Minerals 2020, 10, x FOR PEER REVIEW 10 of 22

Figure 7. The contribution rate of V and S in five different size ranges pores. (a) Pore volume
Figure 7. The contribution rate of VBJHBJH and SBJH BJH
in five different size ranges pores. (a) Pore volume (PV)
(PV) contribution rate of five different size classes pores; (b) specific surface area (SSA) contribution
contribution
Figure 7. The rate of five different
contribution Vsize
rate ofpores. classes pores; (b) specific surface area (SSA) contribution rate
BJH and SBJH in five different size ranges pores. (a) Pore volume (PV)
rate of five different size classes
of five different
contribution ratesize classes
of five pores. size classes pores; (b) specific surface area (SSA) contribution rate
different
As illustrated
of five different in
sizeFigure
classes8,pores.
the plot of PSD of different Hysteresis loop types tight sandstone is
As illustrated in Figure 8, the plot of PSD of different Hysteresis loop types tight sandstone is
showing a different characteristic. H1 type loops are dominated by mesopore-II (averages at 30.11%)
showing a differentin
As illustrated characteristic.
Figure 8, theH1 type
plot loopsofare
of one
PSD dominated
different by mesopore-II
Hysteresis loop (averages at 30.11%)
and mesopore-I (averages at 23.05%), with major pore size peak range of types
2~50nm tight sandstone
(Figure is
8a1,b1).
and mesopore-I
showing a (averages
different at 23.05%),
characteristic. H1 with
type one major
loops are pore size peak
dominated by range of 2~50nm
mesopore-II (Figure
(averages at 8a1 and
30.11%)
The H2 type loop is mainly controlled by the macropore-II (averages at 52.11%) and mesopore-II
8b1). The H2 type
and mesopore-I loop is mainly
(averages controlled
at 23.05%), withsizeby major
one the macropore-II
poreofsize (averages
peak range at 2~50nm
of 52.11%) (Figure
and mesopore-
(averages at 20.57%), with two main pore peak range 10~50nm and 100~200nm (Figure8a1 and
8a2,b2).
II (averages
8b1). The H2 at 20.57%),
type loop iswith
mainlytwo main pore
controlled bysize
the peak range
macropore-II of 10~50nm
(averages at and 100~200nm
52.11%) and (Figure
mesopore-
In addition, the predominant pore size range of H3 type is mesopore –II (averages at 41.32%), which
8a2,b2). In addition,
II (averages the predominant
at 20.57%), with8a3,b3).
two mainporepore
size size
range of H3
peak typeof
range is mesopore
10~50nm and–II (averages
100~200nm at 41.32%),
(Figure
varies from 10–50nm (Figure
which varies from 10–50nm (Figure 8a3,b3).
8a2,b2). In addition, the predominant pore size range of H3 type is mesopore –II (averages at 41.32%),
which varies from 10–50nm (Figure 8a3,b3).

Figure 8. Representative pore size of different hysteresis loop types tight sandstone: (a1)–(a3) dV/dW
Figure 8. Representative pore size of different hysteresis loop types tight sandstone: (a1)–(a3) dV/dW
vs. PW, (b1)–(b3) Incremental V BJH vs. PW.
vs. PW,8.(b1)–(b3)
Figure Incremental
Representative pore size vs.different
VBJH of PW. hysteresis loop types tight sandstone: (a1)–(a3) dV/dW
3.4. The Fractal
vs. PW, Characteristics
(b1)–(b3) Incremental of Nanoscale
VBJH vs. PW.Pores
3.4. The Fractal Characteristics of Nanoscale Pores
In this study, different piecewise linear fitting methods were used by selecting five different
3.4. The Fractal
In this Characteristics
study, different of Nanoscale
piecewise Poresfitting methods were used by selecting five different
linear
relative pressure (P/P 0 ) cutoff value, the ln(V) vs. ln[ln(P0 /P)] curves could be separated into two or
relative
threeIn pressure
this
segments. study,(P/P
The 0) cutoff
different
fractal value,
piecewise
fitting thelinear
curves ln(V)
of vs.typical
ln[ln(P
fitting
three 0/P)] curves
methods
samples were couldby
used
are illustratedbeselecting
separated 9,into
in Figurefive twothe
or
different
where
three
relative
slope segments.
(k)pressure The
was used(P/P fractal fitting
0) cutoff value,
to calculate curves
fractalthe of three
ln(V) vs.value
dimension typical
ln[ln(P samples
(D0/P)] are
curves could
N ) according
illustrated in
be separated
to Equation Figure
into
(1) and 9, where
two or
Equation
the
three
(2), slope
using (k) was
segments. The
calculated used
root to
fractal calculate
fitting
mean fractal
curves
square dimension
of (R
error three showvalue
2 ) totypical samples
the (DN)are
fitting according As to
illustrated
degree. Equation
in Figurein9,(1)
presented and
where
Table 3,
Equation
the
D N slope (2),
calculated(k) using
was
by allcalculated
used
four to
methods root
calculate mean
exhibit square
fractal
good error
dimension
fitting (R
with
2 ) to
value
R 2show(D
valuesthe
N) fitting
according
that are degree.
to
mostly As presented
Equation
higher (1)
than in
and
0.97,
Table
Equation
and the3, calculated
D(2),
N calculated
usingresults by all
calculatedarefourrootmethods
shown mean exhibit
square
in Table 4. errorgood
(R2fitting
) to showwiththeR2fitting
valuesdegree.
that areAs mostly higher
presented in
than
TableIn0.97, Dand
3,the Nfirstthe calculated
calculated
method, bythe results
allunsegmented
four are shown
methods in Table
exhibit
method 4.
goodutilized
was fitting with R2 values
to calculate DN0that are mostly
, which higher
can represent
the In theand
0.97, firstthe
thanheterogeneity method,
calculated
of the unsegmented
the whole results method
are shown
nanoscale pores. inThewas
Table utilized
DN0 4. valuestorange
calculate
fromD2.360
N0, which can represent
to 2.592, averages
the heterogeneity
In the
at 2.446, of the
first method,
which showingthe whole nanoscale
anunsegmented pores.
methodin
ideal fractal feature The D
was values
theutilized
N0 range
nanoscale from
to calculate 2.360 to
DN0, which
pore structure 2.592, averages
can
of He 8represent
Member at
2.446, which showing
the heterogeneity
tight sandstone. of the anwhole
ideal nanoscale
fractal feature
pores.inThe
the Dnanoscale
N0 values porerangestructure
from 2.360 of toHe2.592,
8 Member
averages tight
at
sandstone.
2.446, which showing an ideal fractal feature in the nanoscale pore structure of He 8 Member tight
sandstone.
Minerals 2020, 10, 377 11 of 21

Trichotomy was used in the second method. Three distinct fitting liner segments are obtained
at different relative pressure corresponds to different BJH pore width (W) range respectively. The
DN1 ranges from 2.500 to 2.707 (averaging at 2.597), which is the value correspond to the pore
microstructures complexity of pore size lager than 10 nm, while DN2 is the representative value of
pore structure heterogeneous features with PW range from 2 nm~10 nm, which is varied from 2.168 to
2.539 (averaging at 2.314). Correspondingly, DN3 value represents the heterogeneity characteristic of
micropores (W < 2 nm), ranges from 2.215 to 2.600 with an average of 2.382. The results show that the
heterogeneity of macropores and micropores is generally stronger than that of mesopores.
The dichotomy was used to separate the ln(V) vs. ln[ln(P0 /P)] plot into two segments with relative
pressure point corresponds to the BJH W = 5 nm as the cutoff value, which can fit two straight line
separately and obtained DN4 (Pore size: W > 5 nm) and DN5 (Pore size: W ≤ 5 nm) severally. DN4
values range from 2.481 to 2.660 with an average of 2.566. DN5 values range from 2.063 to 2.191,
averaging at 2.259, which is smaller than DN4 .
In the fourth method, selecting a cutoff value based on the inflection point of N2 -GA isotherms
curve, divided into three the following areas: Region 1: P/P0 > 0.8; Region 2: 0.5 < P/P0 ≤ 0.8; Region 3:
P/P0 ≤ 0.5, where DN6 values ranges from 2.507 to 2.707, with an average of 2.602. DN7 values range
from 2.300 to 2.598, averaging at 2.417, which is lower than DN6 . DN8 values range from 2.058 to 2.494,
averaging at 2.261, which is smaller than DN7 .
 Minerals
Minerals 10, x10,
2020,2020, FOR377PEER REVIEW 12 of 22 12 of 21

Figure 9. Representative plots of ln(V) vs. ln[ln(P0 /P)] reconstructed from the N2 adsorption analysis of different class tight sandstone samples.
Figure 9. Representative plots of ln(V) vs. ln[ln(P0/P)] reconstructed from the N2 adsorption analysis of different class tight sandstone samples.
Minerals 2020, 10, 377 13 of 21

Table 3. Slop (k) and root mean square error (R2 ) obtained from the plot of ln(V) vs. ln[(P0 /P)].

Region: 0.01 < Pore size: Pore size: Pore size: Pore size: Pore size: Region 1: Region 2: 0.5 < Region 3: P/P0
Sample ID P/P0 ≤ 0.99 W > 10nm 2 nm < W ≤ 10 nm W < 2nm W > 5nm W ≤ 5nm P/P0 > 0.8 P/P0 ≤ 0.8 ≤ 0.5
k0 R0 2 k1 R1 2 k2 R2 2 k3 R3 2 k4 R4 2 k5 R5 2 k6 R6 2 k7 R7 2 k8 R8 2
SU-1 –0.624 0.959 –0.408 0.999 –0.805 0.989 –0.625 0.928 –0.448 0.992 –0.893 0.982 –0.408 0.999 –0.658 0.994 –0.888 0.978
SU-2 –0.616 0.971 –0.441 0.996 –0.791 0.992 –0.687 0.979 –0.473 0.993 –0.844 0.992 –0.432 0.996 –0.628 0.992 –0.844 0.990
SU-3 –0.618 0.965 –0.425 0.990 –0.803 0.991 –0.741 0.969 –0.464 0.991 –0.895 0.993 –0.425 0.990 –0.656 0.998 –0.892 0.991
SU-4 –0.640 0.965 –0.420 0.999 –0.832 0.993 –0.511 0.972 –0.469 0.990 –0.860 0.980 –0.420 0.999 –0.700 0.996 –0.851 0.975
SU-6 –0.591 0.962 –0.431 0.994 –0.807 0.994 –0.762 0.971 –0.445 0.995 –0.895 0.994 –0.435 0.993 –0.689 0.997 –0.897 0.993
SU-8 –0.614 0.965 –0.467 0.985 –0.793 0.990 –0.786 0.962 –0.472 0.993 –0.937 0.991 –0.467 0.985 –0.643 0.996 –0.942 0.989
SU-9 –0.456 0.995 –0.391 0.991 –0.487 1.000 –0.527 1.000 –0.415 0.993 –0.506 0.998 –0.380 0.991 –0.473 0.999 –0.506 0.997
SU-10 –0.408 0.982 –0.316 0.978 –0.461 0.995 –0.525 0.973 –0.340 0.986 –0.525 0.996 –0.305 0.974 –0.402 1.000 –0.528 0.996
SU-13 –0.483 0.972 –0.335 0.985 –0.602 0.993 –0.566 0.992 –0.379 0.958 –0.611 0.997 –0.318 0.929 –0.505 0.999 –0.610 0.996
SU-14 –0.548 0.994 –0.500 0.977 –0.627 0.999 –0.400 0.949 –0.519 0.987 –0.538 0.980 –0.493 0.972 –0.583 1.000 –0.524 0.978
SU-15 –0.498 0.963 –0.293 0.931 –0.542 0.994 –0.669 0.970 –0.347 0.959 –0.651 0.993 –0.293 0.931 –0.471 1.000 –0.651 0.993
Minimum –0.640 0.959 –0.500 0.931 –0.832 0.989 –0.786 0.928 –0.519 0.958 –0.937 0.980 –0.493 0.929 –0.700 0.992 –0.942 0.975
Maximum –0.408 0.995 –0.293 0.999 –0.461 1.000 –0.400 1.000 –0.340 0.995 –0.506 0.998 –0.293 0.999 –0.402 1.000 –0.506 0.997
Average –0.554 0.972 –0.403 0.984 –0.686 0.994 –0.618 0.970 –0.434 0.985 –0.741 0.990 –0.398 0.978 –0.583 0.997 –0.739 0.989
Minerals 2020, 10, 377 14 of 21

Table 4. Fractal dimensions from N2 adsorption data of different class He 8 Member tight
sandstone samples.
Minerals 2020, 10, x FOR PEER REVIEW 14 of 22
Sample Hysteresis
DN0 DN1 DN2 DN3 DN4 DN5 DN6 DN7 DN8
ID Loop Types
Table
SU-1 4. FractalH3
dimensions
2.376 2 adsorption data of different class He 8 Member tight sandstone
from N2.592 2.195 2.375 2.552 2.107 2.592 2.342 2.112
samples.
SU-2 H3 2.384 2.559 2.209 2.313 2.527 2.156 2.568 2.372 2.156
Sample
SU-3 Hysteresis
H3 2.382 2.575 2.197 2.259 2.536 2.105 2.575 2.344 2.108
DN02.360 D2.580 D DN3 DN4 DN5 DN6 2.300DN7 2.150DN8
ID SU-4 Loop Types
H3 2.168 2.490 2.531 2.140 2.580
N1 N2

SU-1SU-6 H3 H1 2.409
2.376 2.569
2.592 2.193
2.195 2.238
2.375 2.555
2.552 2.105
2.107 2.565
2.592 2.311
2.342 2.1032.112
SU-2SU-7 H3 H1 2.386
2.384 2.533
2.559 2.207
2.209 2.215
2.313 2.528
2.527 2.063
2.156 2.533
2.568 2.357
2.372 2.0582.156
SU-14
SU-3 H3 H1 2.452
2.382 2.500
2.575 2.374
2.197 2.600
2.259 2.481
2.536 2.462
2.105 2.507
2.575 2.417
2.344 2.4762.108
SU-4SU-9 H3 H2 2.360
2.544 2.580
2.609 2.168
2.513 2.490
2.473 2.531
2.585 2.140
2.494 2.580
2.620 2.300 2.4942.150
2.527
SU-6
SU-10 H1 H2 2.409
2.592 2.569
2.685 2.193
2.539 2.238
2.475 2.555
2.660 2.105
2.475 2.565
2.695 2.311 2.4722.103
2.598
SU-7 H1 2.386 2.533 2.207 2.215 2.528 2.063 2.533 2.357
SU-13 H2 2.517 2.665 2.398 2.434 2.621 2.389 2.682 2.496 2.3902.058
SU-14 H1 2.452 2.500 2.374 2.600 2.481 2.462 2.507 2.417 2.476
SU-15 H2 2.502 2.707 2.458 2.331 2.653 2.349 2.707 2.529 2.349
SU-9 H2 2.544 2.609 2.513 2.473 2.585 2.494 2.620 2.527 2.494
SU-10 H2
Minimum 2.592
2.360 2.685
2.500 2.539
2.168 2.475
2.215 2.660
2.481 2.475 2.507
2.063 2.695 2.300
2.598 2.0582.472
SU-13 H2
Maximum 2.517
2.592 2.665
2.707 2.398
2.539 2.434
2.600 2.621
2.660 2.389 2.707
2.494 2.682 2.598
2.496 2.4942.390
SU-15 H2 2.502 2.707 2.458 2.331 2.653 2.349 2.707 2.529
Average 2.446 2.597 2.314 2.382 2.566 2.259 2.602 2.417 2.2612.349
Minimum 2.360 2.500 2.168 2.215 2.481 2.063 2.507 2.300 2.058
Maximum 2.592 2.707 2.539 2.600 2.660 2.494 2.707 2.598 2.494
4. Average
Discussion 2.446 2.597 2.314 2.382 2.566 2.259 2.602 2.417 2.261

4. Discussion
4.1. Effect of Mineral Composition on Fractal Dimensions
The heterogeneous
4.1. Effect distribution
of Mineral Composition of mineral
on Fractal particles constitutes a diversiform pore-throat system.
Dimensions
FE-SEM images show that pore types of all tight sandstone samples consist of different mineral
The heterogeneous distribution of mineral particles constitutes a diversiform pore-throat system.
edge FE-SEM
can be classified
images show into four
that types:
pore types original intergranular
of all tight pore consist
sandstone samples (Figureof10a), secondary
different mineral dissolved
edge
intragranular pore (Figure 10b), intercrystalline micropores of clay minerals (Figure
can be classified into four types: original intergranular pore (Figure 10a), secondary dissolved 10c–f), and
microfissure (Figure
intragranular 10a).
pore (Figure 10b), intercrystalline micropores of clay minerals (Figure 10c–f), and
microfissure (Figure 10a).

Figure 10. 10.Field

Figure emissionscanning
Field emission scanning electron
electron microscopy
microscopy (FE-SEM) (FE-SEM) images pore
images of different of different
types. (a) pore
types.Intergranular pores; pores;
(a) Intergranular (b) intragranular pores; (c)
(b) intragranular intercrystalline
pores; micropores
(c) intercrystalline of chlorite;
micropores (d)
of chlorite;
intercrystalline micropores
(d) intercrystalline micropores ofof kaolinite;
kaolinite;(e)
(e)intercrystalline
intercrystallinemicropores of illite;
micropores (f) intercrystalline
of illite; (f) intercrystalline
micropores of illite/smectite.
micropores of illite/smectite.
Minerals 2020, 10, 377 15 of 21
Minerals 2020, 10, x FOR PEER REVIEW 15 of 22

Quartz is
Quartz is the
the highest
highest mineral composition
compositionin inall
alltight
tightsandstone
sandstonesamples
samplesaccording
according toto
the X-RD
the X-RD
results(Table
results (Table11and andFigure
Figure3)3)and
andFE-SEM
FE-SEMimagesimages(Figure
(Figure10a).
10a). Therefore,
Therefore, itit isisextremely
extremely important
important to
to point
point outout
thethe relationship
relationship betweenquartz
between quartzand
andDDNN.. The result
result shows
showsthat thatquartz
quartzcontent
contentis is
showing
showing
aagood
goodnegative
negative correlation
correlation with all types of fractal dimensions
dimensions respectively,
respectively, which
whichDDN0N0and andDD N2
N2
showingthe
showing the best
best correlation
correlation with
with quartz
quartzcontent
content(Figure
(Figure11a,b),
11a,b),with
withcorrelation
correlation coefficients
coefficientsof of
0.751
0.751
and 0.748.
and 0.748. AA higher
higher quartz
quartz content
contentindicates
indicatesthe
thepore-throat
pore-throatsystem
systemtendtendtotobebesimpler,
simpler,which
which is is
contrary to the relationship between total clay mineral content and D N (Figure 11c,d), with a positive
contrary to the relationship between total clay mineral content and DN (Figure 11c,d), with a positive
correlationcoefficient
correlation coefficientof of0.865
0.865(D(DN0)) and 0.809 (DN7). This is associated with the extensive distribution
N0 and 0.809 (DN7 ). This is associated with the extensive distribution
of clay minerals and its complex composition,which
of clay minerals and its complex composition, whichprovides
providesaalarge
largeamount
amountofofnano-scale
nano-scale storage
storage
space for the occurrence of tight gas and makes the pore-throat system more
space for the occurrence of tight gas and makes the pore-throat system more complex at the same complex at the sametime.
time.

Figure 11. The effect of mineral content on fractal dimensions. (a) The relationship between quartz
content andThe
Figure 11. DN0effect
; (b) the relationship
of mineral between
content quartz
on fractal content and
dimensions. DN2relationship
(a) The ; (c) the relationship between
between quartz
total clay content and D ; (d) the relationship between total clay content and D
content and DN0; (b) the relationship between quartz content and DN2; (c) the relationship between
N0 N7 ; (e) the relationship
between
total clayillite/smectite
content and D and illite
N0; (d) with
the DN7 ; (f) the
relationship relationship
between between
total clay chlorite
content and DN7 and
; (e)kaolinite with DN7 .
the relationship
between illite/smectite and illite with DN7; (f) the relationship between chlorite and kaolinite with DN7.
In addition, the intercrystalline micropores of chlorite and kaolinite has a smaller SSA than that is
in illite/smectite
In addition,and
theillite because it has
intercrystalline a smoother
micropores edge. Itand
of chlorite alsokaolinite
makes the
hasillite and illite/smectite
a smaller SSA than that has
good positive correlation
is in illite/smectite with
and illite fractalitdimensions
because DN7 edge.
has a smoother (Figure 11e,f),
It also where
makes thethe phenomenon
illite of mixed
and illite/smectite
layer mineral
has good is more
positive obvious.with fractal dimensions DN7 (Figure 11e,f), where the phenomenon of
correlation
mixed layer mineral is more obvious.
Minerals 2020, 10, 377 16 of 21

4.2. Effect of2020,

Minerals Pore10,Size Distribution
x FOR PEER REVIEWon Fractal Dimensions 16 of 22

Pore-throat system is a crucial storage space of tight sandstone gas as well as significant flowing
4.2. Effect of Pore Size Distribution on Fractal Dimensions
channel for natural gas during the entire development process. This means that mineral composition
Pore-throat
has a significant system is
influence ona crucial
SSA, PV, storage
andspace of tight sandstone
DN , respectively. As gas as well
shown in as significant
Figure 12a, flowing
all the tight
channel for natural gas during the entire development process. This means that mineral composition
sandstone samples are arranged in the order of the clay mineral content increasing; the total SBET also
has a significant influence on SSA, PV, and DN, respectively. As shown in Figure 12a, all the tight
has an increasing trend identified. Furthermore, SBET has an excellent positive relationship with all
sandstone samples are arranged in the order of the clay mineral content increasing; the total SBET also
typeshas
of fractal dimensions
an increasing (P-value <
trend identified. Furthermore, of D
0.01, exceptSBET N5an
has and DN8 ), positive
excellent where the correlation
relationship with
with all DN7
(R2 =types
0.783), D (R
of fractal
2 = 0.794) and D
N4 dimensions (P-value (R 2 = 0.783) is more obvious. Similarly, as the increasing of clay
N2< 0.01, except of DN5 and DN8), where the correlation with DN7 (R2
mineral content, PV also has an increasing
= 0.783), DN4 (R = 0.794) and DN2 (R2 = 0.783)
2 tendency
is more(Figure 12b).Similarly,
obvious. Moreover, the increasing
as the relationship between
of clay
DN and SF micropores
mineral content, PV alsovolume
has anisincreasing
significant (P-value
tendency < 0.01,
(Figure 12b).except
Moreover,of Dthe DN8 , and D
N5 ,relationship N3 ), with a
between
DN correlation
positive and SF micropores volume
coefficient is significant
of 0.844 (DN7 ) and(P-value
0.794 (D< N0
0.01, except ofitD
), whereas , DN8
isN5not , and DN3),between
significant with a the
positive of
relationship correlation
DN and coefficient
V BJH , withof a0.844 (DN7) correlation
positive and 0.794 (Dcoefficient
N0), whereasofit is not significant
0.416 (DN7 ) andbetween
0.406 (D the
N0 ).
relationship of DN and VBJH, with a positive correlation coefficient of 0.416 (DN7) and 0.406 (DN0).

FigureFigure 12. The

12. The relationshipbetween
relationship between pore
pore structure
structureparameter
parameterandand
Fractal dimensions
Fractal in the order
dimensions in theoforder
clay mineral content increasing. (a) The relationship between SBET and fractal dimensions; (b) the
of clay mineral content increasing. (a) The relationship between SBET and fractal dimensions; (b) the
relationship between PV and fractal dimensions.
relationship between PV and fractal dimensions.
Moreover, the relationship between the SSA contribution rate (Sr) of different pore size range
Moreover, the relationship between the SSA contribution rate (Sr ) of different pore size range with
with fractal dimensions shows the different characters. Thereinto, the mesopore-II has an excellent
fractal dimensions shows the different characters. Thereinto, the mesopore-II has an excellent positive
relationship with DN8 (R 2 = 0.746,P-vuale < 0.01) (Figure 13a), whereas macropore-II has a negative
Minerals 2020, 10, x FOR PEER REVIEW 17 of 22

positive
Minerals
Minerals relationship
2020,
2020, 10,377
10, withREVIEW
x FOR PEER DN8 (R 2= 0.746,P-vuale < 0.01) (Figure 13a), whereas macropore-II1717 has a
ofof2221
negative correlation with DN1 (R2 = 0.730,P-vuale < 0.01) (Figure 13b), this result shows that where
positive
there is a relationship
smaller Sr ofwith DN8 (R 2= and
mesopore-II 0.746,P-vuale
a lager Sr< of
0.01) (Figure 13a),there
macropore-II, whereas
is a macropore-II has a
simpler pore-throat
correlation
negative with D
correlation
structure, such as SU-14.N1 (R 2
with =D0.730,P-vuale
N1 (R < 0.01)
2 = 0.730,P-vuale (Figure
< 0.01) 13b), this
(Figure result
13b), thisshows
result that
showswhere
that there
where is
a there
smalleris aSrsmaller
of mesopore-II and a lager
Sr of mesopore-II andSraoflager
macropore-II, there is athere
Sr of macropore-II, simpler
is apore-throat structure,
simpler pore-throat
structure,
such as SU-14.such as SU-14.

Figure 13. The relationship between Sr and DN. (a) The relationship between Sr of mesopore-II and
Figure
D theThe
N8; (b)13. relationship
relationship between Sr ofSrmacropore-II
between and DN . (a) The
and relationship
DN1. between Sr of mesopore-II and
Figure 13. The relationship between Sr and DN. (a) The relationship between Sr of mesopore-II and
DN8 ; (b) the relationship between Sr of macropore-II and DN1 .
DN8; (b) the relationship between Sr of macropore-II and DN1.
4.3. Compective Study of Fractal Dimensions
4.3. Compective Study of Fractal Dimensions
4.3.As
Compective
illustratedStudy of Fractal
in Figure Dimensions
9 and Figure 14, the unsegmented and segmented linear fitting methods
As illustrated in Figures 9 and 14, the unsegmented and segmented linear fitting methods both
both are effective
As illustrated way to obtain
andthe fractal curves based onand N2-GA isotherms curve, which can
are effective way to in Figure
obtain the9 fractal
Figure
curves14,based
the unsegmented
on N2 -GA isothermssegmented
curve,linear
which fitting methods
can accurately
accurately
both are therepresent
effective the fractal characteristic of the different pore size range separately and indicate
represent fractalway to obtain the
characteristic fractal
of the curves
different based
pore sizeon N2-GA
range isotherms
separately andcurve, which
indicate thatcan
the
that the distribution
accurately represent of fractal
the the pore throat inof He
characteristic the 8 Member
different poretight
size sandstone
range has and
separately multi-fractal
indicate
distribution of the pore throat in He 8 Member tight sandstone has multi-fractal characteristic. All types
characteristic. All types of offractal dimensions showing 8 an increasing trend as the clayhasmineral content
ofthat thedimensions
fractal distributionshowing theanpore throattrend
increasing in Heas the Member
clay tight
mineral sandstone
content increasing, multi-fractal
which indicate
increasing, whichAllindicate of afractal
good dimensions
relationshipshowing
betweenanmineral composition with
clayDmineral
n. Thereinto, the
a characteristic.
good relationship types
between mineral composition with D increasing trend as the content
n . Thereinto, the value of DN0 is the closest to
value of DN0 is
increasing, the closest
which indicate toathegoodaverage and thebetween
relationship DN2 hasmineral
the bestcomposition
relationship with
with Dthe. average
Thereinto, value
the
the2 average and the DN2 has the best relationship with the average value (R2 = 0.954).
n

(Rvalue
= 0.954).
of DN0 is the closest to the average and the DN2 has the best relationship with the average value
Furthermore, as listed in Table 4, the fractal dimensions always appear the highest average
(R2 Furthermore,
= 0.954). as listed in Table 4, the fractal dimensions always appear the highest average value
value in tight sandstone sample with H2 type hysteresis loops no matter what methods were used,
in tight sandstone as
Furthermore, sample
listed in with
TableH24, the
typefractal
hysteresis loopsalways
dimensions no matter
appear what methods
the highest werevalue
average used,
indicating that pore structure heterogeneity is mainly controlled by the inkbottle-shaped pores and the
indicating that pore structure
in tight sandstone sample with heterogeneity is mainly controlled
H2 type hysteresis by the what
loops no matter inkbottle-shaped
methods were pores and
used,
V r of mesopore.
indicating
the that pore structure heterogeneity is mainly controlled by the inkbottle-shaped pores and
Vr of mesopore.
the Vr of mesopore.

Figure 14. The trends of fractal dimension among different tight sandstone samples.
Figure
Figure14.
14.The
Thetrends
trendsof
offractal
fractaldimension
dimension among
among different tight sandstone
different tight sandstonesamples.
samples.
Minerals 2020, 10, 377 18 of 21

Minerals 2020, 10, x FOR PEER REVIEW 18 of 22

Among different types of fractal dimensions, the overall distribution of DN0 , DN1 , DN4 , and DN6
Among
is more differentwhereas
concentrated, types of thefractal dimensions,
whole distribution theofoverall
DN2 , Ddistribution
N3 , DN5 , DN7ofand DN0D,D ,D
N8N1is N4, and
more DN6 is
scattered
more concentrated, whereas the whole distribution of D , D , D , D
(Figure 15). This is relevant to the heterogeneity of pore structure and mineral composition, which
N2 N3 N5 N7 and D N8 is more scattered
(Figure
expanded 15). This
the is relevant
range of fractalto the heterogeneity
dimension values, inof porewords,
other structure and mineral
this type of fractalcomposition,
dimensions iswhichmore
expanded
sensitive tothe rangespecific
certain of fractal dimension
property. values, in
Correlation other words,
analysis this type
results show thatof fractal
expect ofdimensions
DN3 showing is
a weak relationship with chlorite content (R = 0.252), which present the best correlation among all
more sensitive to certain specific property. 2 Correlation analysis results show that expect of D N3

showing
types of DaNweak relationship
, all the “scattered”with chlorite
fractal contentis(R
dimensions 2 = 0.252), which present the best correlation
bound up with mineral content to some extent,
among all types of D , all the “scattered” fractal
while “concentrated” fractal dimensions is much weaker except
N dimensions is bound
of DN0up . Inwith mineral
addition, DN5content to
and DN8
some extent, while “concentrated” fractal dimensions is much weaker except of
merely present a good relationship with mineral content (especially in quartz content and illite/smectite D N0 . In addition, D N5

and DN8 merely

content) (Figurespresent
11 anda 14)good and relationship with mineral
Sr of mesopore-II, whichcontent (especially
is optimum in quartz
parameter content and
to represent the
illite/smectite content) (Figures 11 and 14) and S of mesopore-II,
complexity of mineral composition and its corresponding micropore shape.
r which is optimum parameter to
represent the complexity of mineral composition and its corresponding micropore shape.

Figure 15. Different types of fractal dimension numerical distribution range in different tight sandstone.
Figure 15. Different types of fractal dimension numerical distribution range in different tight
5. Conclusions
sandstone.

In this paper, nine types fractal dimension were obtained using different piecewise linear fitting
5. Conclusions
methods by selecting five different relative pressure (P/P0 ), and we put forward the concept of
In this paper,
“concentrated” ninedimensions
fractal types fractaland dimension
“scattered”werefractal
obtained using different
dimensions for thepiecewise linear fitting
first time according to
methods by selecting five different relative pressure (P/P ), and we put
its concentration extent of distribute in different samples. Moreover, three types of hysteresis loops
0 forward the concept of
“concentrated”
were distinguished fractal dimensions
that correspond andto “scattered”
different pore fractal
shape dimensions
combination for and
the first time according
the impact of mineralto
its concentration
composition extent
and pore of distribute
structure in different
on different fractalsamples.
dimensions Moreover, three types
were discussed of hysteresis
in detail. loops
These findings
were distinguished
can provide that correspond
new insights to different
for quantitative evaluationporetheshape combination
microscopic and the impact
heterogeneity of tightof mineral
sandstone
composition and pore
reservoir at various porestructure on different
size classes and further fractal
revealdimensions
the controlling were effect
discussed
of porein heterogeneity
detail. These
findings
on natural cangas
provide
storage new
andinsights for quantitative
desorption, which is of evaluation
great significancethe microscopic
for improvingheterogeneity of tight
the exploitation
sandstone
efficiency ofreservoir at various
tight sandstone gas.pore size classes
The main and further
conclusions are summarizedreveal theascontrolling
follows: effect of pore
heterogeneity
(1) Among onall
natural
types gas storage
of fractal and desorption,
dimensions, which is of
DN0 represent great
the significanceoffor
heterogeneity improving
whole the
nanoscale
exploitation efficiency of tight sandstone gas. The main conclusions are summarized
pore, with the ranges of 2.360 to 2.592, averaging at 2.446, which show an ideal fractal feature of the as follows:
(1) Among
nanoscale all typesofoftight
pore structure fractal dimensions,
sandstone in He D 8 N0 represent
Member. the heterogeneity
Meanwhile, the value of of whole
DN0 is the nanoscale
closest
pore,
to thewith the ranges
average while theof 2.360
DN2 hasto 2.592,
the bestaveraging at 2.446,
relationship withwhich show an
the average ideal
value = 0.954).
(R2fractal feature of the
nanoscale
(2) Thepore structurefractal
“scattered” of tightdimensions
sandstone (D in He
N2 , 8
DMember.
N3 , DN5 , D Meanwhile,
N7 ) are more thesensitive
value ofto DN0 is thespecific
certain closest
to the average
property of thewhile the Dincluding
reservoir, N2 has the best relationship
mineral with the average
content (especially value
in quartz (R = 0.954).
content2
and illite/smectite
(2) The
content) and “scattered” fractal dimensions
the Sr of mesopore-II (10–50 nm), (Dwhere
N2, DN3 D, N5
DN5and
, DN7 D)N8arearemore sensitive
optimum to certain
parameter specific
to represent
property of the of
the complexity reservoir,
mineral including
composition mineral
and its content (especially
corresponding in quartzshape.
micropore content and illite/smectite
content) and the Sr of mesopore-II (10–50 nm), where DN5 and DN8 are optimum parameter to
represent the complexity of mineral composition and its corresponding micropore shape.
Minerals 2020, 10, 377 19 of 21

(3) H1 type loop indicated the combination of cylindrical pores and parallel plate shaped
pores; H2 type loop related to the combination of inkbottle-shaped pores and cylindrical pores,
with bowl-shaped pores as a transitional form in the mesopores; H3 type loop is associated with
the combination of slit-/wedge-shaped pores and parallel plate shaped pores. Furthermore, the
heterogeneity of pore structure in this study area is predominantly controlled by inkbottle-shaped
pores and the V r of mesopores.
To sum it up, the analysis of fractal dimensions is a topic of actuality in geosciences in general
and contributes to a better understanding of methane adsorption characteristics in tight sandstone gas
resources. This work addressed the characteristics of volume fractal dimensions of tight sandstone at
various size classes, but the surface fractal dimensions are not discussed in this paper, which could be
a future research direction.

Author Contributions: Data curation, Z.W. and X.J.; Formal analysis, Z.W.; Investigation, Z.W.; Methodology,
M.P. and Y.S.; Project administration, Y.S.; Resources, Y.S.; Supervision, M.P. and Y.S.; Visualization, Z.W.;
Writing—original draft, Z.W.; Writing—review & editing, X.J. All authors have read and agreed to the published
version of the manuscript.
Funding: This research was funded by the National Science and Technology Major Project of China, grant
number 2017ZX05013005-009.
Acknowledgments: The authors greatly appreciate the Changqing Oilfield Branch Company of China National
Petroleum Corporation for all the support during this work. The authors would like to thank all editors and
reviewers for their constructive comments on this paper.
Conflicts of Interest: The authors declare no conflict of interest.

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