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A Caprock Evaluation Methodology For Underground G
A Caprock Evaluation Methodology For Underground G
A Caprock Evaluation Methodology For Underground G
Article
A Caprock Evaluation Methodology for Underground Gas
Storage in a Deep Depleted Gas Reservoir: A Case Study for the
X9 Lithologic Trap of Langgu Sag, Bohai Bay Basin, China
Shanpo Jia 1,2 , Caoxuan Wen 1, *, Xiaofei Fu 1 , Tuanhui Liu 3 and Zengqiang Xi 3
1 Institute of Unconventional Oil & Gas, Northeast Petroleum University, Daqing 163318, China;
jiashanporsm@163.com (S.J.); fuxiaofei2008@sohu.com (X.F.)
2 State Key Laboratory for GeoMechanics and Deep Underground Engineering, China University of Mining &
Technology, Xuzhou 221116, China
3 Exploration and Development Research Institute of Huabei Oilfield Company, CNPC, Renqiu 062552, China;
yjy_lth@petrochina.com.cn (T.L.); yjy_xzq@petrochina.com.cn (Z.X.)
* Correspondence: wencaoxuan1997@163.com
Abstract: The evaluation of caprocks’ sealing capacity is exceedingly important for depleted gas
reservoirs to be reconstructed into gas storage. In this paper, based on the physical sealing mechanism
of caprock, four aspects of ten indexes of caprock quality evaluation were firstly selected, and the
related classification standards were established. Secondly, based on the rock mechanical sealing
mechanism, elastic and plastic indexes were selected to characterize the mechanical brittleness of
caprock, and a brittleness evaluation method of caprock based on complete stress-strain curves
was established. Then, a systematic comprehensive evaluation model (including 5 aspects and
12 evaluation indexes) for the sealing capacity of gas storage caprock was proposed, and the analytic
hierarchy process (AHP) was used to determine the weight of the 12 indexes in the evaluation model,
Citation: Jia, S.; Wen, C.; Fu, X.; Liu,
and the formula for calculating the suitability of the caprock sealing capacity was established. Finally,
T.; Xi, Z. A Caprock Evaluation
the geological data, laboratory, and field test data, including X-ray diffraction, poro-permeability test,
Methodology for Underground Gas
displacement pressure, and tri-axial compression test, were used for the caprock sealing capacity
Storage in a Deep Depleted Gas
evaluation of the X9 depleted gas reservoir, and the result from this model showed that the caprock
Reservoir: A Case Study for the X9
Lithologic Trap of Langgu Sag, Bohai
quality is suitable for underground gas storage.
Bay Basin, China. Energies 2022, 15,
4351. https://doi.org/10.3390/ Keywords: underground gas storage (UGS); caprock; sealing capacity; mechanical brittleness;
en15124351 evaluation system
after it is injected into the gas storage, which controls the vertical distribution, gas abun-
dance, and working pressure of the gas storage. At present, the caprock evaluation of
gas storage is mainly divided into two aspects: the macro- and the micro-effectiveness
evaluation of caprock [5]. From the macro perspective, lithology, thickness, continuity,
and brittle-ductile characteristic have a significant influence on the sealing capacity of
caprock [6–10]. The physical sealing mechanism of the caprock means that the caprock
realizes the function of gas sealing through its physical properties. The clay content and
sedimentary characteristics are considered to be the key parameters affecting the sealing
capacity of the caprock. Generally speaking, the higher the clay content, the better the
sealing capacity, and the mudstone caprock formed by the semi-deep and deep lake facies
has the best sealing capacity [10–12]. The caprock thickness refers to the effective thick-
ness after subtracting the area with no sealing capacity, and statistics show that there is
a thickness lower limit for the sealing capacity, beyond which, the thicker the caprock is,
the higher the cap continuity is, the stronger the sealing capacity is, and the larger the
gas field area formed [9,13–15]. The rock mechanics sealing mechanism means that in the
process of injection and production, the stress state of the caprock will change, leading to
the generation of cracks, which further makes the seal invalid. The construction practice
of underground gas storage also shows that the key factor affecting the failure of the gas
reservoir is the development of caprock fracture (mechanical failure). Although some
caprocks have good physical property conditions, they still cannot play a sealing role. The
generation of cracks is related to the caprock’s brittleness that is characterized by its me-
chanical properties. Many scholars have noticed the change of brittleness and ductility of
mudstone for a long time, and carried out many experiments on mudstone rock mechanics,
and defined the evaluation criteria of mudstone brittleness by using different parameters,
but there are few studies specifically on mudstone caprock of gas storage [4,16,17]. From
the microscopic perspective, porosity, permeability, pore size distribution, specific surface
area, and displacement pressure are the main parameters to reflect the microscopic sealing
capacity of caprock, among which displacement pressure is widely regarded as the most
fundamental parameter that reflects the sealing capacity of caprock [8,13,14,18]. The sealing
mechanism of hydrocarbon caprock can be divided into a capillary seal, hydraulic seal,
overpressure seal, and hydrocarbon concentration seal, among which capillary seal is the
most important sealing mechanism of depleted gas storage caprock. The requirement for
gas seepage in caprock is that the difference between gas pressure and hydrostatic pressure
exceeds capillary pressure at the gas-water interface in caprock, and this difference in
pressure in the critical state is called displacement pressure, which is numerically equal to
capillary pressure. The laboratory test of displacement pressure can be divided into the
direct method (step-by-step method, continuous method, displacement method, and pulse
method) and indirect method (mercury intrusion method), where the step-by-step method
is based on the definition of breakthrough pressure and has a high accuracy [11,19–21]. The
breakthrough pressure can also be obtained by fitting field data, such as the time difference
of acoustic velocity [14,22,23].
You et al. systematically analyzed the geological factors influencing the caprock seal-
ing performance, established the relationship between porosity, median radius, and burial
depth, and breakthrough pressure, and proposed a quantitative evaluation method combin-
ing macro and microscopic [24]. Fu et al. classified the microscopic sealing characteristics of
the caprock and the evaluation parameters of the macroscopic sealing characteristics, and
discussed the comprehensive evaluation method of the sealing capacity of the caprock [25].
By analyzing the relationship between both the specific surface area and the breakthrough
pressure with caprock sealing performance, Fan et al. proposed an evaluation template
of mudstone caprock by combining specific surface area and breakthrough pressure [26].
In addition, some scholars [27,28] conducted statistical studies on more than 40 discov-
ered gas reservoirs in China, and obtained the factors affecting the sealing capacity of
caprocks, such as lithology, thickness, displacement pressure, damage degree of caprocks
caused by faults, gas reservoir pressure, and natural gas viscosity, and established the
Energies 2022, 15, 4351 3 of 22
corresponding evaluation standards. In spite of these, the current gas sealing capacity
evaluation of caprock has the following shortcomings: (a) the evaluation indexes, which are
the parameters that can reflect or affect the sealing capacity of the caprock when one carries
out the sealing evaluation of the caprock, are quite a few, usually one or several, which
cannot fully reflect the sealing capacity of caprock. For example, the influence of brittleness
of caprock on sealing capacity is usually ignored [18]; (b) for the same evaluation index,
the evaluation criteria are inconsistent. Generally, efficient sealing means that when the
value of a parameter that can reflect the sealing capacity of the caprock is less or greater
than a certain value, the caprock has the best gas sealing capacity. Taking permeability as
an example, Bai et al. [14] considered the caprock with a permeability less than 0.1 mD
as a highly efficient sealing caprock, while Zhou et al. [7] considered it as 0.00001 mD; (c)
the evaluation work is not systematic, and the degree of influence of different evaluation
indexes on the sealing performance of the caprock cannot be considered quantitatively.
Based on the analysis above, a caprock sealing capacity evaluation system based on
the analytic hierarchy process (AHP) is proposed, which includes multiple key parameters
related to caprock, such as the physical property parameters and the brittleness character-
ized by the mechanical properties. Then, the caprock sealing capacity of X9 gas storage is
evaluated using this method.
Table 2. Thickness classification of gas storage caprock of depleted oil and gas reservoir.
① ② ③ ④
Water
(Wetting
Pw phase)
Pc
Caprock ① Pc﹤Pc, entry
Figure
Figure 1.1. Mechanism
Mechanism of gasof gas breaking
breaking through
through caprock [20]. caprock [20].
Energies 2022, 15, 4351
Energies 2022, 15, 4351 6 of 22
Confining pressure
& temperature
Saturated with liquid
P V
Confining pressure
& temperature
Breakthrough point
t t
Figure 2.2.AA
Figure step-by-step method
step-by-step for displacement
method pressure. pressure.
for displacement
The displacement pressure of caprock in more than 40 medium- and high-efficiency
The displacement
gas reservoirs pressure
in China is found of caprock
statistically that allin
themore than 40pressure
displacement medium- andofhigh-ef
values
gas reservoirs
caprock in China
of high-efficiency gasisreservoirs
found statistically
exceed 20 MPa, that
andall
thatthe displacement pressure
of medium-efficiency gas va
reservoirsof
caprock all high-efficiency
exceeded 15 MPa [27].
gas Therefore,
reservoirstheexceed
caprock20sealing
MPa,capacity according
and that to
of medium-ef
the displacement pressure can be classified into four grades, as shown in Table 4.
gas reservoirs all exceeded 15 MPa [27]. Therefore, the caprock sealing capacity ac
to the4. displacement
Table pressure
Displacement pressure can be
classification classified
of gas into of
storage caprock four grades,
depleted asgas
oil and shown in Table
reservoir.
Classification
Table 4. Displacement Displacement
pressure classification of gas Pressure/MPa
storage caprock of depleted oil and g
voir. I >20
II 5~20
III
Classification 1~5
Displacement
Pressure/MPa
IV <1
Ⅰ >20
Ⅱ
2.4.2. Acoustic Time Method 5~20
Ⅲdata is also used to study the capillary sealing capacity
The acoustic logging 1~5 of
Ⅳ
mudstone caprock. Acoustic time difference is affected by many geological factors,
<1 such as
lithology, rock structure, buried depth, and geological time. For mudstone caprock, density
is an important factor in controlling the acoustic time difference, and mudstone density
2.4.2. Acoustic
is closely Time
related to rockMethod
porosity. Therefore, the acoustic time difference can effectively
reflectThe
the porosity of mudstone
acoustic logging data caprock.
is also used to study the capillary sealing capacity o
A large number of statistics show that there is the following relationship between
stone caprock. Acoustic time difference is affected by many geological factors,
mudstone porosity and acoustic time difference [29]:
lithology, rock structure, buried depth, and geological time. For mudstone caproc
∆t = Aφ +the
sity is an important factor in controlling B acoustic time difference, and (1)mudsto
sity is closely related to rock porosity. Therefore, the acoustic time difference ca
where, ∆t is the mudstone acoustic time difference; φ is the mudstone porosity; A, B are
tively reflect
empirical the porosity of mudstone caprock.
parameters.
A large
The number
measured of statistics
mudstone show
displacement that has
pressure there is the following
a significant relationship b
inverse relationship
mudstone porosity
with the porosity. and acoustic
The smaller time
the porosity difference
is, the higher the [29]:
compaction degree of mudstone
is, the denser the mudstone is, the better the capillary sealing ability is, and the higher
= Aφ + B displacement pressure and
Δt mudstone
the displacement pressure is. It is assumed that the
porosity satisfy the following relationship,
where, Δt is the mudstone acoustic time difference; φ is the mudstone porosity
Pdw = a exp(−bφ) (2)
are empirical parameters.
The
where, Pdwmeasured mudstone
is displacement displacement
pressure; pressure
a, b are empirical has a significant inverse relat
parameters.
with the porosity. The smaller the porosity is, the higher the compaction degree o
stone is, the denser the mudstone is, the better the capillary sealing ability is, a
higher the displacement pressure is. It is assumed that the mudstone displaceme
sure and porosity satisfy the following relationship,
Energies 2022, 15, 4351 7 of 22
According to Equations (1) and (2), the relationship between the mudstone displace-
ment pressure and the acoustic time difference is obtained:
where, BEM = ( E − Emin )/( Emax − Emin ), BPR = (µ − µmax )/(µmin − µmax ). Emax , Emin ,
µmax , µmin are the maximum and minimum values of the elastic modulus and the maximum
and minimum values of the Poisson’s ratio, respectively.
The plasticity index Bp is used to describe the post-peak curve shape [33]. The solution
steps of Bp are as follows:
(1) Define the relative magnitude of post-peak stress drop:
0
B1 = (τp − τr )/τp (5)
0
where, B1 is the relative magnitude of stress drop, the value range is 0~1; τ p and τ r are the
peak strength and residual strength respectively.
(2) Define the absolute rate of post-peak stress drop:
0
B2 = αlg k ac( AC) (6)
0
where, B2 is the absolute rate of stress drop; α is the adjustment factor, and the value is 0.6;
the geometric meaning of k ac( AC) is the slope of the line connecting the starting point of the
yield stage to the starting point of the residual stage. Since the slope is negative, an absolute
value is added. Taking the common logarithm and multiplying α is to convert the absolute
0
rate of stress drop between 0 and 1, and take B2 = 1 when the post-peak stress falls vertically
to zero. Combining Figure 3 and the magnitude of the relative stress drop and the absolute
0 0
rate of the stress drop, it can be found that the values of B1 , B2 calculated from curve
OACE section are equal to that calculated from the OABCE section. However, due to the
existence of the yield stage in the OABCE section, the rock brittleness corresponding to the
0
two curves is different in fact. To this end, the yield influence coefficient B3 is introduced.
τ p −τ r
B p = B1' B2' B3' = α lg kac ( AC ) (1-
Energies 2022, 15, 4351
τp 8 of 22
σ1−σ3
A B D
a C E
ε
O
Figure 3. Schematic diagram of calculation parameters of plasticity index.
Figure 3. Schematic diagram of calculation parameters of plastici
(3) Define the yield influence coefficient:
Based on the above Ⅱ analysis, the quality of the caprock can be 30~50 classified into four
grades from the perspective of rock brittleness, as shown in Table 5.
Ⅲ 50~60
Table 5. Rock mechanics Classification of gas storage caprock of depleted gas reservoir.
Ⅳ >60
Classification Elasticity Index/% Plasticity Index/%
I <30 >60
II 30~50 50~60
3. Materials and Methods for Study Area
III 50~60 30~50
IV >60 <30
3.1. Study Area of X9 Lithologic Trap
3. Materials and Methods for Study Area
Daxing conglomerate body is located in Langfang Ci
3.1. Study Area of X9 Lithologic Trap
located
Daxingin the downthrown
conglomerate side ofCity,the
body is located in Langfang Daxing
Hebei faultandin the
Province, China,
located in the downthrown side of the Daxing fault in the Gu’an-Jiuzhou fault structural
zone
zone of of Langgu
Langgu sag. It is sag.
close toIt is close
Daxing to the
uplift with Daxing uplift
Daxing fault with the D
as the boundary
to the northwest, and adjacent to the deep zone of Langgu sag to the southeast. Several
the northwest,
conglomerates andfrom
are distributed adjacent to the
north to south, deep
and the zone of
X9 conglomerate Langgu
is located in sa
the middle of the downthrown side of the Daxing fault (Figure 4).
glomerates are distributed from north to south, and the X9
middle of the downthrown side of the Daxing fault (Figur
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23
Figure4.4.Tectonic
Figure Tectonicgeography
geographyofofX9
X9conglomerate
conglomerate(a)
(a)Beijing–Tianjin–Hebei
Beijing–Tianjin–Hebeiarea;
area;(b)
(b)Langfang
Langfangcity;
city;
(c) Distribution of Daxing conglomerate body; (d) Langgu sag.
(c) Distribution of Daxing conglomerate body; (d) Langgu sag.
Thelithology
The lithologyof ofthe
theupper
uppermember
memberof ofEs3
Es3isisconsisting
consistingof ofgray
graymudstone,
mudstone,silty siltymud-
mud-
stone, and gray, gray-white argillaceous silty conglomerate, silty
stone, and gray, gray-white argillaceous silty conglomerate, silty conglomerate, and fine conglomerate, and fine
conglomerate. The
conglomerate. The thickness thickness is generally more
more than 300 m, and the maximum thicknessis
than 300 m, and the maximum thickness
isabout
about700700m. m.TheTheupper
uppermember
member of of Es3 is in in conformable
conformable contact
contact withwiththetheunderlying
underlying
middlemember
middle memberofofEs3. Es3.
Thelithology
The lithologyofofthe theupper
upperpart
partofofthe
themiddle
middlemembermemberof ofEs3
Es3isisbrown-gray
brown-graymudstone mudstone
mixedwith
mixed withgray grayandandgray-white
gray-whiteargillaceous
argillaceoussiltysiltyconglomerate,
conglomerate,silty siltyconglomerate,
conglomerate,and and
fineconglomerate,
fine conglomerate, the the thickness
thickness of which is generally
generally more
more thanthan300 300m. m.As Aswell,
well,the li-
the
thology of
lithology of the
the lower
lower part of the middle member of Es3 is interbedded interbedded with with brownish-gray
brownish-gray
mudstone,
mudstone,dark darkmudstone,
mudstone,gray grayargillaceous
argillaceoussiltysiltyconglomerate,
conglomerate,silty siltyconglomerate,
conglomerate,fine fine
conglomerate,
conglomerate,conglomeratic
conglomeraticconglomerate,
conglomerate,and andfinefineconglomerate.
conglomerate.The Thethickness
thicknessof ofthe
the
lower
lowerpart
partofofthe themiddle
middle member
member of of
Es3 is generally
Es3 is generally more than
more 400400
than m, and it is itconformable
m, and is conform-
contact with the
able contact with underlying lowerlower
the underlying member of Es3.of Es3.
member
The
The lower member of Es3 is a large set brownish-gray
lower member of Es3 is a large set of of brownish-gray andand darkdarkmudstone
mudstone interbed-
inter-
ded with fine conglomerate. The thickness is generally more than
bedded with fine conglomerate. The thickness is generally more than 400 m, and the 400 m, and the thickest
thick-
part is more
est part thanthan
is more 10001000
m. The composition
m. The compositionof the ofgravel is mainly
the gravel limestone
is mainly and dolomite,
limestone and dolo-
and it is
mite, andin unconformable contact contact
it is in unconformable with thewith
underlying strata. The
the underlying X9 conglomerate
strata. The X9 conglomerate body is
located
body isinlocated
the lower member
in the of Es3 (Figure
lower member of Es35).(Figure 5).
According to the sedimentary characteristics of the conglomerate, it can be subdivided
into two sets of producing layers, the I and II set of conglomerates. There are stable
mudstone interlayers between the two sets of producing layers, making the two sets of
producing layers closed and non-connected. As the main production layer, at present, a
total of 15 wells have been drilled into the I conglomerate body, and the lateral development
is stable.
The structure of the top surface of the I set of X9 conglomerate body is the strata
dipping northward, and a lithologic trap is formed by the control of the pinch-out line
of the conglomerate body in the east and south directions. The high point, with a buried
depth of 3720 m, is located at X9-1 well. The trap amplitude is 400 m, and the trap area
is 4.36 km2 . The structure of the bottom surface is the strata dipping northward, and a
lithologic trap is formed by the control of the pinch-out line of the conglomerate body in
the east and south directions. The high point, with a buried depth of 3840 m, is located at
Well X9-1. The trap amplitude is 280 m, and the trap area is 1.71 km2 .
Energies 2022,
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4351 10 of
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of 22
50 Gr 100
0 Gr 100 depth lithology
0 Gr 100 depth lithology
3600
4000
3700
3800
4100
3900
4000
conglomerate
conglomerate
4200
4100 mudstone
mudstone
(a) (b)
Figure 5. Drilling
Figure column
5. Drilling diagram
column of of
diagram a main producing
a main layer
producing of of
layer X9:X9:
(a)(a)
Well X9-2x;
Well (b)(b)
X9-2x; Well X9-9X.
Well X9-9X.
order of them,
t. Among importance of factors
cumulative gas by clarifyingofvague
production the Ⅰ concepts.
conglomerate body is 10.41 × 108 m3
Accordingoil
and cumulative to production
the sealing requirements
of 35.72 × 104oft.gas storage caprock
According in depleted gas
to the reconstructed reservoirs,
structure,
the quality of gas storage caprock is taken as the target layer,
the Ⅰ set of gas geological reserves of conglomerate is calculated by volume method. and the lithology, thickness,
The
porosity and permeability characteristics, displacement pressure,
gas geological reserves of the conglomerate body are 18.03 × 10 m and condensate oil 8 3 and rock mechanical
properties
reserves of the×caprock
are 85.89 104 t. are taken as the criterion layer. Then, the 12 basic indicators were
refined into evaluation layers, and a target hierarchy model based on AHP was established
(Figure
3.2. 6). Model Based on AHP Method
Evaluation
3.2.1. Target Hierarchy of Comprehensive Evaluation
Analytic Hierarchy Process (AHP) is a decision analysis method combining qualita-
tive and quantitative methods, and is an effective method to determine weights [34]. The
mines the order of importance of factors by clarifying vague concepts.
According to the sealing requirements of gas storage caprock in depleted gas reser-
voirs, the quality of gas storage caprock is taken as the target layer, and the lithology,
thickness, porosity and permeability characteristics, displacement pressure, and rock me-
chanical properties of the caprock are taken as the criterion layer. Then, the 12 basic indi-
Energies 2022, 15, 4351 11 of 22
cators were refined into evaluation layers, and a target hierarchy model based on AHP
was established (Figure 6).
Smallest Thickness
Laboratory Results
Caprock Lithology
Clay Content
Elastic Index
Plastic Index
Permeability
Continuity
Porosity
C1 C2 C3 C4 C5 C6 C7 C8 C9 C10 C11 C12
Figure 6. Hierarchical structure model of comprehensive evaluation index of gas storage caprock
Figure 6. Hierarchical structure model of comprehensive evaluation index of gas storage caprock
quality of the depleted gas reservoir.
quality of the depleted gas reservoir.
3.2.2.Weight
3.2.2. WeightCoefficient
Coefficient
Afterthe
After theobjective
objectivehierarchy
hierarchyisisestablished,
established,ititisisnecessary
necessaryto tocarry
carryoutoutaaquantitative
quantitative
analysis of each influencing factor. In order to facilitate the conversion from
analysis of each influencing factor. In order to facilitate the conversion from qualitative to qualitative to
quantitativevalues
quantitative valuesand
anddetermine
determinethe thecomparative
comparativeweightweightvector,
vector,the
the“1–9”
“1–9”scale
scalemethod
method
proposed
proposedbyby T. Saaty
T. Saaty ij takepijthe take
[35], p[35], valuethe
1, 2, value
. . . , 9 and ,
1,2its ,9 and1, its
reciprocal 1/2,reciprocal
. . . , 1/9.
Where,
1,1/ 2, pijrepresents the importance
,1/ 9 . Where, of i-ththe
pij represents factor relative toofj-th
importance factor;
i -th 1/9relative
factor represents
to jthe
-th
lowest degree of importance; 1 represents the same degree of importance; 9 represents the
factor; 1/9
highest degreerepresents the lowest
of importance; degree of importance;
the comparison rules are shown 1 represents
in Tablethe
6. same degree of
importance; 9 represents the highest degree of importance; the comparison rules are
shown
Table in Table 6. of the relative importance of indexes.
6. Classification
For each judgment matrix P, the maximum eigenvalue and its corresponding feature
vector are first obtained, and the feature vector is the weight of each evaluation factor. The
Energies 2022, 15, 4351 12 of 22
method for calculating the factor weight vector ω, the maximum eigenvalue λmax , and the
random consistency ratio CR is as follows:
!1/n
n
ωi = ∏ pij ( j = 1, 2, · · · , n) (10)
j =1
!
n
ωi = ωi / ∑ ωj (i = 1, 2, · · · , n) (11)
j =1
ω = ( ω1 , ω2 , · · · , ω n ) T (12)
1 n
n i∑
λmax = [(Pω)i /ωi ] (13)
=1
where: mi is the quantified value of each evaluation index; ω i is the weight value of each
evaluation index; i = 1, 2, . . . , 12.
By substituting the comprehensive suitability value M of caprock calculated according
to Equation (15) into Table 8 for comparison, the suitability degree of caprock can be
obtained, and the feasibility of the gas storage construction project can be considered
according to the corresponding countermeasures. The trap with “Optimal” caprock has a
good sealing ability and high safety, and is very suitable for building the gas storage. The
trap with “Suitable” caprock is the second choice to build gas storage, but it is necessary
to strengthen the sealed investment and monitoring of gas storage during the operation
period. The trap with “Basically suitable” caprock basically meets the requirement to build
gas storage, but special funds shall be reserved during the construction period to evaluate
the sealing of the gas storage. The trap with “Not suitable” caprock cannot be considered
for building gas storage.
Table 8. Evaluation table of comprehensive suitability grade of gas storage caprock of depleted oil
and gas reservoir.
Mineral Content/%
Well Number Member Lithology Illite-Montmorillonite
Kaolinite Chlorite Illite Mixed Layer Interlayer Ratio
Gray
RS 2X Es2 + 3 6.9 6.7 33.3 53.1 45.8
mudstone
Gray
XG 1 Es3 6.7 5.1 20.6 67.6 37.1
mudstone
The X9 conglomerate body is located in the lower member of the Es3, and the caprock is
a large set of brownish-gray and dark red mudstone with good continuity, and the thickness
is generally more than 400 m. For the X9 lithologic trap gas reservoir, the mudstone caprock
can not only perform vertical sealing but also play the role of lateral sealing (Figure 7).
XG 1 Es3 Gray mudstone 6.7 5.1 20.6 67.6 37.1
The X9 conglomerate body is located in the lower member of the Es3, and the caprock
is a large set of brownish-gray and dark red mudstone with good continuity, and the
thickness is generally more than 400 m. For the X9 lithologic trap gas reservoir, the mud-
Energies 2022, 15, 4351 14 of 22
stone caprock can not only perform vertical sealing but also play the role of lateral sealing
(Figure 7).
(a)
Fault
(b) (c)
Figure 7. Profiles of connected wells in X9 gas reservoir: (a) X9-11x~X9P1~X9-3; (b) X9P2~X9P1~X9-
Figure 7. Profiles of connected wells in X9 gas reservoir: (a) X9-11x~X9P1~X9-3; (b) X9P2~X9P1~X9-
9x; (c) Top structure diagram.
9x; (c) Top structure diagram.
Due
Duetoto the
the lack
lack of samples of
of samples of the
themudstone
mudstonecaprock
caprockininthe
theX9X9 area,
area, thethe caprock
caprock sam-
samples
ples of the same layer in the adjacent area were selected for testing, and the results
of the same layer in the adjacent area were selected for testing, and the results of the porosity of the
porosity and permeability test according to SY/T 5336-2019
and permeability test according to SY/T 5336-2019 are shown in Table 10. are shown in Table 10.
The porosity range of the caprock of the lower member of Es3 in the G15 well is
2.16~8.92%, with an results
Table 10. Laboratory averageof value
porosityof and
4.08%. The permeability
permeability rangeofof
characteristics the caprock
caprock samplesisof
1.16
the
×adjacent
10−3~55.1 ×
well. 10 −3 mD, with an average value of 22.3 × 10−3 mD. The porosity range of the
caprock of the lower member of Es3 of the X8 well is 4.84%~6.66%, with an average value
Number Well Numberof sample Porosity/% Permeability/(10 −3 mD) ·cm −3 )
of 5.59%. The permeability 8 is quite large with the value of 821Density/(g
× 10−3 mD, and
the main1 reason is that the stress release 2.16 causes the micro-cracks
1.16 of mudstone to2.61 open and
the permeability
2 of the caprock becomes 2.91 larger. The permeability
42.80 range of rest samples
2.66 in
X8 well3 is 0.63 × 10−3~15.10
G15 × 10−3 mD,3.19with the average value 8.40of 5.5 × 10−3 mD. The 2.63
porosity
4 3.22 4.06 2.65
range of the caprock of the lower member of Es3 of the T29 well is 3.53%~8.27%, and the
5 8.92 55.10 2.61
6 6.66 0.79 2.53
7 4.98 0.63 2.54
X8
8 5.86 821.00 2.45
9 4.84 15.10 2.51
10 3.53 0.14 2.58
11 T29 8.27 246.0 2.57
12 3.89 1.10 2.57
The porosity range of the caprock of the lower member of Es3 in the G15 well is
2.16~8.92%, with an average value of 4.08%. The permeability range of the caprock is
1.16 × 10−3 ~55.1 × 10−3 mD, with an average value of 22.3 × 10−3 mD. The porosity
range of the caprock of the lower member of Es3 of the X8 well is 4.84%~6.66%, with an
average value of 5.59%. The permeability of sample 8 is quite large with the value of
Table 10. Laboratory results of porosity and permeability characteristics of caprock samples of the
adjacent well.
Tong 29
Xing 8
Gu 15
8
Porosity(%)
Percentage (%)
50
2.5 25
0
Ⅰ Ⅱ Ⅲ Ⅳ
Classfication
The
The breakthrough pressure laboratory
breakthrough pressure laboratorytest
testofof mudstone
mudstone caprock
caprock waswas carried
carried out
out (Fig-
(Figures
ures 9 and9 and10)10) and
and thethe resultsare
results areshown
shownininTable
Table11.
11. The
The breakthrough
breakthrough pressure
pressure values
values
measured
measuredare areall
allgreater
greaterthanthan20 20MPa,
MPa,thethemaximum
maximumvalue valuewas wasabout
about32.11
32.11MPa,
MPa,andandthe
the
permeability measured was basically within 0.10 × 10 −3 ~1.1 × 10 −−3
3 mD. The permeability
permeability measured was basically within 0.10 × 10 ~1.1 × 10 −3 permeability
value
valueof ofrock
rocksample
sample55isisrelatively
relativelylarge
largedue
duetotothetheexistence
existenceofofmicro-cracks,
micro-cracks,and andthe
the
corresponding
correspondingbreakthrough
breakthroughpressure
pressure value is the
value smallest,
is the smallest, about 24 MPa.
about It isItnot
24 MPa. difficult
is not diffi-
to seetothat
cult seethere
that is an obvious
there negative
is an obvious relationship
negative between
relationship permeability
between and breakthrough
permeability and break-
pressure,
through that is, thethat
pressure, greater thegreater
is, the permeability is, the smaller
the permeability the smaller
is, the breakthrough pressure is
the breakthrough
(Figure
pressure 11).
is (Figure 11).
Table 11. Breakthrough pressure of caprock sample of adjacent well in X9 area (confining pressure
60 MPa, temperature 70 ◦ C).
⑧
⑧⑧ ⑩
②
⑩⑩
②② ⑨
① ⑨⑨
①① ⑤
③ ⑤⑤ ⑥
③③ ⑥⑥
⑦
⑦⑦
Figure
Figure 9. Breakthrough
9. 9.
Breakthrough pressure
pressure ofof
of of caprock
caprock test testequipment
equipment
equipment (U-TP-01).
(U-TP-01).
Figure
Figure 9. Breakthrough
Breakthrough pressure
pressure caprock
caprock test
test equipment (U-TP-01).
(U-TP-01).
35
35 35
Gu15-1
Gu15-1
Gu15-1
30
30 30
Inlet pressure/MPa
Inlet pressure/MPa
25 25
pressure/MPa
25
20 20
20
15 15
15
Inlet
10 10
10
5 5
5
0 0
0 00 5 5 10 10 15 15 20 20 25 25 30 30
0 5 10 15 20 25 30
Time/h
Time/h
Time/h
Figure 10.10.
Figure Inlet pressure
Inlet loading
pressure curve
loading and
curve time
and (Gu15-1).
time (Gu15-1).
Figure
Figure10.10.Inlet
Inletpressure
pressureloading
loadingcurve
curveand
andtime
time(Gu15-1).
(Gu15-1).
34
34 T29 Linear Fit
T29
X8 80%Linear Fit Band
Confidence
(MPa)
32 X8
G15 80%80% Confidence
Prediction BandBand
(MPa)
30
pressure
30
y=2
0
28 y .7-2
R 2==20..792ln
0 7 -2.9x
Breakthrough
28
R .2=401 2l
n
0.7 x
Breakthrough
26 40 1
26
24 not considered
for fitting
24 not considered
for fitting
22
0.0001 0.001 0.01 0.1
22 Pemeability (mD)
0.0001 0.001 0.01 0.1
Pemeability
Figure 11. Relationship between (mD) pressure and permeability.
breakthrough
Figure 11. Relationship between breakthrough pressure and permeability.
Figure
Figure11.11.
Relationship between
Relationship breakthrough
between pressure
breakthrough and and
pressure permeability.
permeability.
Energies 2022, 15, 4351 17 of 22
The breakthrough pressure test was also carried out in the same layer of mudstone
in the No.102 well in the adjacent area. Under the conditions of temperature 26 ◦ C and
pressure 30 MPa, the breakthrough pressure reached 40 MPa, which also proved that the
mudstone of this layer has good sealing capacity.
According to Equation (3), and the average acoustic time difference values of mudstone
on the top of the conglomerate body in X9, the displacement pressure of mudstone caprock
in X9 were calculated, in which the empirical parameters c, d are 3673.61 and −0.02764.
The displacement pressure values are all greater than 6 MPa (Table 12), indicating that the
mudstone caprock in the area has good sealing performance.
Displacement Displacement
Well No. ∆t µs/m Well No. ∆t µs/m
Pressure/MPa Pressure/MPa
X9 226 7.11 X9-4 216 9.38
X9-1 232 6.03 X9-6 228 6.73
X9-2 229 6.55 X9-7 221 8.17
X9-3 221 8.17 X9-9 230 6.37
Under simulated formation temperature and pressure, triaxial tests were carried out on
four samples from Well G15 and three samples from Well T29. The triaxial rock mechanics
test system RTR-1000 was used for the test (Figure 12). The test procedure is as follows:
(1) Load the prepared sample into the triaxial chamber, and add axial pressure of 0.5 MPa to
the sample; (2) Close the pressure chamber and inject hydraulic oil; (3) Heating to formation
Energies 2022, 15, 4351 18 of 23
temperature; (4) Add confining pressure to formation pressure; (5) Compressing the sample
with a strain rate of 0.002 mm/s until the sample is failed; (6) Save the experimental data.
5
7 Oil separator
N 8 Acoustic emission probe
9 Confining pressure sensor
15
1 T
2 12
Z 7 16
Tc
Sample
3 J
9 10 13
P
8
4
11 17
Figure12.
Figure 12.Triaxial
Triaxialmechanics
mechanicstesting
testingsystem
system(RTR-1000)
(RTR-1000)ofofcaprock.
caprock.
Rockmechanics
Rock mechanicstest testresults
resultsofofmudstone
mudstonecaprock
caprockof oftwo
twowells
wellsininthe
theadjacent
adjacentarea
area
are shown
are shown in in Figure 13. Due to the existence of microcracks inside sample G3,
13. Due to the existence of microcracks inside sample G3, it sud- it suddenly
breaks
denly whenwhen
breaks the stress valuevalue
the stress is at its
is peak
at its strength, and the
peak strength, and post-peak stage stage
the post-peak is veryis short.
very
All other
short. six samples
All other all show
six samples all obvious
show obviousstrain-softening characteristics,
strain-softening which indicate
characteristics, which indi-that
the caprock
cate in this area
that the caprock has area
in this certain
hasplastic
certain deformation ability under
plastic deformation simulated
ability formation
under simulated
conditions.
formation conditions.
250 250
T1
G1 Confining pressure 49.7MPa
T2
G2 Temperature 120℃
T3
200 G3 200
G4
Stress (MPa)
Stress (MPa)
150 150
100 100
Rock mechanics test results of mudstone caprock of two wells in the adjacent area
are shown in Figure 13. Due to the existence of microcracks inside sample G3, it suddenly
breaks when the stress value is at its peak strength, and the post-peak stage is very short.
All other six samples all show obvious strain-softening characteristics, which indicate that
Energies 2022, 15, 4351 18 of 22
the caprock in this area has certain plastic deformation ability under simulated formation
conditions.
250 250
T1
G1 Confining pressure 49.7MPa
T2
G2 Temperature 120℃
T3
200 G3 200
G4
Stress (MPa)
Stress (MPa)
150 150
100 100
50 50
(a) (b)
Figure13.
Figure 13.Stress
Stress−strain
−straincurves
curvesofofcaprock
caprocksamples:
samples:(a)(a)
Well Gu15;
Well (b)(b)
Gu15; Well T29.
Well T29.
Table13
Table 13 shows
shows the
thelaboratory
laboratory test results
test of caprock.
results of caprock.Under normal
Under temperature
normal and
temperature
lowlow
and confining
confiningpressure, the the
pressure, hard rock
hard generally
rock failsfails
generally in brittle mode.
in brittle mode. WhenWhen thethe
stress
stress
reachesits
reaches itspeak
peakvalue,
value, the
the magnitude
magnitude of of the
the strain
strainisisgenerally
generally1010−
−3. In thisthis
3 . In test, except
test, exceptfor for
G1(strain
G1 (strainmagnitude
magnitudeofof10 10−−33,, elasticity
elasticity index
index of
of 64.68%,
64.68%, plasticity
plasticityindex
indexof of1.57%),
1.57%),allallfail-
failure
ure modes of the other rocks were a ductile failure. Under the simulated
modes of the other rocks were a ductile failure. Under the simulated formation conditions, formation con-
ditions,
the strainthe strain magnitude
magnitude is 10−2 , iniswhich
10−2, inthe
which
axialthe axial compression
compression strain isstrain is 1.36–3.2%,
1.36–3.2%, the elastic
the elastic index is 33.38–58.19%, and the average value is 47.56%.
index is 33.38–58.19%, and the average value is 47.56%. The plasticity index ranges The plasticity indexfrom
ranges from 19.98 to 67.98%, with an average value of 47.60%. Therefore, caprock is be-
19.98 to 67.98%, with an average value of 47.60%. Therefore, caprock is believed to have a
lieved to have a certain plastic deformation capacity.
certain plastic deformation capacity.
Table 13. Rock mechanics test results of caprock samples under formation conditions.
According to the above analysis, the scores of the 12 basic indicators of the X9 depleted
gas reservoir caprock are: 10, 8, 8, 10, 10, 8, 8, 8, 10, 8, 8, 8. The scores of the respective
indexes and the corresponding weight values corresponding to Table 7 are substituted into
Equation (15) to obtain the comprehensive suitability value of the depleted gas reservoir
caprock. According to the classification evaluation of Table 8, it can be seen that the caprock
of the gas storage is of good quality, close to the requirements of optimal caprock, but
the sealing performance monitoring of the gas storage should be strengthened during the
operation phase of the gas storage. The evaluation results are consistent with the expert
argumentation results [36].
4.2. Discussion
It is not difficult to see that the breakthrough pressure measured in the laboratory
is significantly greater than the breakthrough pressure measured by the acoustic time
difference. It is analyzed that: When drilling to plane A, the vertical stress overlying the
core is reduced firstly. During the process of stress unloading in the vertical direction, the
inhomogeneity in the rock mass leads to the incongruity of deformation, which produces
a local stress field in the vertical direction and horizontal tensile cracks in the core. Then,
when the core enters the drilling pipe, the horizontal stress gradually decreases, the wellbore
tends to collapse, and the core expands laterally, resulting in vertical fractures (Figure 14).
Once horizontal or vertical fractures occur in the core, the acoustic time difference increases,
Energies 2022, 15, 4351 19 of 22
and the breakthrough pressure value decreases significantly. For laboratory tests, it is the
Energies 2022, 15, 4351 20 of 23
samples with higher integrity that are selected, and correspondingly, the breakthrough
pressure values are relatively higher.
Drilling fluid
Stress (MPa)
Vertical stress
Drill pipe
Maximum horizontal
Vertical crack stress
Horizontal crack Borehole collapse
tendency
Unloading Time
Lateral Axial tensile Lateral
expansion expansion
Horizontal stress
Horizontal stress
Horizontal stress
Δσ
Plane A
Plane A
Caprock mudstone
(Dark red)
Vertical stress
Accordingtotothe
According theabove
aboveanalysis,
analysis,the thedisplacement
displacementpressure pressureofofthe themudstone
mudstonecaprock
caprock
calculated according to the acoustic time difference and the breakthrough pressure meas-
calculated according to the acoustic time difference and the breakthrough pressure mea-
ured by
sured by laboratory
laboratory experiments
experiments (Tables (Tables11 11and
and12)12)allallindicate
indicatethat thatthethemudstone
mudstonecaprock
caprock
ofofthe
theX9X9gas gasreservoir
reservoirisisofofgood goodsealing
sealingperformance.
performance.
Theexistence
The existenceofofmicro-cracks
micro-cracksnot notonlyonlyaffects
affectsthe
thebreakthrough
breakthroughpressure, pressure,but butalso
alsothe
the
permeability. The permeability measured by laboratory
permeability. The permeability measured by laboratory test is the permeable performancetest is the permeable performance
exhibitedofofthe
exhibited thecaprock
caprockafter afterstress
stressrelease,
release,and andthe
thestress
stressrelease
releaseofofsome somesamples
samplescauses
causes
themicro-cracks
the micro-cracksofofthe themudstone
mudstonetotochange changefrom fromthethestate
stateofofnon-open
non-opentotoopen, open,thus
thusthethe
permeabilitybecomes
permeability becomeslarger.larger.There Thereisisno nosignificant
significantdifference
differencein inthe
theappearance,
appearance,density,
density,
andporosity
and porosityofofcaprock
caprocksamples
samplesfrom fromthe thesame
samestratum,
stratum,but butthe
thedifference
differenceininpermeability
permeability
isisrelatively
relativelyobvious,
obvious, which
which indicates that thatthere
thereisisaasmall
smallamount
amount ofofmicrofractures
microfractures in the
in
the caprock.
caprock. Therefore,
Therefore, it isit necessary
is necessary to adopt
to adopt moremore specific
specific methods
methods to characterize
to characterize thethe
de-
degree
gree ofofmicro-cracks
micro-cracksdevelopment
development in in the
the future when evaluating
evaluating the thesealing
sealingcapacity
capacityofof
the
thecaprock.
caprock.
Hildenbrand
Hildenbrandetetal.al.[20] [20]carried
carried out outsome
some breakthrough
breakthrough pressure
pressure tests andand
tests mademadestatis-
sta-
tics on some
tistics on some previous
previous work. work. These
These results
resultsand the
and theresults
resultsofofthis
thispaper
papershow
showthat thatthethe
higher
higherthe thepermeability
permeabilityis, is,the
thelower
lowerthe thedisplacement
displacementpressure pressureis. is.The
Thecorrelation
correlationcoeffi-
coeffi-
cient
cientbetween
betweenpermeability
permeabilityand andbreakthrough
breakthroughpressure pressureofofhundreds
hundredsofofsamples samplescounted
counted
ininref.
ref. [20] is 0.26–0.99, and that of the test carried out in ref. [20] is 0.71.The
[20] is 0.26–0.99, and that of the test carried out in ref. [20] is 0.71. Thecorrelation
correlation
coefficient
coefficientbetween
betweenpermeability
permeability andandbreakthrough
breakthrough pressure
pressure in this study
in this studyis 0.74, indicating
is 0.74, indicat-
that
ing the
thatcorrelation
the correlationis effective to some
is effective extent.
to some SinceSince
extent. the data
the amount
data amount is notisabundant,
not abundant,this
relationship
this relationshipmay not maybe notaccurate enough enough
be accurate to predict to the breakthrough
predict pressure through
the breakthrough pressure
permeability. In furtherInresearch,
through permeability. more laboratory
further research, tests can tests
more laboratory be carried
can beout to enrich
carried out totheen-
database, so as to obtain a fitting relationship with
rich the database, so as to obtain a fitting relationship with less error. less error.
OnOnthe theother
otherhand,hand,ititcan canbe beseen
seenthat
thatthe thepermeability
permeabilitymeasured measuredininthis thispaper
paperisis
greater than the permeability in [20], but the breakthrough pressure
greater than the permeability in [20], but the breakthrough pressure is also greater than is also greater than the
breakthrough pressure in [20]. In addition to the difference in the
the breakthrough pressure in [20]. In addition to the difference in the core itself, the anal- core itself, the analysis
believes that the
ysis believes thatdifference
the difference in the in testing
the testingprocess is the
process main
is the main reason.
reason. For
Forexample,
example,the the
stepwise gas pressure increasing scheme (0.5 MPa per 120 h) is mentioned in ref [20], while
the loading scheme in this paper follows the Chinese standard SY/T 5748-1995, in which
the holding constant time of each stage pressure is relatively short (0.5–2 h), and the load-
ing pressure increment is 15% of the previous stage. The pressure of externally applied
Energies 2022, 15, 4351 20 of 22
stepwise gas pressure increasing scheme (0.5 MPa per 120 h) is mentioned in ref [20],
while the loading scheme in this paper follows the Chinese standard SY/T 5748-1995, in
which the holding constant time of each stage pressure is relatively short (0.5–2 h), and the
loading pressure increment is 15% of the previous stage. The pressure of externally applied
gas has a good correlation with the time of gas breakthrough, which is the higher the
pressure of externally applied gas, the shorter the breakthrough time, and vice versa [19].
In addition, the confining pressure is also one of the reasons for the difference. In this
study, the confining pressure is set at 60 MPa, which is relatively high and also means that
the same lithologic caprock with deeper depth may have better sealing ability since the
confining pressure is usually positively correlated with depth.
Faults are one of the important factors controlling traps [37]. The research object of
this paper, X9 gas storage, is reconstructed from the lithologic gas reservoir, as shown in the
yellow part of Figure 8, which means there is no fault in the reservoir or caprock. Daxing
fault is hundreds or thousands of meters away from X9 gas storage. Unlike fault-controlled
gas reservoir that is laterally sealed by faults, it is the caprock that plays the role of the
lateral and vertical seal of X9 gas storage. Naturally, the focus of trap sealing evaluation
has become the evaluation of caprock sealing capacity as presented in this study.
Building a geological model and (then) performing both analytical or numerical
geomechanical multiscale assessment using data from a mechanical earth model [38,39]
is considered to be the “gold standard” for sealing and stability evaluation of caprock
and even the whole trap. However, for many gas reservoirs, the pressure and production
information of the reservoir were mainly concerned with the early development of the
gas reservoir. Therefore, the geological model established by PETREL and other software
usually contains only a reservoir model but no caprock, and due to the lack of some data, it is
difficult to establish the entire trap geological model including reservoir, caprock, and fault,
which will be the focus of the future work. By then, many factors can be more carefully
reflected, such as rock heterogeneity based on well log analysis, mercury porosimetry
derived pore size distribution for different rock types, assessment of fracture gradient across
the reservoir and caprock lithologies, the correlation between the geomechanical state (stress
field) and transport properties (permeabilities) of the caprock, the fault characterization,
even the effects of cyclic loading and creep, and in the end, comparison can be made
between a gold standard and the method proposed in this paper.
5. Conclusions
This paper was devoted to putting forward a new qualitative and quantitative sys-
tematic evaluation method, which can comprehensively evaluate the caprock quality of
underground gas storage. By the means of geological data research, field and laboratory
tests, and theoretical analysis, the following conclusions were obtained:
(1) In this paper, the factors influencing the caprock quality are analyzed in detail from
five aspects: caprock lithology, thickness, porosity and permeability characteristics,
displacement pressure, and mechanical properties of caprock, and 12 basic evaluation
indexes are selected. Based on the relevant research results, the classification criteria
for each basic indicator are initially proposed, and the comprehensive evaluation
model based on the Analytic Hierarchy Process method is established.
(2) Based on the failure mechanism of mudstone caprock, an analytical method for
evaluating the sealing capacity of mudstone caprock using the brittleness index
is proposed. The method considers the full stress-strain curve characteristics of
mudstone, based on the mechanical analysis of the whole process of rock failure, and
comprehensively utilizes the peak strain and the post-peak curve shape to form an
evaluation index.
(3) Taking the X9 depleted gas reservoir as an example, the quality of the target caprock
is evaluated by the above method. The caprock suitability value was M = 8.77, the
caprock quality was suitable for underground gas storage, and the conditions for
Energies 2022, 15, 4351 21 of 22
rebuilding into gas storage were available. The evaluation results are consistent with
the expert demonstration results, which verified the effectiveness of the method.
(4) Due to the difficulty of core drilling and preservation of mudstone caprock, the me-
chanics and deformation characteristics of the mudstone caprock are less understood
at present, and the mechanical response which plays a key role in the sealing capacity
of gas storage caprock still needs further study.
Author Contributions: Conceptualization, S.J. and X.F.; Data curation, T.L. and Z.X.; Methodology,
C.W.; Resources, T.L. and Z.X.; Software, C.W.; Supervision, X.F.; Validation, and C.W.; Writing—
original draft, S.J. and C.W.; Writing—review & editing, S.J. All authors have read and agreed to the
published version of the manuscript.
Funding: Fundings were provided by National Natural Science Foundation of China (Grant No.
42072166), the Natural Science Foundation of Heilongjiang Province (Grant No. LH2020D004), and State
Key Laboratory for Geomechanics and Deep Underground Engineering (Grant No. SKLGDUEK2001).
Institutional Review Board Statement: Not applicable.
Informed Consent Statement: Not applicable.
Data Availability Statement: Most of the data are contained in the paper. If specific data are needed,
the corresponding author can be contacted by e-mail.
Acknowledgments: Authors wishing to acknowledge the support from the National Natural Science
Foundation of China (Grant No. 42072166), the Natural Science Foundation of Heilongjiang Province
(Grant No. LH2020D004) and State Key Laboratory for Geomechanics and Deep Underground
Engineering (Grant No. SKLGDUEK2001).
Conflicts of Interest: The authors declare no conflict of interest.
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