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energies

Article
Brittleness Evaluation in Shale Gas Reservoirs and Its
Influence on Fracability
Yapei Ye 1,2,3 , Shuheng Tang 1,2,3, * and Zhaodong Xi 1,2,3
1 School of Energy Resources, China University of Geosciences, Beijing 100083, China
2 Key Laboratory of Marine Reservoir Evolution and Hydrocarbon Enrichment Mechanism, Ministry of
Education, Beijing 100083, China
3 Key Laboratory of Strategy Evaluation for Shale Gas, Ministry of Land and Resources, Beijing 100083, China
* Correspondence: tangsh@cugb.edu.cn

Received: 23 December 2019; Accepted: 9 January 2020; Published: 13 January 2020 

Abstract: The brittleness index (BI) is a key parameter used to identify the desirable fracturing
intervals of shale gas reservoirs. Its correlation with fracability is still controversial. There have been
a variety of methods proposed that can estimate BI. The brittleness evaluation method based on
stress-strain curves according to the energy-balanced law is the most suitable and reliable in this study.
Triaxial compression test, optical microscopy and scanning electron microscopy (SEM) observation,
and X-ray diffraction analysis (XRD) were performed on nine drill core samples from well SY3 located
in the peripheral regions of Sichuan Basin, China. These tests further evaluated several commonly
used methods (brittleness indices based on rock elastic parameters, rock mineral compositions)
and determined the relationship between brittleness, rock elastic parameters, and the content of
minerals. The results obtained indicate that for sedimentary rocks, a higher Young’s modulus reduces
the brittleness of rock, and Poisson’s ratio weakly correlates with brittleness. Excessive amounts
of quartz or carbonate minerals can increase the cohesiveness of rock, leading to poor brittleness.
Furthermore, the most suitable fracturing layers possess a high brittleness index and low minimum
horizontal stress.

Keywords: brittleness; brittle minerals; Young’s modulus; Poisson’s ratio; fracability; in-situ stress

1. Introduction
Shale gas reservoirs are remarkably different compared to conventional reservoirs due to
their ultra-low porosity and permeability. It is of utmost importance to hydraulically fracture
the unconventional oil and gas reservoirs for commercial production. Consequently, the identification
of candidates for prospected fracturing in shale gas reservoirs is necessary to enhance gas productivity.
Brittleness index is an essential mechanical parameter that has been used to evaluate whether shale
gas reservoirs can easily form complex fracture networks [1,2]. Also, shales with high brittleness tend
to close hydraulically created fractures slowly [3]. Therefore, the quantitative evaluation of brittleness
is of considerable significance to the optimization of fracturing intervals.
At present, there exists no unique and universally accepted definition for rock brittleness.
Different definitions are based on their purpose. For example, brittleness has been described as the lack
of ductility [4] or the destruction of internal cohesion [5], the ability for a rock to deform and fail with a
low degree of inelastic behavior has also been used to define brittleness [6], along with the process by
which sudden loss of strength occurs with little or no plastic deformation [7], and the rock’s capability
to self-sustain fracturing [8]. Although there is no consensus on the definition, it is commonly believed
that brittle rocks are characterized by the following features: (1) easily fractured with the formation of
more cracks and (2) little plastic deformation under compression.

Energies 2020, 13, 388; doi:10.3390/en13020388 www.mdpi.com/journal/energies


Energies 2020, 13, 388 2 of 22

Brittleness is a comprehensive response of a rock’s combined mechanical properties.


The influencing factors of rock brittleness are divided into internal factors and external factors.
The intrinsic factors mainly include composition (e.g., total organic carbon (TOC), minerals, water/gas/oil
content), texture, and porosity of the rock. The external factors comprise the ambient pressure and
temperature [9]. Considering different affecting factors, numerous quantification methods for evaluating
rock brittleness have been proposed. The most widely used methods are categorized into three general
groups:(1) brittleness indices based on rock elastic parameters [10], (2) brittleness indices attained
from rock mineral compositions [11–13], and (3) brittleness indices derived from rock stress-strain
curves [8,14].
The aim of this paper is to select the most suitable and reliable brittleness evaluation method
as standard after analyzing these three methods. Through a series of experiments, the brittleness
indices by means of these three methods are respectively calculated and compared with each other.
Meanwhile, the relationship between standard brittleness index, rock elastic parameters, and the
content of minerals are investigated.
The role that brittleness plays in the selection of desired fracturing intervals is also discussed
in this study. The primary motivation of brittleness evaluation is to select prospective gas and oil
shales that can be efficiently fractured for profitable production. However, others believe that the
brittleness parameter usually ignores the actual mechanisms of effective fracturing, failing to select the
desired fracturing intervals [15–17]. Consequently, the “fracability index” is defined to select fracturing
intervals by using the parameters affecting fracability beyond the brittleness index [18]. Accordingly,
the correlation of brittleness index and fracability index is studied.

2. Reviewing and Evaluating the Existing Brittleness Indices

2.1. Brittleness Indices Based on Rock Elastic Parameters


Brittleness is a property of a material correlated with elastic and plastic deformation. If a rock
under stress has a broader region of elastic behavior and a smaller region of ductile behavior, it is
considered more brittle [19]. Therefore, elastic parameters (Young’s modulus and Poisson’s ratio) are
utilized to calculate the brittleness index of materials. Young’s modulus is a ratio of stress and strain.
Poisson’s ratio is a ratio of radial strain over axial strain. Equation (1) proposed by [10] combines
Young’s modulus and Poisson’s ratio to evaluate rock brittleness:

En + vn
BI = , (1)
2
E − Emin vmax − v
En = ; vn = (2)
Emax − Emin vmax − vmin
where E and ν are Young’s modulus and Poisson’s ratio, respectively; En and νn are normalized Young’s
modulus and Poisson’s ratio, respectively; min and max indices in the equation are the minimum and
maximum of the elastic parameters in the study area, respectively.
In this framework, the brittle rocks with a higher Young’s modulus and lower Poisson’s ratio
experience less axial strain and less radial strain under the same applied force. This indicates that these
brittle rocks can transform more absorbed energy into elastic energy to promote the initiation and
extension of cracks. However, the controversial debate of whether Young’s modulus and Poisson’s
ratio can be used to assess brittleness has intensified recently. These two parameters are elastic
parameters only corresponding to non-permanent (or elastic) deformation, but the failure of materials
refers to not only non-permanent deformation but also permanent deformation [16]. Furthermore,
previous research works found that the brittleness indices calculated from this model tend to remain
almost unchanged, or even increase, with an increase in confining pressure [15,20]. This observation
conflicts with the fact that a decrease in confinement stress increases rock brittleness [7,21]. Therefore,
the brittleness index based on elastic modulus is inappropriate to evaluate rock brittleness correctly.
Energies 2020, 13, 388 3 of 22

2.2. Brittleness Indices Attained from Rock Mineral Compositions


Minerals are regarded as the most significant factor in controlling brittle rock behavior. In this
framework, it is universally regarded that brittle minerals (e.g., quartz, carbonate minerals) tend to
promote rock brittleness while ductile matters (e.g., clay minerals, organic matter) diminish brittle
rock characteristics. Consequently, the method based on rock mineral components is expressed as
follows [11–13]:
wb
BI = , (3)
wb + wd
where Wb is the weight fraction of brittle minerals that tend to promote rock brittleness, Wd is the
weight fraction of ductile minerals that diminish rock brittle characteristics.
The content of rock minerals is easily obtained from laboratory tests or well-logging data, so it is
convenient for researchers to understand this method and calculate the brittleness index. However,
three problems exist in this methodology. First, the confirmation of brittle minerals fails to reach a
consensus. Apart from quartz, it is controversial whether carbonate minerals, pyrite, and feldspar
are “brittle” minerals. Therefore, the calculation formulas vary in different study areas. As a result,
outcomes calculated by various formulas may be extremely different. Second, each mineral is assigned
the same weight coefficient, which means that every mineral has the same contribution to rock
brittleness. This lacks a sufficient scientific basis because there are apparent mechanical differences
for various minerals [22]. Third, this method does not take other affecting factors into account, such
as rock porosity and rock texture. In this formulation, the brittleness indices of rocks with the same
mineral composition but different porosity are consistent. This contradicts the fact that brittleness
decreases with increasing porosity [23]. Moreover, rock texture is primarily responsible for brittleness
characteristics, such as the laminar structure of shales and the fine-grained micritic textures of carbonate
rocks [17,24]. This implies that mineralogical compositions cannot solely be used to accurately estimate
rock brittleness.

2.3. Energy-Based Brittleness Indices Derived from Rock Stress-Strain Curves


The complete stress-strain curves of a rock sample under external loads show the deformation and
rupture characteristics of the sample. Figure 1 illustrates the internal micromechanical mechanisms
of rock deformation and failure behaviors under compression loading. The entire failure process
can be divided into five stages: (1) oa: Pre-existing micro-cracks and micro-pores close; this stage
is terminated at crack closure stress (σcc ). (2) ab: Linear elastic deformation of rock occurs with the
tangent modulus of Young’s modulus until the crack initiation stress (σci ) is reached. σci is the turning
point of the rock from elasticity to plasticity, also known as the yield point. (3) bc: Micro-cracks stably
propagate before crack damage stress (σcd ). (4) cd: Cracks propagate in an unstable manner until the
limit strength of the rock is reached at a stress level known as failure stress (σf ). (5) de: At the peak
stress (σf ), the rock is in an unsteady state with high energy. The internal cracked surfaces of the rock
intersect then form one or several macro-fracture surfaces. Subsequently, the rock mass slides along
the macro-fracture surfaces, and the bearing capacity of the sample rapidly decreases until reaching
the residual strength (σr ).
Energies 2020, 13, 388 4 of 22
Energies 2020, 13, x FOR PEER REVIEW 4 of 23

Figure 1. Typical compression stress-strain curve and associated deformation and failure characteristics
Figure 1. Typical compression stress-strain curve and associated deformation and failure
for brittle rocks. σcc : crack closure stress; σci : crack initiation stress; σcd : crack damage stress; σf : failure
characteristics for brittle rocks. σcc: crack closure stress; σci: crack initiation stress; σcd: crack damage
stress; σr : residual stress; εp : plastic strain; εcd : strain at crack damage threshold; εf : failure strain; εr :
stress; σf: failure stress; σr: residual stress; εp: plastic strain; εcd: strain at crack damage threshold; εf:
residual strain; E: Young’s modulus; H: hardening modulus and M: drop modulus (modified from [17]).
failure strain; εr: residual strain; E: Young’s modulus; H: hardening modulus and M: drop modulus
(modified
The processfromof[17]).
rock failure is essentially a balancing process of energy absorption and
release [17,25–29]. During the pre-peak stage, the rock undergoes elastic and plastic deformation.
The process of rock failure is essentially a balancing process of energy absorption and release
The total elastic energy (Wet) accumulated during elastic deformation increases the internal energy of
[17,25–29]. During the pre-peak stage, the rock undergoes elastic and plastic deformation. The total
rock. Also, plastic energy (Wp) dissipates during plastic deformation due to crack closure and frictional
elastic energy (Wet) accumulated during elastic deformation increases the internal energy of rock.
sliding. A more brittle rock can turn more the absorbed external energy into elastic energy instead
Also, plastic energy (Wp) dissipates during plastic deformation due to crack closure and frictional
of plastic energy, and the more elastic energy accumulated during loading favors rock rupture and
sliding. A more brittle rock can turn more the absorbed external energy into elastic energy instead of
fracture extension.
plastic energy, and the more elastic energy accumulated during loading favors rock rupture and
According to the characteristics of rock behavior in the post-peak region, the failure modes were
fracture extension.
classified into two types [30]. As Figure 2 illustrates, the negative drop modulus (M < 0) corresponds to
According to the characteristics of rock behavior in the post-peak region, the failure modes
Class I behavior, which means that additional energy is required to support rock failure as the amount
were classified into two types [30]. As Figure 2 illustrates, the negative drop modulus (M < 0)
of elastic energy from material is not sufficient. The positive drop modulus (M > 0) corresponds to
corresponds to Class I behavior, which means that additional energy is required to support rock
Class II behavior, which means that rock failure can be self-sustained and fully developed. The excess
failure as the amount of elastic energy from material is not sufficient. The positive drop modulus (M
energy (the yellow area in Figure 2) in Class II failure is consumed to overcome the confinement
> 0) corresponds to Class II behavior, which means that rock failure can be self-sustained and fully
pressure and transformed into the failure process dynamics [8]. Hydrocarbon-bearing reservoirs are
developed. The excess energy (the yellow area in Figure 2) in Class II failure is consumed to
generally characterized by Class I behavior; therefore, Class II behavior is not discussed in this research.
overcome the confinement pressure and transformed into the failure process dynamics [8].
Hydrocarbon-bearing reservoirs are generally characterized by Class I behavior; therefore, Class II
behavior is not discussed in this research.
Energies 2020, 13, 388 5 of 22
Energies 2020, 13, x FOR PEER REVIEW 5 of 23

Figure2.2.Post-peak
Figure Post-peak energy balance for rocks of class ⅠI and class
energy balance class Ⅱ, E: Young’s
II, E: Young’s modulus; M:drop
modulus; M: drop
modulus
modulus(modified
(modifiedfrom
from[8]).
[8]).

After
Afterthethepeak,
peak,thethe accumulated
accumulated elastic
elastic energy
energy isis gradually
gradually released
released to to form
formmacro-fractures.
macro-fractures.
However,
However,because
becauseofof thethe
plasticity of materials
plasticity of materialsandand
the effect of confining
the effect of confiningpressure, the elastic
pressure, energy
the elastic
stored before the peak is not enough for complete self-sustaining rock failure.
energy stored before the peak is not enough for complete self-sustaining rock failure. Therefore, Therefore, additional
energy (the blue
additional energy area in Figure
(the blue area2) provided
in Figure by 2) loading
providedis byneeded.
loadingCompared
is needed. toCompared
brittle rocks,
to ductile
brittle
rocks
rocks,require
ductilemore additional
rocks requireenergy
more to maintain energy
additional rupture.toAtmaintain
the end ofrupture.
the compression
At the endexperiment,
of the
there is still some
compression energy known
experiment, there asis the
stillresidual elastic energy
some energy known (Wer)
as the existing
residualin the rocks.
elastic energy (Wer)
Overall,
existing therocks.
in the stress-strain curves provide a comprehensive insight into rock deformation and brittle
failureOverall,
mechanisms under various
the stress-strain curves loading
provideconditions. Under certain
a comprehensive insight ambient conditions,
into rock deformationall ofand
the
internal factors affecting brittleness can be considered in this process. An accurate
brittle failure mechanisms under various loading conditions. Under certain ambient conditions, all brittleness evaluation
method based on
of the internal energy
factors balancebrittleness
affecting rule can becan obtained throughin
be considered analyzing the entire
this process. stress-strain
An accurate curve.
brittleness
The BI is defined
evaluation methodas follows
based on [17]:energy balance rule can be obtained through analyzing the entire
stress-strain curve. The BI is defined as follows [17]:
1 1 We We
BI = (BI1 + BI2 ) = ( + ), (4)
21 2 1WrWe Wet +We Wp (4)
BI = ( BI1 + BI 2 ) = ( + )
2 1
2 Wr Wet + Wp ,
Wet = σ2f , (5)
2E
1 1 2 (5)
We = WetWet ==
− Wer σ(σf 2,f − σ2r ),
2 E2E
(6)
Z εr
1 2
Wr = Wet + Wa − Wer = (1σ f − σ2r ) + σdε, (7)
(6)
σ σ
2 2
We = Wet − Wer =2E ( f − rε)f
Z 2ε fE
1 2 ,
Wp = Wt − Wet = σdε − σ , (8)
0 2E f
1 εr (7)
Wr = Wetof+the
The corresponding definitions Wacalculation
2E
(σ 2f − σ r2 )are
− Wer = parameters + presented
ε f

σ dε in Figure 1. We is the
, (Wet) and the residual
consumed elastic energy, which is the difference between the total elastic energy
elastic energy (Wer); Wt is the total consumed energy during the pre-peak stage; Wr represents the
εf 1 2 additional energy consumed (8)
rupture energy, which is the sum Wp = Wt
of the − Wet
total = energy
elastic

σdε −(Wet)σand
by rock failure from loading the system (the blue area0 in Figure2 E
f
1); and, Wp represents the dissipated
plastic energy during the pre-peak region.
The corresponding definitions of the calculation parameters are presented in Figure 1. We is the
In this model, BI1 determines the extent to which the fracturing process occurs in a self-sustaining
consumed elastic energy, which is the difference between the total elastic energy (Wet) and the
manner. BI2 represents the fraction of the total absorbed energy during the pre-peak region released in
residual elastic energy (Wer); Wt is the total consumed energy during the pre-peak stage; Wr
the post-peak rupture process. These two values vary in the range from 0 to 1. Accordingly, the value
represents the rupture energy, which is the sum of the total elastic energy (Wet) and additional
of BI changes continuously from 0 to 1, and the degree of brittleness transforms from full ductility to
energy consumed by rock failure from loading the system (the blue area in Figure 1); and Wp
absolute brittleness.
represents the dissipated plastic energy during the pre-peak region.
In this model, BI1 determines the extent to which the fracturing process occurs in a
3. Materials and Measurements
self-sustaining manner. BI2 represents the fraction of the total absorbed energy during the pre-peak
region
3.1. released in the post-peak rupture process. These two values vary in the range from 0 to 1.
Materials
Accordingly, the value of BI changes continuously from 0 to 1, and the degree of brittleness
Nine drill core samples from well SY3 underwent a series of laboratory tests (Figure 3). Two of
transforms from full ductility to absolute brittleness.
the samples are from the Upper Ordovician Baota Formation. The remaining seven are from
3. Materials and Measurements

3.1. Materials
Nine
Energies 2020,drill core
13, 388 samples from well SY3 underwent a series of laboratory tests (Figure 3). Two 6 of of
22
the samples are from the Upper Ordovician Baota Formation. The remaining seven are from the
Upper Ordovician Wufeng Formation and Lower Silurian Longmaxi Formation, which are
the Upper shale
important Ordovician Wufeng
gas-bearing Formation
layers and Lower
in the Sichuan BasinSilurian
and itsLongmaxi
peripheralFormation,
regions in which
southwestare
important shale gas-bearing layers in the Sichuan Basin and its peripheral regions
China. The paleogeographic settings of these formations in the study area have been reported in in southwest
China.
previousThe paleogeographic
works settings
[31,32]. Briefly, of thesemember
the upper formations in the
of the study
Baota area have
Formation been reported
mainly consists in of
previous works [31,32]. Briefly, the upper member of the Baota Formation
limestone with polygonal reticulate structures developed in a platform environment. Themainly consists of limestone
with polygonal reticulate
Wufeng-Longmaxi structures
Formation can bedeveloped
divided intointwo
a platform
sectionsenvironment. The Wufeng-Longmaxi
according to their sedimentary facies.
Formation
The Lowercan be divided
Member intoWufeng-Longmaxi
of the two sections according to their sedimentary
Formations is dominantly facies. The up
made Lower Member
of deep blackof
the Wufeng-Longmaxi Formations is dominantly made up of deep black siliceous
siliceous shale, carbonaceous shale, and gray-black shale [33], indicating a deep-water shelf shale, carbonaceous
shale, and gray-black
sedimentary shale [33],
environment. indicating
The primary a deep-water
lithology of theshelf
Upper sedimentary
Member ofenvironment.
the Longmaxi The primary
Formation
lithology of the Upper Member of the Longmaxi Formation is gray, silty mudstone,
is gray, silty mudstone, and argillaceous siltstone, deposited in a shallow-water shelf sedimentary and argillaceous
siltstone, deposited in a shallow-water shelf sedimentary environment.
environment.

Figure 3.
Figure Geological drilling
3. Geological drilling histograms of the Wufeng-Longmaxi Formations from well SY3.

3.2. Measurements
3.2. Measurements
Triaxial compression tests were used to evaluate the failure characteristics of the rock samples.
Triaxial compression tests were used to evaluate the failure characteristics of the rock samples.
The external loading can be described as follows:
The external loading can be described as follows:

σ11 == σσcc++σσa a; ;σ2σ=2 =σ3σ=3 =


σ σcσ
c
(9)

where σ1 , σ2 , σ3 are the principal stresses; σa is the axial deviatoric stress; σc is the confining stress.
A TAW-1000 stiff autonomous triaxial compression experimental machine (Aojin industry,
Guangdong, China) with a loading capacity of 1000 KN and a maximum confining pressure up
to 80 MPa is adopted as the testing apparatus. In this study, confining pressures of 30 MPa were
designated for simulating true in-situ stress, and cylindrical samples were cored to 25 mm in diameter
Energies 2020, 13, 388 7 of 22

and 60 mm in length. Defective rock samples caused during sample preparation were removed.
To avoid the influence of the bedding planes and loading rate on rock failure behavior, all specimens
were loaded at a strain rate of 0.12 mm/min, and bedding planes were perpendicular to the axis of
the cylinders.
After triaxial compression tests, the microstructures of the rock samples were also studied through
various analytical methods such as optical microscopy, scanning electron microscopy (SEM). Also,
the mineral compositions of the samples were determined by X-ray diffraction analysis (XRD), and the
specific method of XRD analysis was consistent with that in reference [34]. The experimental results
were shown in Table 1.

Table 1. Summary of measured compositional properties of tested samples. Qz (quartz), Fsp (feldspar),
Py (pyrite), Cb (carbonate minerals), TOC (total organic carbon).

Samples Formation Qz (wt%) Fsp (wt%) Cb (wt%) Clay (wt%) Py (wt%) TOC (wt%)
1 48.0 20.0 11.0 19.0 2.0 0.22
2 Longmaxi 30.0 10.0 40.0 16.0 4.0 1.92
3 45.0 16.0 4.0 30.0 5.0 1.65
4 62.0 16.0 2.0 18.0 2.0 2.27
5 72.0 9.0 5.0 14.0 0 1.75
Wufeng
6 53.0 13.0 16.0 17.0 1.0 6.48
7 75.0 2.0 4.0 19.0 0 2.31
8 15.6 3.8 71.2 9.4 0 0.34
Baota
9 17.8 4.3 75.7 2.2 0 1.02

4. Results

4.1. The Difference of Mechanism between Diverse Brittleness Indices


The energy-based brittleness indices derived from rock stress-strain curves of the rock samples
vary from 0.18 to 0.78 (Table 2). The post-peak curves of samples 1 and 4 sharply dropped from
the peak stress (σf ) to a low residual stress (σr ) (Figure 4). The residual elastic energy (Wer) and
post-peak fracture energy (Wr) of samples 1 and 4 are small, indicating that the total elastic energy
(Wet) accumulated in pre-peak stage is mostly used for the fracture of samples, and less additional
energy (Wa) is needed to maintain the fracture extension during the failure process. This type of rock is
conducive to the formation of fractures. Consequently, samples 1 and 4 have high brittleness indices of
0.63 and 0.78, respectively. The post-peak curves of samples 7 and 9 smoothly dropped from the peak
stress (σf ) to a high residual stress (σr ), and the residual elastic energy (Wer) and rupture energy (Wr)
are relatively large. This indicates that the consumed elastic energy (We) is insufficient to maintain
fractures propagation, and additional (Wa) is necessary, so this type of rock is hard to form fractures.
Therefore, samples 7 and 9 have low brittleness indices of 0.28 and 0.18, respectively.

4.2. The Effect of Confining Pressure on Brittleness


According to the classification method of brittle and plastic minerals proposed in [13], sample
3 has a large weight fraction of clay minerals (30%). Sample 8 has a significant weight fraction of
brittle minerals (17.8% quartz, 4.3% feldspar, 75.5% carbonate minerals) and low weight fraction of
clay minerals (2.2%). However, these two samples both exhibit obvious plastic deformation before the
peak, and the plastic energy of samples 3 and 8 are high, 147 and 98, respectively (Table 2). Hence, rock
plasticity is not only affected by clay mineral content but also high confining stress. This is consistent
with the well-established fact that rocks tend to show higher plastic characteristics at elevated confining
stresses [7,21].
In addition, the post-peak curves for all rock samples except for samples 1 and 4 slowly decreased
from the peak stress (σf ) to residual stress (σr ) (Figure 4). The applied confining pressure hinders the
Energies 2020, 13, 388 8 of 22

radial dilation followed by further blocking the development of the macrocracks during the post-peak
region, thus leading to decreased brittleness [35].

Table 2. Summary of mechanical parameters obtained from complete stress-strain curves of tested
samples. E (Young’s modulus), ν (Poisson’s ratio), σf (failure stress), σr (residual stress), Wet (total
elastic energy), Wer (residual elastic energy), We (consumed elastic energy), Wr (rupture energy), Wp
(plastic energy), Wa (additional energy), BI1 (We/Wr), BI2 (We/(Wet+Wp)), BI (brittleness index).
Energies 2020, Formation
Samples 13, x FOR PEER REVIEW
E (Gpa) ν σf (Mpa) σr (Mpa) Wet Wer We Wr Wp Wa BI1 BI2 BI8 of 23
1 22.4 0.21 123 60 31 7 23 33 12 9 0.72 0.55 0.63
2 Longmaxi
is consistent with the31.7
well-established
0.30 242 fact 150
that rocks
102 tend
39 to63show114 higher
0 plastic
51 characteristics
0.55 0.62 0.58 at
3 35.3 0.28 266 90 140 16 124 266 147 142 0.46 0.43 0.45
elevated confining stresses [7,21].
4 26.9 0.19 228 105 91 19 72 72 48 17 1.00 0.55 0.78
In
5 addition, the42.1post-peak
0.32 curves
262 for100all rock
52 samples
21 31 except
74 for0 samples
43 0.431 and
0.48 4 0.45
slowly
Wufeng
6 35.1 0.16 264 173 172 74 98 185 0 87 0.50 0.56
decreased from the peak stress (σf) to residual stress (σr) (Figure 4). The applied confining pressure 0.53
7 56.7 0.22 275 200 96 51 45 188 39 143 0.24 0.32 0.28
hinders the radial dilation followed by further blocking the development of the macrocracks during
8 37.8 0.23 244 170 61 30 31 73 98 41 0.43 0.19 0.31
the post-peakBaota
region, 55.5
thus leading to
9 0.23 269decreased
225 brittleness
74 54 [35].
20 182 0 162 0.10 0.26 0.18

Figure 4. Stress-strain curves of different samples under triaxial compression.


Figure 4. Stress-strain curves of different samples under triaxial compression.
5. Discussion
Table 2. Summary of mechanical parameters obtained from complete stress-strain curves of tested
5.1. Correlations
samples. E of Brittleness
(Young’s and Elastic
modulus), Parameters
ν (Poisson’s ratio), σf (failure stress), σr (residual stress), Wet (total
elastic energy), Wer (residual elastic energy), We (consumed elastic energy), Wr (rupture energy),
The brittleness index based on elastic parameters are calculated by Equation (1) and compared
Wp (plastic energy), Wa (additional energy), BI1(We/Wr), BI2 (We/(Wet+Wp)), BI (brittleness index).
with the energy-based brittleness indices derived from rock stress-strain curves. There is a negative
correlation between
Samples these Etwo
Formation (Gpa) ν of𝝈𝒇calculations
types (Mpa) 𝝈𝒓 (Mpa)
(Figure
Wet 5).
Wer In We
order
WrtoWp
explain
Wa BI this
1 phenomenon,
BI 2 BI
1
the relationship between the22.4 elastic
0.21 parameters
123 60
(Young’s31 modulus
7 23 33
and12Poisson’s
9 0.72 ratio)
0.55 0.63
and the
2 Longmaxi 31.7 0.30 242 150 102 39 63 114 0 51 0.55 0.62 0.58
energy-based
3
brittleness index
35.3
derived
0.28
from
266
rock stress-strain
90
curves are analyzed.
140 16 124 266 147 142 0.46 0.43 0.45
4 26.9 0.19 228 105 91 19 72 72 48 17 1.00 0.55 0.78
5 42.1 0.32 262 100 52 21 31 74 0 43 0.43 0.48 0.45
Wufeng
6 35.1 0.16 264 173 172 74 98 185 0 87 0.50 0.56 0.53
7 56.7 0.22 275 200 96 51 45 188 39 143 0.24 0.32 0.28
8 37.8 0.23 244 170 61 30 31 73 98 41 0.43 0.19 0.31
Baota
9 55.5 0.23 269 225 74 54 20 182 0 162 0.10 0.26 0.18
The brittleness index based on elastic parameters are calculated by Equation (1) and compared
with the energy-based brittleness indices derived from rock stress-strain curves. There is a negative
correlation between these two types of calculations (Figure 5). In order to explain this phenomenon,
the relationship between the elastic parameters (Young’s modulus and Poisson’s ratio) and the
Energies 2020, 13, 388 9 of 22
energy-based brittleness index derived from rock stress-strain curves are analyzed.

Figure 5.
Figure Comparison between
5. Comparison between the
the energy-based BI and
energy-based BI and elastic BI.
elastic BI.

The relationship
The relationshipbetween
betweenYoung’sYoung’s modulus
modulus and and
brittleness has been
brittleness has discussed by manybyscholars.
been discussed many
The brittleness evaluation method proposed in [10] supposes that a
scholars. The brittleness evaluation method proposed in [10] supposes that a higher Young’shigher Young’s modulus results in
a more brittle rock. In [33], it is believed that a formation with higher Young’s
modulus results in a more brittle rock. In [33], it is believed that a formation with higher Young’s modulus values induces
more microcracks,
modulus which shows
values induces moreamicrocracks,
strong brittlenesswhichinducing
showsa more complex
a strong hydraulic
brittleness fractureasystem.
inducing more
On the contrary, the paper [36] proposes that rocks with a high Young’s
complex hydraulic fracture system. On the contrary, the paper [36] proposes that rocks with a high modulus only create shorter
fracture apertures
Young’s modulusfor their
only limited
create deformation
shorter fractureability. In contrast,
apertures for their rocks with deformation
limited a low Young’sability.
modulus In
tend to form fractures with larger average apertures. This leads to
contrast, rocks with a low Young’s modulus tend to form fractures with larger average apertures. fracturing fluids penetrating
the fracture
This leads totips quickly,fluids
fracturing resulting in a greater
penetrating the fracture
fracture conductivity. The experimental
tips quickly, resulting in a greater datafracture
in this
study indicates that Young’s modulus is negatively correlated with
conductivity. The experimental data in this study indicates that Young’s modulus is negativelyenergy-based brittleness indices
(Figure 6a).with
correlated As shown in Figure
energy-based 6b, samples
brittleness 5, 7, 8,
indices and 9, 6a).
(Figure which Ashave
shown higher Young’s
in Figure 6b,modulus
samples values,
5, 7, 8,
consume less elastic energy (We). Specifically, the stored elastic
and 9, which have higher Young’s modulus values, consume less elastic energy (We). energy in rocks with higher Young’s
Specifically,
modulus
the storedvalues
elastic is not enough
energy in rockstowith self-sustain the development
higher Young’s of cracks,
modulus values leading
is not enough to to
theself-sustain
reduction
of the
the brittleness index.
development The relationship
of cracks, leading to the between the stress-strain
reduction curve and
of the brittleness Young’s
index. Themodulus also
relationship
further proves this conclusion (Figure 6c,d). Young’s modulus (E) of
between the stress-strain curve and Young’s modulus also further proves this conclusion (Figure the specimens tend to increase
with the
6c,d). increasing
Young’s moduluspeak(E)strength (σf ) (Figuretend
of the specimens 7), which is alsowith
to increase verified by others [37,38].
the increasing Therefore,
peak strength (σf)
(Figure 7), which is also verified by others [37,38]. Therefore, assuming other parametersstrength
assuming other parameters remain constant, an increase of Young’s modulus (E) and peak remain
(σf ) resultsan
constant, in decreased
increase oftheYoung’s
consumed elastic energy
modulus (E) and(the difference
peak strengthbetween total elastic
(σf) results energy (Wet)
in decreased the
and residual elastic energy (Wer)), and additional energy (the sum
consumed elastic energy (the difference between total elastic energy (Wet) and residual elasticof blue area and orange area as
shown in Figure 6c,d) is necessary to maintain the development of cracks.
energy (Wer)), and additional energy (the sum of blue area and orange area as shown in Figure 6c,d) This results in the decreased
brittleness
is necessaryofto the rocks. the development of cracks. This results in the decreased brittleness of the
maintain
rocks.
Energies 2020, 13, 388 10 of 22
Energies 2020, 13, x FOR PEER REVIEW 10 of 23
Energies 2020, 13, x FOR PEER REVIEW 10 of 23

Figure 6.6.The
The relationship between brittleness index and Young’s modulus. (a) A negative
Figure
Figure 6. Therelationship
relationship between brittleness
between indexindex
brittleness and Young’s modulus.modulus.
and Young’s (a) A negative
(a) Acorrelation
negative
correlation
of Young’s ofof Young’s
modulus modulus and energy-based BI;
BI; (b) Samples (b) Samples 5, 7, 8, and 9 with higher Young’s
correlation Young’sand energy-based
modulus and energy-based BI; (b)5,Samples
7, 8, and5,97,with higher
8, and 9 withYoung’s
highermodulus
Young’s
modulus less
consume consume less
elasticless elastic
energy (We,energy (We, the difference
the difference Wetbetween
and Wer); Wet andThe Wer); (c,d). The change of
modulus consume elastic energy (We, the between
difference between Wet(c,d).
and Wer); change
(c,d). of energy
The with
change of
energy with
the increase the increase of Young’s modulus and peak strength
(σf ). Wp (σ f ). Wp (plastic energy), Wet (total
Wet (total elastic energy),
energy with of
theYoung’s
increase modulus
of Young’sand modulus
peak strength
and peak (plastic
strength (σenergy),
f). Wp (plastic energy), Wet (total
elastic
Wer energy),
(residual Wer (residual
elastic energy). elastic energy).
elastic energy), Wer (residual elastic energy).

Figure
Figure 7. The relationship
7. The relationship between
between Young’s
Young’s modulus
modulus and
and peak
peak strength.
strength.
Figure 7. The relationship between Young’s modulus and peak strength.
The
The results
results do
do not
not indicate
indicate that
that all
all materials with aa lower
materials with lower Young’s
Young’s modulus
modulus areare more
more brittle.
brittle.
Themodulus
Young’s results do not indicate
measures a that
rock’s all materials
hardness rather with
than abrittleness,
lower Young’s
so modulus
materials withare moreYoung’s
higher brittle.
Young’s modulus measures a rock’s hardness rather than brittleness, so materials with higher
Young’s
modulus modulus measures
are difficult breakadownrock’ssimply
hardness rather than brittleness, so materials with needed,
higher
Young’s modulus are to
difficult to break downdue to
simply the higher
due to thefracture
higher initiation stress state
fracture initiation stress state
Young’s
for modulus
example, are difficult
diamond and to break
granite down
[39]. simply
On the other due to the higher fracture initiation stress state
needed, for example, diamond and granite [39]. Onhand, complicated
the other networks
hand, complicated of fractures
networksare of
needed, for example, diamond and granite [39]. On the other hand, complicated networks of
fractures are difficult to generate in materials with low Young’s modulus, such as rubber and wax.
fractures are difficult to generate in materials with low Young’s modulus, such as rubber and wax.
Energies 2020, 13, x FOR PEER REVIEW 11 of 23

Therefore, Young’s modulus should have a reasonable range of values for ideal brittle materials. The
relationship between Young’s modulus and brittleness can be determined by Equation. (10). When
Energies 2020, 13, 388 11 of 22
the energy absorbed per unit surface area attains its critical value (GC), fractures propagate along the
pre-existing fractures. Materials with lower Gc will generate more fractures, supposing the given
energy
difficultisto
kept constant.
generate The critical
in materials value
with low(Gc) is defined
Young’s below such
modulus, [13]: as rubber and wax. Therefore,
Young’s modulus should have a reasonable range of values for 2 ideal brittle materials. The relationship
2 (0.313 + 0.027 × E )
between Young’s modulus Gcand −ν )
= (1brittleness can be determined by3 Equation. (10). When the energy
× 10 (10)
E
absorbed per unit surface area attains its critical value (GC ), fractures propagate along the pre-existing
fractures.
WhenMaterials
Poisson’swith
ratiolower Gc willconstant,
(ν) remains generatethe
more fractures,
change supposing
in Young’s the can
modulus given energy
then is kept
analyze the
constant. Thebetween
relationship critical value
Gc and(Gc)E.isAs
defined below
Young’s [13]: increases, Gc first decreases then increases.
modulus
When Young’s modulus is 11.6 GPa, Gc has reached its minimum value. However, the value of
Young’s modulus is generally greater than (0.313
2 11.6 GPa + under E)2 stress
0.027 ×in-situ 3 for most sedimentary rocks
Gc = (1 − ν ) × 10 (10)
E
[13], hence rocks with a higher Young’s modulus are difficult to fracture.
Energy-based
When Poisson’s brittleness
ratio (ν) indices
remainsdoconstant,
not correlate with Poisson’s
the change in Young’sratio (Figure 8).
modulus canUnder triaxial
then analyze
compression, the applied confining pressure tends to hinder the radial dilation
the relationship between Gc and E. As Young’s modulus increases, Gc first decreases then increases. during the post-peak
region. Consequently,
When Young’s modulusmost Poisson’s
is 11.6 GPa, Gc ratio values its
has reached fluctuate
minimumin avalue.
small However,
range of 0.2 theto 0.3, of
value leading
Young’sto
the weak is
modulus correlation betweenthan
generally greater Poisson’s
11.6 GPa ratio andin-situ
under brittleness.
stress This observation
for most sedimentaryis also confirmed
rocks by
[13], hence
others [17,35].
rocks with a higher Young’s modulus are difficult to fracture.
Because the energy-based
Energy-based brittleness
brittleness indices index
do not of rockwith
correlate negatively correlates
Poisson’s with Young’s
ratio (Figure 8). Under modulus
triaxial
and weakly related to Poisson’s ratio, the brittleness index calculated by elastic
compression, the applied confining pressure tends to hinder the radial dilation during the post-peak parameters is vastly
different from the actual brittleness value, that is, the energy-based brittleness
region. Consequently, most Poisson’s ratio values fluctuate in a small range of 0.2 to 0.3, leading toindex in this study.
Therefore, the brittleness
the weak correlation betweenevaluation
Poisson’s method
ratio andbased on elastic
brittleness. Thisparameters
observation hasis severe theoretical
also confirmed by
defects that limit
others [17,35]. its application.

Figure 8. The relationship between brittleness index and Poisson’s ratio.


Figure 8. The relationship between brittleness index and Poisson’s ratio.
Because the energy-based brittleness index of rock negatively correlates with Young’s modulus
5.2.
andCorrelations
weakly relatedof Brittleness withratio,
to Poisson’s Mineral
theComposition
brittleness index calculated by elastic parameters is vastly
different
The from the actual
brittleness indexbrittleness
of samples value,
basedthat
on is, the energy-based
mineral compositionbrittleness indexfollowing
are calculated in this study.
the
Therefore, the brittleness
formula proposed by [13,40]: evaluation method based on elastic parameters has severe theoretical defects
that limit its application.
(
BI mi = WQz + WFsp + WCb + WPy / WTot
5.2. Correlations of Brittleness with Mineral Composition
) (11)

where BImi is the mineral BI and is dimensionless; WQz is the weight fraction of quartz, %; WFsp is the
weightThe brittleness
fraction index of
of feldspar, %;samples based
WCb is the on fraction
weight mineralofcomposition are calculated
carbonate minerals, %; WPyfollowing the
is the weight
formula of
fraction proposed
pyrite, %; byand
[13,40]:
WTot is the weight fraction of total minerals, %.
 
BImi = WQz + WFsp + WCb + WPy /WTot (11)
Energies 2020, 13, 388 12 of 22

where BImi is the mineral BI and is dimensionless; WQz is the weight fraction of quartz, %; WFsp is the
weight2020,
Energies fraction of feldspar,
13, x FOR %; WCb is the weight fraction of carbonate minerals, %; WPy is the 12
PEER REVIEW weight
of 23
fraction of pyrite, %; and WTot is the weight fraction of total minerals, %.
In this formula,
In this formula,quartz,
quartz, feldspar,
feldspar, carbonate
carbonate minerals,
minerals, and pyrite
and pyrite are regarded
are regarded as brittleas brittle
minerals,
minerals,
while clayswhile clays are
are regarded regarded
as plastic as plastic
minerals. For theminerals.
method basedFor onthemineral
method based on mineral
compositions, a higher
compositions,
content of brittle a higher
mineralscontent of brittle
and lower contentminerals
of plasticandminerals
lower content
leads toof plastic
a more minerals
brittle leads toBI).
rock (higher a
more brittle rock
The calculated (higherindices
brittleness BI). The calculated
attained from rock brittleness indices attained
mineral compositions from higher
are vastly rock mineral
than the
compositions
energy-basedare vastly higher
brittleness index than
(Figure the9).
energy-based
The mineralbrittleness index1,(Figure
BI of samples 9). The
2, 3, 4 and 6 aremineral BI of
in the range
samples 1, 2, with
of 0.70–0.84, 3, 4 anandaverage
6 are in of the
0.8. range of 0.70–0.84, brittleness
The energy-based with an average
indicesof of 0.8.
these Thefiveenergy-based
samples are
brittleness
in the rangeindices of these
of 0.45–0.78, five
with an samples
average of are0.6.
in Although
the rangethereof 0.45–0.78, with positive
is not a strong an average of 0.6.
correlation
Although there is not a strong positive correlation between these two calculations
between these two calculations for these five samples, generally speaking, the differences between for these five
samples,
these twogenerally speaking,
BI are still within the differencesrange.
a reasonable between Thethese
minor two BI are stillmay
difference within a reasonable
be influenced byrange.
other
The minor
factors, suchdifference may be the
as rock texture, influenced
contentby of other
organic factors,
mattersuch
andas rock texture,
porosity. the content
However, of organic
it is worth noting
matter
that theand porosity.
mineral BI ofHowever,
samples 5, it 7,
is 8,
worth
and 9noting that in
are high, thethe
mineral
range ofBI 0.81–0.98,
of sampleswith 5, 7,an8, average
and 9 are of
high, in the
0.89, but range
their of 0.81–0.98,
energy-based with an indices
brittleness averageare of low,
0.89, in
but their energy-based
a range brittleness
of 0.18–0.45, with an averageindices are
of 0.28.
low,
Thereinisaarange of 0.18–0.45,
considerable withbetween
difference an average the of
two0.28. There ismethods
calculation a considerable
for thesedifference
four samples between the
(marked
two
by acalculation
red dotted methods for these
line in Figure 9). four samples (marked by a red dotted line in Figure 9).

Figure 9.
Figure Comparisonbetween
9. Comparison betweenthe
theenergy-based BI and
energy-based BI and the
the mineral BI.
mineral BI.

The quartz
The quartz and
and carbonate
carbonatecontents
contentsin insamples
samples5,5,7,7,8,8,and and99are
arehigh,
high,exceeding
exceeding70%70%(Table
(Table2).
2).
The Young’s
The Young’smodulus
modulusofofthese thesefourfour samples
samples is also
is also relatively
relatively high,
high, withwith an average
an average of 48 of 48 This
GPa. GPa.
This indicates that they have a stronger cohesive strength. Based on
indicates that they have a stronger cohesive strength. Based on the SEM results (Figure 10), thethe SEM results (Figure 10),
the minerals in these four samples are tightly structured and cemented,
minerals in these four samples are tightly structured and cemented, and there are few weak and there are few weak
mechanical interfaces
mechanical interfaces in in these
these rocks
rocks (Figure
(Figure 10a).
10a). TheThe cracks
cracks that
that do
do exist
exist terminate
terminate into
into the
the uniform
uniform
and compact rock texture (Figure 10b). This indicates why the four
and compact rock texture (Figure 10b). This indicates why the four specimens are so hard to specimens are so hard to be
be
fractured, which is a result of their excessive amount of single brittle mineral
fractured, which is a result of their excessive amount of single brittle mineral (quartz or carbonate (quartz or carbonate
minerals). By
minerals). By contrast,
contrast, although
althoughthe thesample
sample 1, 1,
2, 4,
2, and 6 mainly
4, and consist
6 mainly of quartz,
consist the content
of quartz, of quartz
the content of
is less than 70%. In addition, appropriate content of various brittle minerals
quartz is less than 70%. In addition, appropriate content of various brittle minerals and clay minerals and clay minerals in
these
in four
these samples
four samples form many
form weak
many mechanical
weak mechanical planes existing
planes at theatboundaries
existing of different
the boundaries grains
of different
(Figure 10c). These weak structural surfaces are conducive to crack initiation,
grains (Figure 10c). These weak structural surfaces are conducive to crack initiation, then then the generated cracks
the
bypass mineral particles and extend to interact with other cracks, leading to
generated cracks bypass mineral particles and extend to interact with other cracks, leading to the the formation of a complex
network cracking
formation system network
of a complex (Figure 10d). Overall,
cracking systemthe excessive content
(Figure 10d). of quartz
Overall, the or carbonate
excessive minerals
content of
hinder fracture initiation and propagation.
quartz or carbonate minerals hinder fracture initiation and propagation.
Energies 2020, 13, 388 13 of 22
Energies 2020, 13, x FOR PEER REVIEW 13 of 23

Figure
Figure Microstructural
10.10. Microstructuralcharacteristics
characteristicsof of rock
rock samples
samples in in SEM.
SEM.(a)(a)Sample
Sample5 5mainly
mainly consists
consists of of
oneone
brittle mineral,
brittle mineral,andandthere
thereare
arefew
fewweak
weakstructural
structuralplanes;
planes;(b)
(b)A A crack
crack bypasses
bypasses aa particle
particle and
andextends
extends a
short distance
a short around
distance the grain,
around and then
the grain, and isthen
terminated due todue
is terminated the uniform and compact
to the uniform rock texture
and compact rock in
sample 5; (c)
texture Sample5;4 is
in sample (c)made
Sample up 4ofisappropriate
made up ofcontent of various
appropriate brittle
content minerals,
of various so there
brittle are many
minerals, so
weak structural
there are many planes
weakbetween different
structural planesmineral
between particles;
different(d)mineral
When the crack propagates,
particles; (d) When the it connects
crack
thepropagates,
weak structural surface
it connects theexisting along thesurface
weak structural edge ofexisting
the grains,
alongleading to of
the edge a longer distance
the grains, extension
leading to a
in sample 4.
longer distance extension in sample 4.

Because
Because an an
excessive amount
excessive of single
amount brittle brittle
of single minerals (quartz (quartz
minerals or carbonate minerals)minerals)
or carbonate diminishes
rock
diminishes rock brittleness, the relationship between the brittleness and various minerals carbonate
brittleness, the relationship between the brittleness and various minerals (quartz, (quartz,
minerals,
carbonate feldspar andfeldspar
minerals, clay minerals)
and clayare further are
minerals) analyzed. As FigureAs
further analyzed. 11aFigure
illustrates, when thewhen
11a illustrates, quartz
the quartz
content is lesscontent
than 70%,is less than brittleness
the rock 70%, the rock brittleness
increases increases
with the increasewith thequartz
of the increase of the However,
content. quartz
content.
when quartz However,
content is when quartz
greater thancontent is greater
70%, rock than 70%,
brittleness rock brittleness
suddenly decreases.suddenly decreases.
The variation The of
tendency
variation
Young’s tendency
modulus of a of Young’s
rock modulus quartz
with increasing of a rock with increasing
contents quartz
is the opposite ofcontents is the opposite
the brittleness index. Thisof is
the brittleness
consistent with the index. This
results is consistent
discussed with 5.1
in Section the (Figure
results 11b).
discussed in Section
In general, 5.1 (Figure
the content 11b). In
of terrigenous
general,(quartz,
minerals the content of terrigenous
feldspar, minerals in
and clay minerals) (quartz, feldspar,
sedimentary andisclay
rocks minerals)
positively in sedimentary
correlated with each
rocks is positively correlated with each other. Furthermore, the excessive
other. Furthermore, the excessive amount of quartz is mainly authigenic quartz (Figure amount of quartz is mainly
12a) [41],
andauthigenic
the content quartz (Figure 12a)
of authigenic [41],isand
quartz the content
unrelated to theofcontent
authigenic quartz is unrelated
of terrigenous mineralsto[42].the Therefore,
content
of terrigenous minerals [42]. Therefore, when the content of quartz is low (<20%), such as samples 8
when the content of quartz is low (<20%), such as samples 8 and 9 (Figure 12b), the content of other
and 9 (Figure 12b), the content of other terrigenous minerals (feldspar and clay minerals) are also
terrigenous minerals (feldspar and clay minerals) are also low. This indicates that the rock consists of
low. This indicates that the rock consists of carbonate minerals, and the compact texture of this type
carbonate minerals, and the compact texture of this type of rock leads to poor rock brittleness. When the
of rock leads to poor rock brittleness. When the quartz content is 20–70%, the existence of
quartz content is 20–70%, the existence of terrigenous quartz indicates that the rocks also contain a
terrigenous quartz indicates that the rocks also contain a moderate amount of other terrigenous
moderate amount of other terrigenous minerals (feldspar and clay) (Figure 12c), along with variable
minerals (feldspar and clay) (Figure 12c), along with variable amounts of carbonate minerals. In this
amounts
case, theofrock
carbonate
contains minerals.
many weak In this case, the
mechanical rock contains
structural surfaces,many
henceweak mechanical
brittleness structural
increases with
surfaces, hence brittleness increases with the increase of quartz content. When
the increase of quartz content. When quartz content exceeds 70% in rocks, such as samples 5 and quartz content exceeds
7
70% in rocks, such as samples 5 and 7 (Figure 12d), the excessive amount of quartz can enhance Young’s
modulus, leading to decreased rock brittleness.
Energies 2020, 13, x FOR PEER REVIEW 14 of 23
Energies 2020, 13, x FOR PEER REVIEW 14 of 23

(Figure
(Figure 12d),
12d), the
theexcessive
excessiveamount
amountofofquartz
quartzcan
canenhance
enhanceYoung’s
Young’smodulus,
modulus,leading
leadingtotodecreased
decreased
Energies 2020, 13, 388 14 of 22
rock brittleness.
rock brittleness.

Figure 11.
11.(a)
Figure11. (a)Relationship
Relationshipbetween
betweenenergy-based
energy-basedBI
BIand
andquartz
quartzcontent;
content;(b) Relationship
Relationshipbetween
(b)Relationship between
Figure (a) Relationship between energy-based BI and quartz content; (b) between
Young’s modulus
Young’smodulus and
modulusand quartz
andquartz content.
quartzcontent.
content.
Young’s

12. Microstructural characteristics


Figure 12.
Figure characteristics of rock samples
samples under an an optical microscope
microscope and SEM; SEM; Qz
Figure 12.Microstructural
Microstructural characteristicsofofrock rock samplesunderunder anoptical
optical microscopeand and SEM;Qz Qz
(quartz); Fsp
(quartz); Fsp (feldspar);
(feldspar); CbCb(carbonate
(carbonate minerals).
minerals).(a) Amount
(a) of authigenic
Amount of quartzquartz
authigenic developed in sample
developed in
(quartz); Fsp (feldspar); Cb (carbonate minerals). (a) Amount of authigenic quartz developed in
5; (b) Sample
sample 9 mainly9consists of carbonate minerals (75.7%), leading to high cohesion, and the rhombic
sample5;5;(b) (b)Sample
Sample 9mainly
mainlyconsists
consistsofofcarbonate
carbonateminerals
minerals(75.7%),
(75.7%),leading
leadingtotohigh
highcohesion,
cohesion,andand
cleavage
the rhombicof calcite is
cleavage visible; (c) Microstructural
ofofcalcite isisvisible; (c) characteristics
Microstructural of sample 3 in
characteristicsSEM, sample
ofofsample 3 is
33made up
ininSEM,
the rhombic cleavage calcite visible; (c) Microstructural characteristics
of the ideal content of various minerals (45% quartz, 16% feldspar, and 30% clay minerals), and the sample SEM,
sample
sample3of 3isismade
made up
upofofthe
theideal
idealcontent
content ofofvarious
various minerals (45%(45%quartz, 16% feldspar,
feldspar,and 30%
30%clay
amount weak mechanical structural surfaces in theminerals
rock is conducive quartz,
to the 16%
development and clay
of fractures.
minerals),
minerals), and the
and the amount of weak
amount ofamount mechanical
weak mechanical structural
structural surfaces
surfaces in the
in the rock is conducive
rocktoisform
conducive to the
to the
(d). Under SEM, an excessive of quartz (72%) in sample 5 makes it hard fractures.
development
developmentofoffractures.
fractures.(d).
(d).Under
UnderSEM,SEM,an anexcessive
excessiveamount
amountofofquartz
quartz(72%)
(72%)ininsample
sample55makes
makesitit
hard
As
hard totoform
Figureform13afractures.
illustrates, when the carbonate mineral content is low (<15%), there is no significant
fractures.
correlation between the brittleness index and carbonate mineral content. In this case, when the rocks
are mainly composed of quartz, they show poor brittleness, such as samples 5 and 7. By contrast, when
Energies 2020, 13, x FOR PEER REVIEW 15 of 23

As Figure 13a illustrates, when the carbonate mineral content is low (<15%), there is no
significant
Energies correlation
2020, 13, 388 between the brittleness index and carbonate mineral content. In this15case, of 22
when the rocks are mainly composed of quartz, they show poor brittleness, such as samples 5 and 7.
By contrast, when the quartz content of rocks is in an appropriate range of 20–70%, the rocks show
the
goodquartz contentsuch
brittleness, of rocks is in an 1appropriate
as samples range of2,20–70%,
and 4. For sample the rocks
the carbonate show content
mineral good brittleness,
was 40%,such
and
as samples 1 and 4. For sample 2, the carbonate mineral content was 40%, and rock brittleness
rock brittleness was 0.58, indicating that an appropriate amount of carbonate minerals benefit was rock
0.58,
indicating
brittleness.that
Foran appropriate
samples 8 andamount
9, whichof carbonate
both haveminerals benefit rock
a high content brittleness.
of carbonate For samples
minerals 8 and
(>70%), the
9, which both have a high content of carbonate minerals (>70%), the brittleness coefficients
brittleness coefficients suddenly decrease. Similarly, the Young’s modulus of samples 8 and 9 are suddenly
decrease. Similarly,
also relatively high the Young’s
(Figure 13b).modulus of samples 8 and 9 are also relatively high (Figure 13b).

13. (a) Relationship between energy-based


Figure 13. energy-based BI
BI and carbonate mineral content;
content; (b)
(b) Relationship
between Young’s
Young’s modulus
modulus and
andcarbonate
carbonateminerals
mineralscontent.
content.

Feldspar content is positively correlated with the energy-based brittleness brittleness index
index (Figure
(Figure 14).
14).
When
When the the content
content of of feldspar
feldspar is
is low
low (<10%),
(<10%), such as samples 5, 7, 8, and 9, because a large proportion
of feldspar is of terrigenous
terrigenous origin, the content of clay minerals from the same same terrigenous
terrigenous source is
also relatively low (Figure
(Figure 15).
15). This
Thisindicates
indicatesthat
thatthe
therock
rockcontains
contains anan excessive
excessive amount
amount of of quartz
quartz or
or carbonate
carbonate minerals,
minerals, resulting
resulting inin poorbrittleness
poor brittlenessofofthe
therock.
rock.With
Withthe
the increase
increase of feldspar content
(>10%),
(>10%), thethe content
contentofofterrigenous
terrigenous clay minerals
clay mineralsandand
quartz in rocks
quartz also also
in rocks increases. In this
increases. Incase,
this the rocks
case, the
are noare
rocks longer dominated
no longer by a single
dominated mineral,
by a single and many
mineral, weak weak
and many mechanical structural
mechanical surfaces
structural exist
surfaces
Energies 2020, 13, x FOR PEER REVIEW 16 of 23
between different
exist between mineralmineral
different boundaries in the rocks.
boundaries in theThis leads
rocks. to the
This enhancement
leads of rock brittleness.
to the enhancement of rock
brittleness.
As Figure 16 illustrates, when the clay mineral content is low (<20%), rock brittleness indices
increase with the increase of clay mineral content. It should be noted that this phenomenon is mainly
caused by the existence of quartz or carbonate minerals, instead of the increase of clay mineral
content. This variation tendency and its reasons are the same as that of feldspar. However, when the
content of clay minerals exceeds 20%, such as in sample 3, the brittleness suddenly decreases, which
indicates that clay minerals decrease the brittleness of rocks.
It is concluded that quartz can appropriately characterize the shale brittleness among all
minerals. Shale brittleness increases with the increase of quartz content, but an excessive amount of
quartz (> 70%) decreases shale brittleness.

Figure 14. The relationship between energy-based BI and feldspar content.


Figure 14. The relationship between energy-based BI and feldspar content.
Energies 2020, 13, 388 16 of 22
Figure 14. The relationship between energy-based BI and feldspar content.

Figure 14. The relationship between energy-based BI and feldspar content.

Figure 15. The relationship between the content of clay minerals and feldspar content.

As Figure 16 illustrates, when the clay mineral content is low (<20%), rock brittleness indices
increase with the increase of clay mineral content. It should be noted that this phenomenon is mainly
caused by the existence of quartz or carbonate minerals, instead of the increase of clay mineral content.
This variation tendency and its reasons are the same as that of feldspar. However, when the content of
clay minerals exceeds 20%, such as in sample 3, the brittleness suddenly decreases, which indicates
that clay minerals decrease
Figure 15. the brittleness
The relationship of the
between rocks.
content of clay minerals and feldspar content.

Figure 16. The relationship between energy-based BI and the content of clay minerals.

Figure 16. The


The relationship
relationship between energy-based BI and the content of clay minerals.

It is concluded that quartz can appropriately characterize the shale brittleness among all minerals.
Shale brittleness increases with the increase of quartz content, but an excessive amount of quartz
(>70%) decreases shale brittleness.

5.3. Correlation of Brittleness and Fracability


As research continues, some have argued that it is not enough to merely use the brittleness
index to select fracturing layers [15–17]. The ‘fracability index (FI)’ is a new term that can evaluate
the degree to which shale gas and oil reservoirs can be fractured [18]. In recent years, numerous
quantification methods for evaluating the fracability of unconventional oil and gas reservoirs have
been proposed [43–45]. In these methods, apart from BI, other main factors controlling fracability are
selected to calculate formation fracability, such as fracture toughness, diagenesis, natural crack density,
differential horizontal stress, and so on. However, it should be noted that there are several problems
As research continues, some have argued that it is not enough to merely use the brittleness
index to select fracturing layers [15–17]. The ‘fracability index (FI)’ is a new term that can evaluate
the degree to which shale gas and oil reservoirs can be fractured [18]. In recent years, numerous
quantification methods for evaluating the fracability of unconventional oil and gas reservoirs have
been proposed [43–45]. In these methods, apart from BI, other main factors controlling fracability are
Energies 2020, 13, 388 17 of 22
selected to calculate formation fracability, such as fracture toughness, diagenesis, natural crack
density, differential horizontal stress, and so on. However, it should be noted that there are several
problems
with thesewith these First,
methods. methods.the BIFirst, the BI
derived derived
from from rock
rock mineral mineral compositions
compositions or elastic
or elastic parameters
parameters
are utilized are utilized to
to calculate FIcalculate
in these FI in theseyet
methods, methods,
this hasyet thisproven
been has been to proven to be in
be incorrect incorrect
previous in
previous sections of this paper. Second, it is hard to develop an effective quantification
sections of this paper. Second, it is hard to develop an effective quantification method of fracability by method of
fracability selecting
randomly by randomly selecting theFormation
the parameters. parameters. Formation
fracability is afracability
complicated is a function
complicated function
of various rockof
various rock compositional,
compositional, textural, physical,textural, physical, and
and mechanical mechanical
properties underproperties under
specific in-situ specific in-situ
temperatures and
temperatures and pressures. Other dominant factors may be neglected in
pressures. Other dominant factors may be neglected in these methods. Third, these fracability-relatedthese methods. Third,
these fracability-related
factors are not independent factors are have
and can not independent
a similar impactand on
canfracturing
have a similar
behavior.impact on fracturing
For example, rock
behavior. For example, rock elastic parameters are closely correlated with the
elastic parameters are closely correlated with the mineral composition and subjected to in-situ stress. mineral composition
and subjected in
Consequently, to these
in-situ stress. Consequently,
methods, the effect of rockin mineral
these methods,
content on thefracability
effect of rock mineral content
is calculated on
repeatedly,
fracability
which is reasonable.
is not calculated repeatedly, which is not
Hence, to determine thereasonable.
correlationHence, to determine
of brittleness the correlation
and fracability, we need of
brittleness and fracability, we need to assess formation fracability on the premise
to assess formation fracability on the premise of evaluating the brittleness index scientifically, rather of evaluating the
brittleness
than randomly.index scientifically, rather than randomly.
It can
It can bebe stated
stated that
that scientific
scientific fracability
fracability evaluation
evaluation needs
needs to to comprehensively
comprehensively combinecombine all all
affecting factors according to rock failure mechanisms. Fracability is determined
affecting factors according to rock failure mechanisms. Fracability is determined by not only the by not only the
petrophysicalproperties
petrophysical properties of rock
of rock butgeological
but also also geological
conditions,conditions, including
including ambient ambient
pressure, pressure,
temperature,
and pre-existing (natural) fractures. The influence of petrophysical properties on fracability can on
temperature, and pre-existing (natural) fractures. The influence of petrophysical properties be
fracability by
expressed canenergy-based
be expressedBI,by energy-based
which BI, which
has been proven has in
correct beenthisproven
paper. correct
The nextinstep
thisispaper. The
to discuss
nextimpact
the step isof togeological
discuss theconditions
impact ofon geological conditions on fracability.
fracability.

5.3.1. In-Situ Earth Stresses


theprincipal
In the principal stress
stress of three
of three directions,
directions, the minimum
the minimum horizontal
horizontal stress (Shstress (Sh) is significant
) is extremely extremely
significant
when whenfracturing
designing designing fracturing
treatments [46].treatments
The simulated[46].fractures
The simulated
will growfractures will grow
perpendicular to Sh,
perpendicular
which urges theto induced
Sh, whichfracture
urges the induced
to close. In fracture
addition,toasclose.
the SInh increases,
addition, as thethe Sh increases,
rock failure modethe
rock failure
changes frommode
tensilechanges
failure tofrom
sheartensile
failure failure
(Figureto17),
shear failure
limiting the(Figure
vertical17), limiting
growth the vertical
of fractures [47].
growth of fractures
Therefore, [47]. Therefore,
for formations with higherforShformations with
, it is difficult for higher Sh,to
fractures it is difficult
extend for fractures
vertically to extend
to connect other
vertically to connect
pre-existing fracturesother
[48]. pre-existing fractures [48].

Figure 17. Influence of minimum horizontal stress (Sh ) on failure mode.


Figure 17. Influence of minimum horizontal stress (Sh) on failure mode.
The minimum horizontal stresses can be estimated using the following equation [49,50]:
The minimum horizontal stresses can be estimated using the following equation [49,50]:
ν Eνε
𝑆 = ××(S𝑆V −−αP
Sh = 𝛼𝑃P ) ++αP
𝛼𝑃P +
+ (12)
1−ν 1 − ν2
where ν is Poisson’s ratio; SV is the vertical stress, psi; α is the Biot’s constant and is a dimensionless
where ν is Poisson’s ratio; SV is the vertical stress, psi; α is the Biot’s constant and is a dimensionless
value; 𝜀 is the tectonic strain parameter, psi; PP is pore pressure, psi.
value; ε is the tectonic strain parameter, psi; PP is pore pressure, psi.

5.3.2. Temperature Effects


Due to thermally activated deformation mechanisms, for instance, the dislocation slide of clay
minerals, temperature influences the brittleness of shales. Typically, shales show a transition from
brittle to more ductile only when temperature increases by several tens of degrees [3,20]. However,
the vertical thickness of the target interval in a region is typically not large enough (<100 m). Assuming
a geothermal gradient of 25 ◦ C/km (uncertainty <30%), temperature varies only slightly in the objective
Energies 2020, 13, 388 18 of 22

layers, which yields no significant change of rock mechanics. Accordingly, the effect of temperature on
formation fracturing can be neglected.

5.3.3. Natural Fractures


During hydraulic fracturing treatment, natural fractures can facilitate the leakage of fracturing
fluid into reservoirs to generate complex hydraulic fractures network, constituting the high-speed path
of shale gas output [51,52]. Therefore, to some extent, formations with denser natural fractures are
equivalent to a higher fracability. Natural cracks are not taken into consideration in the fracability
quantification model in this study. That does not mean that pre-existing fractures are neglected during
the process of hydraulic fracturing; rather, formations with denser natural fractures are considered
separately. The reasons are as follows. First, the crack density and its effect on fracability is extremely
difficult to be quantitatively evaluated [13,53]. Second, fractured strata can be detected by engineering
techniques, such as tiltmeters, well logging, and micro-seismic events. These formations should not
simply be considered as good fractured layers but should be judged whether they intersect aquifer
formations and faults to prevent the upward migration of shale gas. Third, under the same crustal
stress state, brittle rocks may contain more abundant fractures compared to ductile rocks [54]. In the
history of structural geology, if there is no substantial difference in the tectonic stress between different
strata, the degree of fracture development depends on the brittleness characteristic of the rock. In this
regard, to some extent, the brittleness of the rock represents the degree of development of natural
fractures. Overall, natural cracks are no longer considered as a separate factor in our analysis.
In conclusion, the energy-based brittleness index derived from stress-strain curves and minimum
horizontal stress are the essential parameters for fracability. Therefore, a new method of fracability
evaluation is proposed as follows:
BIn + Sh_n
FI = , (13)
2
BI − BImin
BIn = , (14)
BImax − BImin
Sh_max − Sh
Sh_n = , (15)
Sh_max − Sh_min
where BIn and Sh_n are normalized brittleness and normalized minimum horizontal stresses. Max and
min are the maximum and minimum values of corresponding variables for the investigated
formation, respectively.
FI is in the range of 0 to 1.0. A formation with FI = 1.0 is the best candidate for hydraulic fracturing,
and a formation with FI = 0 is the worst candidate for hydraulic fracturing. In this framework,
the most suitable fracturing layers possess a high brittleness index and low minimum horizontal stress.
The formation with lower BI and higher Sh compared to the adjacent formations is regarded as a
fracture barrier. The main purpose of fracture design is not only the detection of potential layers but
also fracture barriers [47]. Fracture barriers not only limit the vertical growth of hydraulic fractures
but can also prohibit hydraulic fractures from invading water-bearing layers or fault zones.
The minimum horizontal stress and fracability index of the formations in which the nine samples
located are calculated and summarized in Table 3. Additionally, according to the formula for Sh
(Equation (12)), the minimum horizontal stress increases with the increased Poisson’s ratio which
ranges between 0.1 and 0.45. The Poisson’s ratio of the nine samples are positively correlated
with the minimum horizontal stress of the formations in which the samples are located (Figure 18).
Small fluctuation in Poisson’s ratio can also cause substantial changes in the minimum horizontal
stress. Therefore, Poisson’s ratio indirectly affects the fracability through controlling the minimum
horizontal stress, and the fracability index decreases with an increasing Poisson’s ratio (Figure 19).
for Sh (Equation (12)), the minimum horizontal stress increases with the increased Poisson’s ratio
which ranges between 0.1 and 0.45. The Poisson’s ratio of the nine samples are positively correlated
which ranges between 0.1 and 0.45. The Poisson’s ratio of the nine samples are positively correlated
with the minimum horizontal stress of the formations in which the samples are located (Figure 18).
with the minimum horizontal stress of the formations in which the samples are located (Figure 18).
Small fluctuation in Poisson’s ratio can also cause substantial changes in the minimum horizontal
Small fluctuation in Poisson’s ratio can also cause substantial changes in the minimum horizontal
stress. Therefore, Poisson’s ratio indirectly affects the fracability through controlling the minimum
stress. Therefore,
Energies 2020, Poisson’s ratio indirectly affects the fracability through controlling the minimum
13, 388 and
horizontal stress, the fracability index decreases with an increasing Poisson’s ratio (Figure19 of 22
19).
horizontal stress, and the fracability index decreases with an increasing Poisson’s ratio (Figure 19).
Table 3. The value of Sh and fracability index of nine samples.
Table 3.
Table The value
3. The value of Shh and
of S and fracability
fracability index
index of
of nine
nine samples.
samples.
Sample Sh (Mpa) Sh_n BI BIn FI
Sample
Sample SShh (Mpa) SSh_n
h_n BI BIn FI
FI
1 23 0.72 0.63 0.76n 0.74
11
2
23
23
36
0.72
0.72
0.32
0.63
0.63
0.58
0.76
0.76
0.67
0.74
0.74
0.50
22
3
36
36
32
0.32
0.32
0.43
0.58
0.58
0.45
0.67
0.67
0.45
0.50
0.50
0.44
33
4
32
21
0.43
0.79
0.45
0.78
0.45
0.45
1.00
0.44
0.44
0.89
44
5 21
46 0.79
0.00
0.78
0.45
1.00
1.00
0.45
0.89
0.89
0.22
55 46 0.00 0.45 0.45
0.45 0.22
0.22
6 14 0.99 0.53 0.58 0.79
66 14 0.99 0.53 0.58
0.58 0.79
0.79
7 24 0.68 0.28 0.17 0.42
77 24
24 0.68
0.68 0.28
0.28 0.17
0.17 0.42
0.42
88
8
28
28
28
0.56
0.56
0.56
0.31
0.31
0.31
0.22
0.22
0.22
0.39
0.39
0.39
99
9
32
32
32
0.45
0.45
0.45
0.18
0.18
0.18
0.00
0.00
0.00
0.22
0.22
0.22

Figure 18. The relationship between minimum horizontal stress and Poisson’s ratio.
Figure 18.
Figure The relationship
18. The relationship between
between minimum
minimum horizontal
horizontal stress and Poisson’s ratio.

Figure 19.
Figure The relationship
19. The relationship between
between fracability
fracability index
index and
and Poisson’s
Poisson’s ratio.
ratio.
Figure 19. The relationship between fracability index and Poisson’s ratio.
6. Conclusions
The following conclusions are drawn from this study:
• The brittleness index assessment methods based on rock elastic parameters and mineral
compositions lack a scientific theory basis. The brittleness index derived from stress-strain
curves according to energy conservation law is reliable because it can comprehensively reflect the
deformation and rupture characteristic of rock.
• For rocks with a higher Young’s modulus, the consumed elastic energy (We) is insufficient to
generate a complex fracture network, leading to the reduced rock brittleness index. Because the
Energies 2020, 13, 388 20 of 22

surrounding stress limits the radial dilation of rocks, there are weak correlations between Poisson’s
ratio and brittleness.
• When a rock is composed of a variety of brittle minerals of moderate content, many weak structural
planes exist between different mineral particles, which contributes to the development of cracks.
Therefore, this type of rock is more brittle. By contrast, rocks which mainly consist of excessive
amount of quartz or carbonate minerals are characterized by high cohesiveness. There are few
weak structural planes in this type of rock, which leads to poor brittleness.
• The premise of fracability evaluation is to accurately assess rock brittleness. Apart from the
brittleness index, the minimum horizontal principal stress should also be regarded as an essential
parameter in selecting potential fracturing layers. The most suitable fracturing layers possess a
high brittleness index and low minimum horizontal stress. Poisson’s ratio positively correlates
with the minimum horizontal stress. Therefore, with the increased Poisson’s ratio, the minimum
horizontal stress increases, resulting in a reduced fracability index.

Author Contributions: Y.Y. conceived and designed the experiments; Y.Y. and Z.X. performed the experiments;
Y.Y. wrote the paper; S.T. and Z.X. revised the paper. All authors have read and agreed to the published version of
the manuscript.
Funding: The authors would like to thank National Science and Technology Major Project of China (grant
no. 2017ZX05035) and Project funded by China Postdoctoral Science Foundation (grant no. 2019M660737).
Acknowledgments: The authors gratefully acknowledge the China National Administration of Coal Geology for
sample support and their permission to publish the results of this study. We also greatly thank the anonymous
reviewers and editors for their critical comments and valuable suggestions, which were very helpful to improve
the manuscript.
Conflicts of Interest: The authors declare no conflict of interest.

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