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Investigating Shale-Fluid Interactions and Its Effect on Proppant Embedment

Using NMR Techniques

Conference Paper · June 2021

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Ekrem Alagoz Mukul Sharma

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ARMA 21–1129

Investigating Shale-Fluid Interactions and Its Effect on Proppant

Embedment Using NMR techniques
Ekrem Alagoz
The University of Texas at Austin, Austin, TX, USA
Mukul M. Sharma
The University of Texas at Austin, Austin, TX, USA

Copyright 2021 ARMA, American Rock Mechanics Association

th
This paper was prepared for presentation at the 55 US Rock Mechanics/Geomechanics Symposium held in Houston, Texas, USA, 20-23 June
2021. This paper was selected for presentation at the symposium by an ARMA Technical Program Committee based on a technical and critical
review of the paper by a minimum of two technical reviewers. The material, as presented, does not necessarily reflect any position of ARMA, its
officers, or members. Electronic reproduction, distribution, or storage of any part of this paper for commercial purposes without the written
consent of ARMA is prohibited. Permission to reproduce in print is restricted to an abstract of not more than 200 words; illustrations may not be
copied. The abstract must contain conspicuous acknowledgement of where and by whom the paper was presented.

ABSTRACT: It is essential to know about any adverse interactions between a shale and fracturing fluid additives. Some frac fluids
can alter shale rock petrophysical properties and this can lead to shale softening and fines generation. The softer the shale, the more
proppant embedment will occur, and the more severe the reduction in fracture conductivity as the effective stress increases. In this
study, we present a Nuclear Magnetic Resonance (NMR) technique to evaluate various frac fluids. We show that the extent of
proppant embedment correlates very well with the extent of imbibition of water into the shale (as measured by NMR). For example,
our test results show that Surfactant#7 and a clay inhibitor with KCl significantly reduced water imbibition into the shale. These
chemicals also showed the least embedment. The primary reason for this reduction is due to a decrease in rock plastic deformation.
The effect of shale mineralogy was also studied in this work using X-ray fluorescence. The results show that water imbibition into a
shale is also sensitive to its mineralogy. The higher the clay content, the more the imbibition and embedment. This correlation
between NMR-measured imbibition and proppant embedment can be used to evaluate the impact of different fracturing fluids on
proppant embedment. Such tests will significantly simplify the testing of different frac fluid additives for compatibility with shales.

fracture closure and limits the hydrocarbon production

1. INTRODUCTION
severely.
Unconventional reservoir development has changed the
Several factors control the embedment, including rock
oil and gas industry in extraordinarily profound ways in
elastic, plastic, and creep deformations (Alagoz et al.,
a very short time. The term unconventional reservoir is
2020), shale rock mineralogy (Alagoz et al., 2020;
used here to denote reservoirs whose permeability is in
Alramahi and Sundberg, 2012; Wu, W., 2017), and
the micro to nano-Darcy range (million times smaller
formation hardness (Volk et al., 1981). In this paper, we
than conventional reservoirs). The main challenge in
study the impact of fracturing fluid composition and
developing these reservoirs is the low recovery factor
imbibition on the extent of embedment using NMR T2
and rapid depletion. Therefore, hydrocarbons can only
distributions.
be produced through horizontal drilling and multi-stage
hydraulic fracturing. With horizontal drilling, more
stimulated reservoir volume is exposed, and the reservoir 2. METHODOLOGY
drainage area expands.
Alagoz [2] conducted experiments on Utica shale
Hydrocarbon flow paths are opened into the well with samples to study proppant embedment mechanisms. He
hydraulic fracturing. The process starts with fracturing presented two experimental setups to analyze shale rock
fluid injection into the well. A proppant slurry is then deformation. Figures 1 and 2 illustrate these
injected into the well to place the proppant between the experimental instruments. The extent of proppant
created fracture surfaces to keep them open and maintain embedment was measured using these methods. Later,
hydrocarbon flow. When the fractures begin to close, the the same shale samples were used to measure the extent
proppant grains are exposed to a high confining stress. of imbibition using NMR scans. Experimental
As the closure pressure increase, the proppants embed procedures are discussed in Section 2.2
into the fracture faces. This embedment results in

Fig. 1. An AutoCAD view of load-controlled test, not to scale
(Alagoz, 2020)
A constant load experimental apparatus was designed for
the load-controlled tests. In these tests, all three–elastic,
plastic, and creep–deformations of the shale are
measured. Figure 1 shows a schematic of the load-
controlled test; the test's main element is a simple Class
2 lever that pushes the proppant into the shale with
weights and leverage. This lever configuration also has a
geometric advantage that allows for precision
measurement since the lever arm's far point moves ten
times the distance as the proppant load. An electronic
device (electrical digital indicator) is used as a
displacement measurement of the shale sample during
tests. A microcomputer (a raspberry pi) controls the data
acquisition and recording. It tells the displacement gauge
to send out a measurement at set time intervals. For all
tests, this time interval was set as 2 seconds. The
raspberry pi records the data and timestamps every entry
for later analysis.
Fig. 2. An AutoCAD view of displacement-controlled test, not
to scale (Alagoz, 2020)
The displacement controlled apparatus was built to
quantify elastic and plastic deformations separately.
Time dependent rock deformation, which refers to creep,
proved to be negligible since this set up was designed for
quick tests that usually lasted less than a minute. Figure
2 shows a schematic of the displacement-controlled test;
the main element is a high precision screw with 80
threads per inch, which is twice as accurate as a
micrometer. Each degree of rotation of the screw
translates to less than 0.0009 millimeters of linear
motion. An indicator pin attached to the precision screw
projects radially out to a position just above a printed
protractor; this allows for precise angular positions are
obtained. A precision load cell is located underneath the
shale sample to measure transmitted load through the
shale. With the combination of displacement and load
data, elastic-plastic load curves are relatively easy to
generate.
2.1. Nuclear Magnetic Resonance(NMR) Theory
and Interpretation
Nuclear Magnetic Resonance(NMR) is a technique
which has been used in the oil and gas industry for a
variety of applications, including measuring porosity,
and fluid saturations in the formation. T1 and T2 are the
most common proton relaxation time measurements.
Proton-NMR measurements are designed to be sensitive
to fluids containing hydrogen atoms (Coates et al.,
1999). In this study, we used T2 measurements as these
scans are faster and easier to perform than many of the
other NMR measurements.
The process of proton relaxation involves surface, bulk,
and diffusion relaxation. The following equation gives
the T2 relaxation(Dunn et al., 2002).
1 1 1 1
  
T2 T2, Surface T2, Diffu si on T2, Bulk (1)
Fig. 3. An example of NMR T2 Measurements (Mulkay, 2019)
For most NMR results, two distinct peaks are observed.
The first peak on the left is usually the T2 relaxation time
between 0.1 and 1 ms., the second peak on the right at a
T2 relaxation time between 10 and 30 ms if from the
water in the pore space. The first peak gives information
about clay-bound water, while the second peak shows
water in inter-granular pores. T2 relaxation times are
greater in large pores and lower in smaller pores. For
that reason, the X-axis on the NMR scan can be thought
of as representing pore sizes as well. The higher peak
magnitudes indicate more fluid volume. In other words,
when the fracturing fluid imbibition increases, NMR
measurement gives a higher peak, as illustrated in Figure
4.
Fig. 4. NMR signal interpretation
2.2. Experimental Procedure
After the embedment test is performed, Utica Shale
samples are crushed to 5-10 mesh particle size. Then the
shale pieces are oven-dried and vacuumed at 200 oF for
24 hours to eliminate any residual fluid saturation. This
shale sample preparation is demonstrated in Figure 5.
Fig. 5. Shale sample preparation
Before the shale samples are exposed to any fracturing
fluid, the samples are scanned with a portable XRF
device to obtain their mineralogy. Figure 6 shows the
XRF device and its components.
Fig. 6. X-Ray fluorescence spectrometer (Alagoz, 2020)
XRF scanning gives us the element distribution of a
shale sample. An example XRF scanning data set is
plotted in Figure 7. Every element has a designated
channel number, shown on the X-axis, and the intensity
shows the quantity of the elements in that particular
channel.
The relative abundance of minerals was scaled to the
average element concentrations measured, and clay
content estimates were made by making the following
assumptions:
1) Aluminum (Al) is found only in clay.
2) Clay consists of 1:1 and 2:1 clay minerals only.
3) The fraction of the aluminum is equal in both
kaolinite and illite.
4) Calcium (Ca) is attributed to calcite and
dolomite.
More detailed calculation steps and equations can be
found in Appendix F of Alagoz [2].
Fig. 7. A data example of X-Ray fluorescence scanning
After XRF scanning, the samples are grouped based on
their relative mineralogy before soaking in a fracturing
fluid. Then, different fracturing fluid combinations were
prepared in the beakers, and 15 g of shale particles added
to beakers. A list of the fracturing fluids are shown in
Table 1. Shales were allowed to imbibe the fluids at
atmospheric pressure for three days. Determination of We observed interesting observations in the second
imbibition time was made based exposure time peak. Firstly, effective pore spaces are filled in the first
experiments conducted in the past and explained in hour, and then the amount of fluid starts to decrease. It is
Section 3.1. The shale particles were then removed from thought that the mechanism responsible for this process
the fluid after imbibition and placed in a fume hood for is that DI water imbibes into matrix quicker than the
20 mins to eliminate the surface fluids. As a final step, effective pore spaces because the matrix pores are larger.
NMR T2 scans were run to obtain the results. While balancing the amount of water in the matrix and
the pores, the change occurs in the second peak.
Table 1. Shale samples exposed to the following chemicals
(Alagoz et al., 2020)
3.2. Effect of Shale Mineralogy
Chemicals Name Fraction
There has been a lot of research done on shale
DI Deionized water Base fluid
mineralogy and rock-fluid interactions (Alotaibi et al.,
KCl Potassium Chloride 3%
2011; Chen et al., 2014). Wu [10] reported that
FR1 Friction Reducer#1 0.1%
FR2 Friction Reducer#2 0.1%
mineralogy strongly affects shale rock mechanical
Cl Clay Inhibitor 0.1% properties. Figure 9 shows that shale rocks do not reach
S7 Surfactant#7 0.1% the same fracture conductivity value after releasing the
S8 Surfactant#8 0.1% stress because rocks do not deform elastically. In
addition, samples with less clay content give higher
fracture conductivity.
3. RESULTS AND DISCUSSION
The main results from our experiments are summarized
in this section.
3.1. Time Dependence
Mulkay [8] and Zeng et al., [11] researched shale
imbibition, and both papers show that most of the shale
imbibition occurred in the first three days. Figure 8
illustrates the imbibition process of Eagle Ford shale
sample. Six Eagle Ford shale sample prepared and
soaked in DI water for various time periods before NMR
scanning. As can be seen in Figure 8, most of the fluid
imbibition occurred in the first hour of the process. After
one week, the amount of imbibed fluid is almost the
same as after three days of soaking. For this reason,
three days soaking time was selected for the entire test
matrix.
Fig. 9. Fracture Conductivity vs Closure Pressure Eagle Ford
shale sample (Wu, 2017)

Alagoz et al. [1] conducted a proppant embedment study

that clearly showed that shale embedment is dominated
by plastic deformation and creep (time-dependent)
deformation. They also showed that high clay shale
samples experience more deformation and more
embedment, as shown in Figure 10 and 11.

Fig. 8. Time dependency of shale imbibition(Mulkay, 2019)


Fig. 10. Utica shale mineralogy (Alagoz et al. 2020)
Fig. 11. Utica shale embedment results (Alagoz et al. 2020)
In the light of these previous studies, shale samples with
various clay content were soaked in DI water and
scanned with an NMR machine. The results confirm that
the presence of clay minerals increases the fluid
imbibition into the rock. More liquid imbibition results
in a softer shale and ultimately more severe proppant
embedment. Figure 12 shows this correlation clearly.
Fig. 12. Utica Shale NMR results for Utica shales with
different clay content.
In high clay content shale, DI water showed a more
significant increase, and in low clay content shale, DI
water gives a smaller amount of imbibition.
3.3. Effect of Fracturing Fluid
Various fracturing fluids were tested with Utica Shale
samples and those fracturing fluid additives listed in
Table 1. As shown in Figure 13, dry samples are at the
bottom of the plot while the shale imbibes DI water
more than 3% KCl. Adding KCl in the solution reduces
the imbibition, and this behavior also seen in the
embedment tests.
Fig. 13. Utica Shale NMR results.
In Figure 14, NMR results for a combination of various
chemicals with DI water are shown. DI water already
has a high tendency to imbibe into shale. Adding a clay
inhibitor reduces the imbibition; however, KCl shows
the least amount of imbibition.,The proppant embedment
tests show the same trend: 3% KCl in DI water shows
the least embedment, as shown in Figure 15. The reason
for this reduction is that the addition of KCl reduces
plastic and creep deformation more than other fracturing
fluid additives.
Fig. 14. Utica Shale NMR results with different fracturing
fluids.
 Fig. 17. Deformation results with fracking fluids with
Fig. 15. Deformation results with fracking fluids in deionized Surfactant#7 (Alagoz et al. 2020)
water with additives (Alagoz et al. 2020)
Addition of KCl into the surfactant-based brine fluid
Surfactant-based fracturing fluids were also studied in
also provided good protection for the shale i.e. less
this study; all the solutions started with a (0.1% S7 in DI
imbibition in the NMR tests and less embedment in the
water) composition to which other frac-fluid chemicals
embedment tests. Another interesting observation here is
were added. The results of these tests are shown in
that FR1 reduced the imbibition in the S7 plus DI water;
Figure 16: the blue line represents shale imbibition in the
however, the same FR1 additives increased the
samples soaked with the S7 base fluid. The addition of
imbibition when KCl is present in the solution, as shown
clay inhibitor to the S7 solution (black line) yielded the
in Figure 18. On the other hand, while the effect of FR1
best result, followed by the S7 plus FR2 solution.
in the embedment test is small, CI gives the most
reduction in the amount of embedment.

Fig. 16. Utica Shale NMR results.

Fig. 18. Utica Shale NMR results.
As noted, the dominant modes of shale deformation
during embedment are plasticity and creep, and the
addition of clay inhibitor to the fluid dramatically
reduced the plastic deformation. Figure 17 shows the
embedment results for these fluids and the trend agreed
very well with the NMR imbibition results.

Fig. 19. Preserved Utica shale sample deformation (Alagoz et
al. 2020)
4. CONCLUSIONS
The main findings of this research work are:
 We have developed and used new constant
displacement and constant load experiments to
measure the extent of proppant embedment caused
by elastic, plastic and creep deformation.
 We have shown clearly that exposure of shales to
fracturing fluids affects plastic deformation and
creep more than elastic deformation.
 Higher clay content in the shale sample leads to an
increase in fluid imbibition and results in softer
shale samples and more embedment.
 Chemical additives such as S7 + KCI + CI in
deionized water can mitigate the imbibition tendency
of the shale sample and reduce embedment
 NMR T2 scans can be used to quickly evaluate the
impact of different frac fluids on proppant
embedment in shales with different clay content.
Society of Petroleum Engineers. doi:10.2118/129972-
MS
4. Alramahi, B., & Sundberg, M.I. 2012. Proppant
embedment and conductivity of hydraulic fractures in
shales. American Rock Mechanics Association.
5. Chen, L., Zhang, G., Wang, L., Wu, W. and Ge, J.
2014. Zeta potential of limestone in a large range of
salinity. Colloids and Surfaces A: Physicochemical and
Engineering Aspects, 450:1-8.
6. Coates, G.R., Xiao, R., Prammer, M.G. 1999. NMR
Logging Principles and Applications. Halliburton
Energy Services, Houston, Texas.
7. Dunn, K.J., Bergman, D.J., LaTorraca, G.A. 2002.
Nuclear Magnetic Resonance Petrophysical and
Logging Applications. Elsevier Science Ltd., UK.
8. Mulkay, C.D. 2019. Investigating the Utilization of
Surfactant in Liquid Unloading Experiments of a
Propped Fracture. MS Thesis, The University of Texas
at Austin.
9. Volk, L.J., J.R. Clarence, B.C. Herbert, and S.S. Judy.
1981. Embedment of High Strength Proppant into Low-
Permeability Reservoir Rock. Paper SPE/DOE 9867.
10. Wu, W. 2017. Unpropped Fractures in Shales: Surface
Topography, Mechanical Properties and Hydraulic
Conductivity. PhD Dissertations, The University of
Texas at Austin.
11. Zeng, T., Miller, C.S., & Mohanty, K. 2018.
Application of Surfactants in Shales Chemical EOR at
High Temperatures. Society of Petroleum Engineers.

ACKNOWLEDGMENTS
The authors would like to thank The University of Texas
at Austin for the opportunity to publish this paper and
acknowledge BP for providing funding for this work and
the Utica Shale samples.

REFERENCES

1. Alagoz, E., Wang, H., Russell, R.T., and Sharma, M.M.

2020. New Experimental Methods to Study Proppant
Embedment in Shales. American Rock Mechanics
Association.
2. Alagoz, E. 2020. Interaction of Fracturing Fluids with
Shales: Proppant Embedment Mechanisms. MS Thesis,
The University of Texas at Austin.
3. Alotaibi, M.B., Azmy, R., & Nasr-El-Din, H.A. 2010.
Wettability Challenges in Carbonate Reservoirs.

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