Journal of Petroleum Science and Engineering 141 (2016) 125132

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Journal of Petroleum Science and Engineering

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Mechanisms of imbibition during hydraulic fracturing in shale

formations
Z. Zhou a,n, H. Abass a, X. Li a, D. Bearinger b, W. Frank c
a
Colorado School of Mines, United States
b
Nexen Energy ULC, Canada
c
Devon Energy Production Company L.P., United States

art ic l e i nf o a b s t r a c t

Article history: Hydraulic fracturing technology has been proven to signicantly increase production from shale gas and
Received 20 May 2015 oil formations. However, during a hydraulic fracturing treatment a large percentage of the fracturing uid
Received in revised form usually remains unrecovered. Therefore, the reasons for this low fracturing uid recovery have become
20 October 2015
the focus of many studies. Imbibition of fracturing uid in the shale is believed to be one of the ex-
Accepted 16 January 2016
planations for the low amount of the fracture uid recovery. The uid is imbibed by the shale matrix and
Available online 21 January 2016
trapped inside the rock.
Keywords: Capillarity has generally been the primary mechanism considered during imbibition in conventional
Hydraulic fracturing formations, such as sandstone and carbonate formations. In shale formations osmosis diffusion also
Shale
exists and cannot be ignored because the clay in the shale rock functions similarly to that of a membrane.
Matrix imbibition
It is believed that both capillarity and osmosis diffusion work together to result in imbibition during
Capillarity
Osmosis hydraulic fracturing in shale formations. This paper investigates the effects of both capillarity and os-
mosis diffusion as the key mechanisms in uid imbibition through simultaneous imbibition experiments.
The results of these tests illustrate that the imbibition process is dominated by both capillarity and
osmosis diffusion. This domination is based on the change of water saturation in shale rocks. In addition,
the capillary and osmotic pressures, which inuence the imbibed rate, can be qualitatively determined by
the contact angle and salinity, respectively. Higher capillary and osmotic pressures correlate to faster
rates of imbibition.
This study, which examines the mechanisms of imbibition and their inuences, can improve the
understanding of uid behavior when imbibition occurs during hydraulic fracturing in shale formations.
The understanding of this behavior is useful for further simulation research.
& 2016 Elsevier B.V. All rights reserved.

1. Introduction injected fracturing uid can be recovered (Alkouh and Watten-

Hydraulic fracturing stimulation treatments, which are applied
in the development of shale oil and gas formations, have ve
general steps: pad uid injection, gel uid with proppant slurry
injection, ush uid injection, well shut-in, and fracture uid re-
covery. The fracture uid recovery (called owback or cleanup) is
the last step of the hydraulic fracturing process, and can control
and minimize damage from the fracturing uid, such as clay
swelling, water blockage, and decreased conductivity. Hence, the
recovery of as much water as possible is of signicant importance
during the hydraulic fracturing process. However, many operators
have reported that in shale formations less than 50% of the
n
Correspondence to: Petroleum Engineering Department, Colorado School of
Mines, Marquez Hall #101, 1600 Arapahoe Street, Golden, CO 80401, USA.
E-mail address: zzzhouzhou@gmail.com (Z. Zhou).
barger, 2013). Three areas are believed to retain the large volume
of unrecovered hydraulic fracture stimulation uid. One area is in
the primary fractures that are hydraulic fractures. Another is in the
secondary fractures that are induced and/or reactive and active
natural fractures. The last is in the rock matrix where the fracture
uid has been imbibed (Fan et al., 2010; Ghanbari et al., 2013;
Zhou et al., 2014). Imbibition, therefore, is considered a cause of
low water recovery following the hydraulic fracture process.
Imbibition during hydraulic fracturing is a mechanism that
describes a displacement of the immiscible uids between the
outside and inside of the formation matrix. Generally, the uid
outside of the formation matrix is the water based fracturing uid;
and the uid inside the rock matrix includes crude oil, gas, and
other formation uids. Displacement occurs any time the fractur-
ing uid contacts the formation face. During imbibition, capillarity
is usually considered to be the only mechanism to cause uid
displacement (Hadley and Handy, 1956; Handy, 1960). That may be

http://dx.doi.org/10.1016/j.petrol.2016.01.021
0920-4105/& 2016 Elsevier B.V. All rights reserved.
126 Z. Zhou et al. / Journal of Petroleum Science and Engineering 141 (2016) 125132
true in sandstone and carbonate. However, in clay rich shale, os-
mosis diffusion cannot be ignored and should also be considered.
Osmosis diffusion is a spontaneous movement of water mole-
cules from low-salinity to high salinity. The uid movement occurs
only in the presence of a semi-permeable membrane and a con-
centration difference. The semi-permeable membrane is a barrier
that permits certain molecules to pass through it (Tuwiner, 1962).
That permission is based on a molecule's size and its electrical
properties (Gregor and Gregor, 1978). In geology, clay is considered
to be a semi-permeable membrane that has a salt-exclusionary
behavior due to its structure and electrical restriction (Fritze,
1986). Clay minerals have an electric double layer because the
lower valence cation substitutes for the higher valence cation in
the clay structure. Therefore, the surface of the clay mineral has a
net negative charge and needs to attract cations in the vicinity of
the negatively charged substrate to be neutral (White et al., 1965;
Grim, 1968; Stumm and Morgan, 1970). Because of the negative
potential between the clay platelets, the anions of salts are re-
pelled when they try to pass through the clay so that the cations of
the salt have to stay with those anions to remain electrically
neutral. Hence, salt cannot be transported through the clay, but
water is freely permitted to move through the clay structure
(Fritze, 1986). In petroleum engineering, osmosis diffusion is stu-
died for its effect on drilling and water ooding operations. In
drilling engineering, osmotic studies can help optimize mud
properties and ensure wellbore stability (Bol et al., 1994; Abass
et al., 2006; Lu et al., 2012). Osmotic research in water ooding can
be used to optimize low-salinity water to enhance oil recovery
(Fakcharoenphol et al., 2014).
During hydraulic fracturing treatments in shale formations,
capillarity and osmosis diffusion both cause that imbibition hap-
pens and the fracturing uid is unable to be recovered. Therefore,
study of the mechanisms of imbibition can help to understand the
behavior of fracturing uids that come in contact with shale rocks.
This study of uid imbibition may also contribute to further si-
mulation research. This paper proves that osmosis diffusion and
capillarity are both mechanisms of imbibition in shale formations.
The data derived from the imbibition experiments distinguished
the periods that are dominated by either osmosis diffusion or ca-
pillarity. This paper also discusses how capillarity and osmosis
diffusion inuence the imbibition of uid into shale rocks.
2. Shale samples
For this research, shale samples were obtained from the Horn
River, Woodford, and Niobrara shale formations. Shale samples
from the Horn River and Woodford formations were provided
through the courtesy of the companies that have operations in
those formations. The Niobrara shale samples were obtained from
a quarry near Lyons, Colorado, United States. Fig. 1 shows the cores
from these three formations, respectively.
The samples were measured to determine their rock properties
before conducting imbibition experiments. Measurements include
permeability, porosity, initial water saturation, contact angle, and
salinity.
Permeability and porosity were measured and calculated in-
ternally with the CMS-300 Automated Permeameter and Por-
osimeter manufactured by CoreLab. Instrument-calculated per-
meability is based on pressure decay method, and porosity was
determined by the instrument using Boyle's Law method.
Initial water saturation was determined by measuring the
sample weight before and after drying. The measured sample was
collected from core adjacent to the core used for the imbibition
experiment. To determine the initial water saturation, the sample
was dried in an oven at 275 F until there was no weight change.
The difference in weight before and after drying was the initial
weight of uid in the sample. Then, the initial water saturation of
the sample was calculated based on its bulk volume, porosity, and
uid density (assuming it is equal to the water density).
Contact angle measurements were obtained from the Kruss
DSA-100. A camera picture was taken when a drop of oil attached
to the surface of a solid under a liquid environment. The contact
angle between the oil and the solid was then calculated (Fig. 2).
The method for measuring shale pore water salinity is from the
paper of Abass et al. (2006). Salinity measurement had two steps.
The rst step was to prepare a brine that dissolved formation salt
from the samples. A sample was heated until its weight ceased to
change; then, the dried sample was ground into a powder using a
mortar and pestle, and mixed with distilled water to dissolve
formation salt in the powder. Finally, the mixed uid was ltered
from the powder, isolating the brine for the next step. The second
step was to analyze the brine to determine the concentration of
sodium chloride. Ion Chromatography (IC) measured the chloride
ion concentration; and Inductively Coupled Plasma Mass Spec-
trometry (ICP-MS) was applied to calculate the concentration of
the sodium ions. Finally, salinity of the shale pore water was cal-
culated by the following equation.
(CNa+ + CCl) Vwater
Salinity=
Vsample (1)
where:
CNa+ : concentration of the sodium ions;
CCl: concentration of the chloride ion;
Vwater: distilled water volume;
Vsample: sample volume;
: sample porosity.
Table 1 summarizes the rock properties of the shale samples
that are from the Horn River, Woodford, and Niobrara shale for-
mations. In addition to the measurements described above, Table 1
also includes clay content and TOC data that were provided by the
companies that contributed the samples.
3. Imbibition experiment
The imbibition experiments in this paper used the under-
weighing approach (Fig. 3). The principle of the under-weighing
method is to measure the weight increase of the sample when the
liquid is imbibed by the sample. Compared to other methods, the
under weighing approach can keep samples totally immersed in
the uid during testing. Total immersion is necessary and im-
portant because it can minimize any buoyancy effects.
The balance used in these imbibition experiments was the
Mettler Toledo New Classic S204 balance. Its maximum capacity is
220 g, with a measurement resolution of 0.0001 g. The balance is
able to automatically record the weight changes as a function of
time.
In each group of experiments, three imbibition tests were
running at the same time until each sample's weight reached its
asymptote. The purpose of the simultaneous imbibition experi-
ments was to provide equal conditions during the testing to
minimize factors that can cause variations in results. Running the
tests simultaneously can prevent environmental disturbances.
Fig. 4 shows the simultaneous imbibition experimental cong-
uration in the laboratory.
During the experiments, the balances provided weight changes
as a function of time. To compare the results from various rock
samples when analyzing data, the measured weight is
 Z. Zhou et al. / Journal of Petroleum Science and Engineering 141 (2016) 125132 127

Fig. 1. From left to right: cores from the Horn River, the Woodford, and the Niobrara formations.

Fig. 3. Schematic of the imbibition experimental design.

To investigate the mechanisms of uid imbibition, the liquids in

Fig. 2. Approach of contact angle measurement for Kruss DSA-100.
transformed to the imbibed liquid saturation based on uid den-
sity, sample volume and porosity.
4. Results and discussion
Capillarity and osmosis diffusion, as previously introduced,
should be considered to be the mechanisms that dominate the
imbibition in shale formations during the hydraulic fracturing
process. Both of the mechanisms are illustrated and discussed
herein.
the three simultaneous imbibition experiments were 24% KCl,
distilled water, and crude oil (API 47), respectively. The 24% KCl
water concentration was expected to be higher than the salinity of
any shale sample used in the experiment. In osmosis diffusion, as
noted previously, water ows from a lower to a higher salinity
environment. Therefore, osmosis diffusion can be observed when
the imbibed liquid saturation reduces which means the water
inside the sample ows out due to osmosis diffusion. However, in
real fracturing operations, both osmosis diffusion and capillarity
take place in the same direction towards the reservoir rock where
pore water salinity is higher than the usual KCl percentage used in
slick water fracturing.
The distilled water and crude oil in the imbibition experiments
were used to determine the wettability of the sample in order to
know the wetting phase and the non-wetting phase. Capillary
pressure was a driving force that pushed the wetting phase uid
into the pore spaces of the sample. Capillarity is observed when
the imbibed liquid saturation of the wetting phase increases. Al-
though contact angle measurements already provided results of
the sample's wettability, some pore spaces of the sample may have
different wettability resulting from various minerals and

Table 1
Rock properties of shale samples.

Formations Permeability (ld) Porosity (% of BV) Initial water saturation (% of Contact angle Salinity (mg/l) Clay Content (% of TOC (%)
PV) (deg.) weight)

Horn River 0.0990.48 3.487.41 14.153.34 14.165.2 17,50092,620 1853 0.556.83

Woodford 0.0197 0.465.33 14.9960.83 37.865.3 35,500130,100 1130.2 0.69.17
Niobrara 0.0820.79 2.17.47 12.6317.32 25.651.5 16,00065,500 511
128 Z. Zhou et al. / Journal of Petroleum Science and Engineering 141 (2016) 125132

Fig. 4. Laboratory view of the imbibition experiment.

Fig. 5. Results of imbibition experiments in 24% KCl, distilled water, and crude oil.

saturation history. Therefore, the results of the wettability from
the imbibition tests were supplementary evidence to examine the
conclusions from contact angle measurements. Once the wetting
phase is found, the effect of capillarity can be determined.
As shown in Fig. 5, the imbibition results from the distilled
water and crude oil indicate that those shale samples from the
Horn River formation are water wet because minimal crude oil
was imbibed compared with that of distilled water. Fluctuation in
saturation of crude oil is scatter because of its low level of values.
The graph of the 24% KCl illustrates the three stages that are
dominated by capillarity, osmosis diffusion, and capillarity, re-
spectively. Stage one occurred once the sample was immersed in
the uid, and took only one hour. During the rst stage, because of
capillary pressure, the 24% KCl uid was imbibed into the sample
and increased the imbibed liquid saturation up to approximately
9% (see the enlarged graph in Fig. 5). In Stage two, a decline of the
imbibed liquid saturation was observed indicating that the uid
inside the sample owed out. This decline is caused by osmotic
pressure because of the concentration difference between the uid
outside the sample, 252,430 mg/l (24%KCl), and the uid inside the
sample, 21,725 mg/l. Hence, uid owed from the low-salinity area
to the high salinity area under the domination of osmosis diffu-
sion. The capillary pressure, which has a reciprocal relation to the
water saturation, increased when the saturation inside the sample
decreased. Stage three began when the capillary pressure became
high enough to control the imbibition. In the third stage, the im-
bibed liquid saturation continued to ascend. During the imbibition
experiment with the distilled water, there is no Stage two because
the salinity of the water outside the sample was lower than that of
the uid inside the sample.
In another group of imbibition experiments conducted on Horn
River shale samples, there were six separate stages of the im-
bibition process with the 24% KCl which showed that capillarity
and osmosis diffusion alternately dominate the imbibition process
(Fig. 6). Fig. 6, with an enlarged graph, shows imbibed liquid sa-
turation changed in all stages of the imbibition experiment in 24%
KCl uid. In Stage 1, the imbibed liquid saturation of 24% KCl in-
creased to 10% in twenty minutes. In Stage 2, the imbibed liquid
 Z. Zhou et al. / Journal of Petroleum Science and Engineering 141 (2016) 125132 129

Fig. 6. Results of imbibition experiments for the Horn River shale samples.

saturation decreased to 11%. Then, it increased to 18% in the

third stage, and decreased again. Those increases and decreases
were repeated in the fth and sixth stages. When the capillary
pressure controlled, a large volume of the water was imbibed by
the sample so that the capillary pressure dropped off as the sa-
turation increased. Then, the osmotic process was observed and
the imbibed liquid saturation decreased. As the liquid saturation
decreased, the capillary pressure increased and dominated im-
bibition again. However, it needs to clarify the stages in these two
cases of Horn River samples are used to academically explain how
osmosis diffusion and capillarity may work. There may be more
stages during imbibition.
Another conclusion from Fig. 6 is that the wettability of the
samples can be investigated through the imbibition experiments.
The contact angle measurements show that the three samples are
all water wet. The crude oil is the non-wetting phase. However, in Fig. 7. Results of imbibition experiments for the Woodford shale samples.
the imbibition tests the crude oil is still imbibed by the sample, but
the amount of the imbibed volume is much less than that of dis- that decline is believed not to be caused by osmosis diffusion
tilled water. Therefore, the samples are water wet, but some pore because that decrease is too small, only 1% imbibed liquid sa-
spaces in the samples are oil wet. turation. In Figs. 5 and 6, the changes are at least 10% at both stage
The experimental results from the Woodford and Niobrara 1 and stage 2. Therefore, it is concluded that the decline of 1% is
shale samples are different from the results from the Horn River considered as data measurement issue rather than a phenomenon.
shale samples (Figs. 7 and 8). In both the Niobrara and Woodford Additionally that is the only data observed as no repeatability is
shale samples, capillarity dominated when the samples were im- detected in all other distilled water tests. It is always the case that
mersed in the 24% KCl, and the imbibed liquid saturation con- in distilled water, the imbibition continues to its asymptote
tinued to increase until the asymptote was reached. Then the without declining.
imbibed liquid saturation began to decline because of osmosis The reason for those differences in imbibition was that the
diffusion. samples from the Niobrara and Woodford formations had very low
In Fig. 7, there is a 1% decrease at the beginning of the im- water saturations. The initial water saturation of the Woodford
bibition experiment with distilled water. After careful analysis, shale sample in the 24% KCl was about 23.4%, and that of the
130 Z. Zhou et al. / Journal of Petroleum Science and Engineering 141 (2016) 125132
Fig. 8. Results of imbibition experiments for the Niobrara shale samples.
Niobrara shale sample in 24% KCl was approximately 17%. Both
initial saturations were lower than the saturation of the Horn River
shale samples in 24% KCl which was about 50%. Therefore, the
capillary pressure in those samples with lower saturations was
much higher and stronger, and as a result, the capillarity domi-
nated at rst during imbibition. Then, osmosis diffusion began to
control the imbibition process when the saturation of the sample
was high enough and the capillary pressure was lower than the
osmotic pressure. In addition, the duration of Stage 1 in both the
Niobrara and Woodford shale samples was much longer than that
in the Horn River shale samples. A possible explanation is that for
the Niobrara and Woodford shale samples, because of lower initial
water saturation the sample needed more time to achieve suf-
cient imbibed volume to lead to high enough water saturation and
the change of dominant pressure from capillary pressure to os-
motic pressure.
In order to prove the conclusion that capillarity dominates the
imbibition process when samples have very low initial water sa-
turations, imbibition experiments were run on three dried shale
samples from the Horn River, Woodford, and Niobrara shale for-
mations, respectively. Before starting the imbibition experiments,
the three samples were dried in an oven at 275 F until there was
no weight change. Therefore, all the samples had very low initial
water saturation at the beginning of the experiments. According to
Fig. 9, in 24% KCl test uid, all samples, including the sample from
the Horn River formation, behaved similarly in that imbibed liquid
saturation continued to increase until reaching peak saturation,
and then began to decrease. The decrease in liquid saturation did
not appear at the early stage of the experiments. The increase in
liquid saturation was still believed to be controlled by capillarity,
Fig. 9. Results of imbibition experiments for the dried shale samples.
Faster rate
Contact Angle: 15.09
Slower rate
Contact Angle: 48.82
Fig. 10. Effect of the capillary pressure.
and the decrease was dominated by osmosis diffusion. Hence,
capillarity strongly controls imbibition when the uid rst con-
tacts rock that is at a sub-irreducible water saturation condition.
According to the experiments, capillary and osmotic pressures
have the ability to inuence the rate of imbibition. Capillary
pressure can be qualitatively determined by the contact angle.
When the contact angle of the water on the sample is less than 90
and approaches 0, the sample is strongly water-wet. The value of
the capillary pressure is also greater in the strongly water-wet
sample than in the sample with a larger contact angle. Fig. 10
shows that the imbibed rate is faster in distilled water when the
water contact angle is smaller which means capillary pressure is
greater. The salinities of these two samples are similar at ap-
proximately 53,000 mg/l, so the values of osmotic pressure are
also similar. The slope of the imbibed liquid saturation represents
the rate of imbibition. The steeper slope indicates the imbibed rate
is faster.
Osmotic pressure is calculated by Eq. (2).
RT a wI
= ln
w a wII (2)
: osmotic pressure;
R: gas constant, 0.08205 liter atm/mole K;
T: temperature;
w : mean partial molar volume of water;
a wI : water activity of the uid outside rocks;
a wII : water activity of the uid inside rocks;
The gas constant, temperature, and mean partial molar volume
are considered to stay the same for all the imbibition experiments.
The water activity depends on the salinity of the uid. The water
activity of pure distilled water is one, and decreases to zero with
an increase in salinity. Hence, when the water activity of the uid
outside the rock is constant, the higher salinity inside the rock
leads to a smaller a wII and a higher osmotic pressure. With higher
osmotic pressure the rate of imbibition is faster when the imbibed
liquid saturation decreases (Fig. 11). The shale samples in Fig. 11
have similar contact angles.
When the uid outside the rock sample is distilled water, with
a lower salinity than the uid inside the sample, the higher os-
motic pressure still results in a faster imbibed rate (Fig. 12).
 Z. Zhou et al. / Journal of Petroleum Science and Engineering 141 (2016) 125132
Slower rate
Faster rate
Fig. 11. Effect of osmotic pressure on the outside uid with a higher salinity.
Faster rate
Slower rate
Fig. 12. Effect of osmotic pressure on the outside uid with a lower salinity.
5. Conclusion
This paper analyzed the data from simultaneous imbibition
experiments to investigate the mechanisms that control the im-
bibition process in shale formations during the hydraulic fractur-
ing process. The conclusions are summarized as follows.
1. Besides capillarity, osmosis diffusion is underpinned especially
when the results of 24% KCl are compared with those from the
distilled water. Because of the clay in the shale, which acts as a
kind of membrane, osmosis diffusion can occur when con-
centration differences exist between the outside and the inside
of shale rocks. Therefore, osmosis diffusion is one of the me-
chanisms controlling imbibition in clay rich shale. During the
hydraulic fracturing treatment in shale formations, if salinity of
the fracturing uid is less than pore water salinity in the for-
mation, osmotic pressure is also a driving force to cause that the
fracturing uid is imbibed by shale formations.
2. During imbibition in shale samples, both osmosis diffusion and
capillarity dominate the process. The domination is inuenced
by the water saturation in the shale samples. Because of the
reciprocal relationship between capillary pressure and water
saturation, the capillary pressure is high and dominates the
imbibition process when the water saturation is low. In most
shale formations, the initial water saturation is under the sub-
irreducible saturation condition. Therefore, capillarity controls
imbibition when the uid rst contacts the rock. With the in-
creased volume of imbibed uid in the rock, the capillary
pressure becomes smaller until the osmotic pressure dominates
the imbibition process.
131
3. The strongly water wet sample has a high capillary pressure
which is related to the rate of imbibition. The higher capillary
pressure results in a faster rate of imbibition.
4. When the salinity of the uid outside the rock is constant, high
salinity inside the rock can produce a larger osmotic pressure
than low-salinity inside the rock. The imbibed rate is faster with
the higher osmotic pressure. If the salinity outside the sample is
higher than the inside, the higher osmotic pressure can help the
water inside the rock to ow out faster. If the salinity outside
the sample is lower than inside, the higher osmotic pressure can
lead to a faster inow rate of imbibition.
5. According to the conclusion 4, adjusting the wettability and
salinity of the fracturing uid to change capillary and osmotic
pressures in the shale formation can control imbibition. Using
surfactant to change near fracture formation into higher contact
angle and increasing the fracturing uid salinity can lead to a
slower imbibed rate; and if the fracturing uid salinity is higher
than the pore water salinity, osmosis diffusion can be reversed
and cause water molecules leave the formation into the created
fracture domain.
6. The imbibition experiments can distinguish the wetting phase
and non-wetting phase of the rock. The results from the im-
bibition tests are more accurate than those from the contact
angle measurement. During imbibition experiments, the im-
bibed volume and rate show the distinct difference between oil
and water. The imbibition experimental result provides a more
concrete indication of wettability on pore spaces in the samples,
but the contact angle measurement only indicates wettability
on surfaces of the sample.
This paper provides a qualitative analysis of the effects from
osmosis diffusion and capillarity on the imbibition process in
shale. Further studies are required to quantify the contributions
from osmotic and capillary pressures to imbibition. Since osmosis
diffusion is related to the clay content in shale, imbibition as a
function of clay content should also be investigated fully. In ad-
dition, simulation of uid imbibition in shale formations should
include the inuence of both osmosis diffusion and capillarity.
Acknowledgments
The authors appreciate the Fracturing, Acidizing, Stimulation
Technology (FAST) Consortium at the Colorado School of Mines for
sponsoring this project, and also thank Nexen Energy ULC, INPEX
Gas British Columbia Ltd, and Devon Energy Production Company
L.P. for their contribution of the shale samples used in the study. In
addition, the authors thank Dr. Xiaolong Yin and Mr. Joe Chen for
their help in conducting the experiments.
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