| DOI: 10.3933/APPLRHEOL-27-64433 | WWW.APPLIEDRHEOLOGY.

ORG

Hydrogel Formulation for Sealing Cracked Wellbores

for CO2 Storage

Mohammadreza Shafiei1, Steven Bryant2, Matthew Balhoff3, Chun Huh3,

Roger T. Bonnecaze1*

1McKetta Department of Chemical Engineering, University of Texas at Austin, Austin, TX 78712, USA
2Department of Chemical and Petroleum Engineering, University of Calgary, Calgary, T2N 1N4 Canada
3Department of Petroleum Engineering, University of Texas at Austin, Austin, TX 78712, USA

*Corresponding author: rtb@che.utexas.edu

Received: 13.7.2017, Final version: 22.9.2017

Abstract:
A challenge for underground CO2 storage is the leakage of the buoyant supercritical gas through microcracks in wellbores that
cannot be sealed with current oilfield cements that are too viscous and cannot penetrate the cracks. Polymer gels consisting
of pH-sensitive hydrogel particles suspended in an aqueous solution offer a potential alternative. The rheology of aqueous
solutions of Carbopol 934 as a model pH-sensitive gel is measured to find the compositions and pHs for both ease of injection
and to seal cracks against the flow of bulk CO2 and CO2 dissolved in brine. The polymer gels have low viscosity at low pH and
can easily flow into the microcracks. In the elevated pH of the microcracks, the particles swell creating a significant yield stress
sufficient to seal leakage pathways. The yield stress reaches a maximum at pH 5 and it increases with increasing concentration.
The flow curves of stress versus shear rate for all pHs and concentrations are well-described by the Herschel-Bulkley model
with an exponent of about 0.34 except for highly acidic conditions when the gelant solutions show a much lower yield stresses
and higher exponents. The flow curves can be collapsed onto a single universal flow curve rescaled with the yield stress, the
low frequency shear modulus and the suspending fluid viscosity. The presence of salts, especially high valence salts, reduce
the yield stress of the gels considerably. It is shown that the addition of chelating agents mitigates this effect and can restore
more than 30 % of the yield stress of the gelant.

Key words:
CO2 , Carbopol, yield stress, Herschel-Bulkley, pH-sensitive gelant

1 INTRODUCTION
Geologic carbon storage GCS is a path on the transition
to renewable energy by capturing carbon dioxide CO2
and injecting it deep underground via wells into geo-
logical reservoirs [1]. GCS involves capture of CO2 from
power plants, transport to geological formations, and
finally compression of the gas and injection into a for-
mation, where its movement is monitored and the
quantity stored is regularly verified [1, 2]. A major con-
cern for GCS is the ability of the formation to hold CO2
over the long term.
Many reservoirs that meet the required specifica-
tions for CO2 storage are located in areas with aban-
doned preexisting wells and no owner or operator [3,
4]. These wells are constructed with cement between
the steel casing and the rock formation layers to form
a seal to prevent uncontrolled flow of liquid and gas.
The seals on these old wells are often imperfect [5 – 7].
Small channels can be created during the initial curing
of the cement [8, 9]. Chemical attack from formation
fluids and mechanical stressing, drilling, and hydraulic
fracturing can create cracks in the cement that then
leaks [10, 11]. The challenge is to ensure the integrity of
the cement to prevent any potential leakage of CO2
from the formation.
Current technology for sealing damaged wells is
so-called cement squeeze in which slurry cement is
forced into cavities behind the casing and near leakage
pathways to restore the integrity of existing wells. This
technique is often unsuccessful as the fractures are too
narrow to be filled and repaired with highly viscous oil-
field cement. Here we explore and develop the formu-
lation of a polymer gelant based on a model pH-sensi-
tive microgels to seal small channels and microcracks
from which CO2 could leak from the formations [12, 13].

© Appl. Rheol. 27 (2017) 64433 | DOI: 10.3933/ApplRheol-27-64433 | 1 |

The material allows for low viscosity injection at low pH
and then forms a strong yield stress material at the high
pH conditions of the cement and CO2-laden brine of the
formation.
Specifically, we use Carbopol 934 as a model sys-
tem of polyacrylic acid hydrogels. When dissolved in
water, the polymer partially dissociates and forms a rel-
atively thin liquid at a low pH. The polyacrylic acid forms
particles that swell with sufficiently high pH due to the
deprotonation of the acid and subsequent balancing of
electrostatic repulsion and gel elasticity, thus forming
a jammed, concentrated of suspension of soft particles
[14, 15]. The aim here is to inject the hydrogel solution
at low pH so it has a low viscosity and can easily pene-
trate the cracks. When the polymer contacts the hydrat-
ed cement, which is strongly alkaline, the pH increases
and the polymer swells and forms a yield stress fluid.
Carbopol 934 was chosen because it contains high mol-
ecular weight polyacrylic acid and has higher yield
stresses compared to many other grades, which is im-
portant to seal the cracks.
Typical yield stresses required to seal cracks with
the aperture of 150 microns have been estimated at 10
to 100 Pa, which is within the range of yield stresses ob-
tained for cross-linked polyacrylic acid polymers
[16 – 18]. The polymer solution will also contact the for-
mation fluid, a brine with a high salt concentration,
Table 1: Experimental conditions and fitted Herschel-Bulkley
shear stress versus shear rate flow curve parameters of yield
stress sg , consistency index k and power law index n.
© Appl. Rheol. 27 (2017) 64433 | DOI: 10.3933/ApplRheol-27-64433
which can interfere with the pH-triggered change from
a thin fluid to a gel with a yield stress. The aim of this
paper is to determine the formulation of polymer, pH
and additives such as chelating agents to ensure the
material performs as a sealant for the cracks in the ce-
ment.
The outline for the remainder of the paper is as fol-
lows. In Section 2, the materials and methodology are
described. In Section 3, the flow curves of the polymer
solutions in water are determined for varying concen-
tration of polymer, pH and salt concentration. A univer-
sal flow curve following a Herschel-Bulkley form is
found for the Carbopol 934 for a wide range of formu-
lations. In Section 4 we discuss the results in the context
of the specific application of sealing cracks in well-bores
and more broadly for highly concentrated suspensions
of soft particles.
2 METHODOLOGY
2.1 MATERIALS
Carbopol 934 was obtained from the Lubrizol Company
in powder form. It is one of the most widely used gelling
agents for various applications in personal care prod-
ucts, pharmaceuticals and enhanced oil recovery. Sodi-
um hydroxide, sodium chloride, calcium chloride and
sodium triphosphate in solid form were purchased
from Fisher Scientific, Inc.
2.2 SAMPLE PREPARATION
The gel was prepared by slowly dispersing varying con-
centrations of the Carbopol 934 polymer in deionized
water. Powder was added in small increments to the
vortex created by a mixer in a beaker. The dispersion
was covered and stirred for one day to ensure the poly-
mer was fully hydrated. A solution of 1.0 M NaOH was
added to the dispersion to adjust the pH to the desired
values. Samples with pH ranging from 2.5 to 12.0 were
prepared (Table 1). A waiting period of 24 hours was nec-
essary to make sure the pH was uniform and the gel at
equilibrium. To eliminate trapped air bubbles, samples
were centrifuged at 2000 rpm for 10 min.
2.3 RHEOMETRY
The rheological properties of the gels were measured
using a stress controlled AR-G2 rheometer equipped
with a parallel plate tool. The plate was 40 mm in di-
ameter. A solvent trap was used to prevent water evap-
oration during measurements. To avoid wall slip espe-
cially at low shear rates, sandpaper with a roughness
| 2 |
Figure 1: Shear stress versus shear rate for 1.0 wt.% Carbopol
934 for varying pH.
of 200 µm was glued to both the plates. Samples were
pre-sheared for two minutes to erase any shear history
during sample preparation and loading. Samples were
then allowed to rest for two minutes before the mea-
surements. Strain sweep tests were conducted for
strains ranging from 0.002 to 18000 % with a fixed fre-
quency of 0.1 Hz that ensure the measurements were
within the linear viscoelastic region. We determined
flow curves by applying varying shear stresses and mea-
suring the resulting shear rates. For points close enough
to yield stress, the gel was sheared about 104 seconds
in order to reach equilibrium. At stresses above the yield
stress, the plot of shear rate versus time shows a
plateau, which is a representative of steady state [15].
Creep test, stress ramp and strain sweep were also con-
ducted to measure and verify the yield stress of the gels.
With the help of creep test, we could measure shear
rates as low as 10-5 s-1 which was impossible to achieve
with other methods.
3 RESULTS AND DISCUSSION
3.1 EFFECT OF PH ON FLOW BEHAVIOR
The shear stress s versus shear rate g ̇for 1.0 wt.% Car-
bopol 934 for varying pH is shown in Figure 1. For all pHs,
the material exhibits a Herschel-Bulkley behavior with
a plateau or yield stress sy at low shear rates. The yield
stress increases by almost two orders of magnitude as
pH varies from 3.3 to 5.9. Increasing the pH from 5.0 to
9.0 does not affect the yield stress values but the further
increase of pH values lowers the yield stresses to some
extent. The highest yield stress is achieved at pH = 5.9
(see Figure 1), consistent with studies on other Carbopol
gels [19 – 21]. This increase in stress is known very well
and could be attributed to the swelling of the cross-
linked polyacrylic acid when the carboxylic acid groups
are deprotonated [14, 21, 22]. The polymer particles swell
due to the osmotic pressure ultimately balanced by the
© Appl. Rheol. 27 (2017) 64433 | DOI: 10.3933/ApplRheol-27-64433
Figure 2: Shear stress versus shear rate for varying concentra-
tions of Carbopol 934 at pH = 4.5.
elasticity of the polymer network. The maximum thick-
ening is achieved when the sodium hydroxide deproto-
nates approximately all the carboxylic acid groups along
the polymer backbone. The yield stress sy was deter-
mined by fitting the flow curves to the Herschel-Bulkley
model
(1)
Where sy, k and n represent yield stress, consistency in-
dex, and power law index. The flow curves in Figure 1
are well described by the Herschel-Bulkley model,
which is in accordance to previous studies done on oth-
er polyacrylic acid microgels [12, 13, 15, 20, 21]. The values
of the Herschel-Bulkley parameters from the flow
curves are listed in Table 1.
3.2 EFFECT OF POLYMER CONCENTRATION ON FLOW
BEHAVIOR
To investigate the effect of polymer concentration,
samples of varying polymer concentration for a given
pH were prepared. Stress ramp and creep tests were
conducted to obtain flow curves. A plot of shear stress
as a function of shear rate for range of concentrations
of polymer at pH = 4.5 is shown in Figure 2. As the con-
centration of polymer increases, the yield stress and the
viscosity of polymer gelant increase. For polymer con-
centrations greater than 3.0 wt.%, the dispersion and
injection of polymer gelant becomes impractical. The
values of sy, k, and n for several concentrations of the
polymer neutralized to 4.5 is given in Table 1.
3.3 EFFECT OF PH AND CONCENTRATION ON YIELD
STRESS
Yield stress was obtained via three different methods.
The stress ramp method was the primary technique
used, but creep tests and strain sweep tests were also
| 3 |
Figure 3: Yield stress versus pH for Carbopol 934 for polymer Figure 4: The variation of the low frequency modulus G0 with
concentrations of 1, 2, and 3 wt.%. pH of Carbopol 934 polymer.

used to confirm the yield stress values. We found good

agreement between these three methods in obtaining
yield stress values (less than 2 % difference in almost all
cases). As shown in Figure 3, the yield stress increases
as the polymer concentration increases and reaches a
maximum at pHs ranging from 4.0 to 6.0 depending on
the concentration. The yield stress is high for a broad
range of pH, though it decreases around pH = 12.0. Qual-
itatively similar results have been observed with other
gels [19 – 21]. Lalehrokh et al. showed a yield stress of 10
to 100 Pa is required to seal microcracks. Here we
achieved yield stresses up to 350 Pa, which makes the
polymer gel achievable for field application [16 – 18]

3.4 EFFECT OF PH ON LOW FREQUENCY MODULUS G0

The oscillatory strain sweep tests were conducted at a
frequency of 0.1 Hz. At low strain values, storage and
loss moduli are constant. The values of storage modu-
lus G' at the low strains are reported as G0, the low fre-
quency shear modulus [23]. The variation of G0 versus
pH is shown in Figure 4. The low frequency shear mod-
ulus shows a similar trend with pH as the yield stress,
including a sharp rise to a maximum around pH = 4.0
for 3.0 wt.% polymer concentration. The low frequency
shear modulus exhibits a maximum at pH ranging from
4.0 to 6.0, and it decreases with increasing polymer
concentration. Gutowski et al. also noted the sharp rise
in the low frequency modulus with the Carbopol Ultrez
10 and Carbopol ETD 2050 used in their studies [21]. Fig-
ure 5 shows the yield stress as a function of G0. The low
frequency shear moduli follow the same linear depen-
dence with yield stress, regardless of pH and polymer
concentration.
3.5 EFFECT OF PH ON CONSISTENCY AND POWER LAW
INDICES
We also investigated the effect of pH on consistency in-
dex and power law index. The values for k and n were
Figure 5: Yield stress sy versus low frequency shear modulus G0
for Carbopol 934 at polymer concentrations of 1, 2, and 3 wt.%.
obtained from the Herschel-Bulkley fit of the flow
curves. Figure 6 shows the k and n as functions of pH.
As can be seen from Figure 6, the power law index n re-
mains constant at about 0.34 for a range of pH values
greater than about 4.5. The values of power law index
here are relatively insensitive to both concentration
and pH, unlike the results for Carbopol Ultrez 10 and
Carbopol ETD 2050 [21], where the n in these cases in-
creased or decreased from about 0.39 – 0.59 with con-
centration, depending on the Carbopol.
3.6 MASTER FLOW CURVE FOR HYDROGEL
Master flow curves have been proposed for microgels, mi-
celles and compressed emulsions that collapse data for a
variety of particle concentrations, contact stiffness and
suspending fluid viscosity [15, 22, 24, 25]. In Figure 7, a mas-
ter curve is plotted using the flow curves of several differ-
ent samples, in which s/sy is plotted against (μS ġ)/G0.
The data for a wide range of polymer concentrations and
pH collapse onto a single master curve. The master curve

© Appl. Rheol. 27 (2017) 64433 | DOI: 10.3933/ApplRheol-27-64433 | 4 |

Figure 6: (a) Consistency index k versus pH for varying concentrations of Carbopol 934 polymer, (b) power law index n versus
pH for varying concentrations of Carbopol 934 polymer for polymer concentrations of 1, 2, and 3 wt.%.

is well-described by the expression

(2)

The fact that the data can be collapsed on the master

curve is due in part to the fact that the power law index
is approximately constant for a wide range of pH and
polymer concentration. As noted earlier, such a trend
has not been observed for all Carbopol materials [21].
This master curve is similar to that proposed by Cloitre
et al., where the shear rate is rescaled with G0/μS except
here the exponent that best fits the data is 0.34 com-
pared to 0.5 that has been found for microgels, micelles
and compressed emulsions [15, 22, 24]. The difference
may be due to the fact that the Carbopol microgel par-
ticles are very polydisperse compared to those used in
Figure 7: Universal flow curve of dimensionless shear stress ver-
the other studies.
sus shear rate for a range of pHs and polymer concentrations.

3.7 EFFECT OF SALT CONCENTRATION ON YIELD

STRESS
Salts like NaCl and CaCl2 are common in the brine of for-
mations for CO2 storage and in contact with cement of
wellbores. These salts can cause the polymer to precip-
itate into two different phases including salt-precipi-
tated syneresed polymer and water. Sodium and calci-
um ions also screen carboxylic charges on the hydro-
gels, which cause the polymer to collapse due to lack of
repulsive forces. Measurements of flow curves with
varying concentrations of NaCl and CaCl2 are shown in
Figure 8. These flow curves show that salt significantly
reduces the yield stress of the gel. The yield stress for
a 3.0 wt.% gel at pH = 4.5 drops from 350 to 200 Pa at
only 0.5 wt.% NaCl and it drops further to about 40 Pa
at 3.0 wt.% NaCl (Figure 8a). The effect is even greater
for 1.25 wt.% CaCl2 where the divalent salt and the re-
sulting additional screening of electrostatic forces
cause the yield stress to practically vanish (Figure 8b).
In order to improve the resistance of polymer against
the salt, the polymeric gel was formulated with two
chelating agents, ethylenediaminetetraacetic acid ED-
TA and sodium triphosphate (Na5P3O10) which chelate
sodium and calcium ions to inhibit polymer syneresis.
The restoration of more than 30 % of the yield stress of
the gel formulated with sodium triphosphate in a solu-
tion of CaCl2 is shown in Figure 8b. The restoration of
the yield stress to 100 Pa is still adequate for sealing the
microcracks. Similar results were observed for the ED-
TA. Samples of the hydrogel treating with chelating
agents in contact with cement and the CaCl2 were
found to retain their yield strength for over one year.

© Appl. Rheol. 27 (2017) 64433 | DOI: 10.3933/ApplRheol-27-64433 | 5 |

Figure 8: Shear stress versus shear rate for 3.0 wt.% polymer concentration: (a) Varying concentrations of (0.5, 1, 2, 2.5, and 3
wt.%) NaCl at pH = 4.5 (b) 1.25 wt.% CaCl2 at pH = 6.5 before and after treatment with sodium triphosphate.

Figure 9: (a) The untreated gel after precipitation and (b) treated gel in brine-filled environment.

In another experiment, a cube of cement was
placed inside a treated gel. In order to prevent the gel
from drying out, the gel was maintained inside a cov-
ered beaker in the lab’s environment for about 20
months. It was found the treated gel did not undergo
precipitation and maintained the yield stress of 140.8
Pa. Figure 9a shows the precipitation of the untreated
polymer gel in contact with cement core. Figure 9b de-
picts how a treated gel could withstand against brine-
filled environment. Furthermore, the graphs of shear
stress against shear rate for untreated and treated poly-
mer gels are plotted in Figure 10. Note that the untreat-
ed sample was not exposed to saline media while the
treated one was in contact with brine-filled environ-
ment. The flow curves show that the salinity could af-
fect the gel’s strength to some extent. From Figure 10,
the yield stress values of untreated and treated 2.0 wt.%
Carbopol 934 at pH = 7.1 were determined 223.3 and
140.8 Pa, respectively. The 140.8 Pa is still above the 100
Pa threshold value, which confirms our claim that the
treated polymer could maintain the yield strength for
more than a year when exposed to saline-filled media.
Since long-term storage is required, aging could
adversely affect the sealing purpose to some extent.
However, 3 wt.% Carbopol (97 wt.% water) is very cheap
to prepare and it could be maintained in reservoir con-
dition at least for one year. In order to assure long-term
containment, the polymer could be injected in regular
intervals (for example annually) until the CO2 is trapped
in any of known trapping mechanisms.
3.8 COMPARISON OF YIELD STRESS-LOW FREQUENCY
SHEAR MODULUS WITH HYDROGELS
The plot of yield stress versus low frequency shear mod-
ulus for different hydrogels has been plotted in Fig-
ure 11. Ultrez 10, ETD 2050 and MAA/EA show lower val-
ues of yield stress when compared to Carbopol 934 and

© Appl. Rheol. 27 (2017) 64433 | DOI: 10.3933/ApplRheol-27-64433 | 6 |

Figure 10: The change in gel strength after 20 months expo-
sure to saline environment.
940 [21, 26]. It has been shown below some concentra-
tions called CG (entropic glass transition) samples be-
have like dilute colloidal suspensions. For concentra-
tions CG < C < CJ, where CJ is jamming transition, the
long-range displacement of particles is restricted [26].
Above CJ, the steric hindrance results in flat contacts
which is responsible for repulsive forces and hence the
onset of elastic [14]. The elastic modulus, which is a
function of elastic contact forces increases rapidly as
concentration increases which could be attributed to
the increase in number of particles per contact and
compression of particles [14, 27]. The low frequency
shear modulus of MAA/EA changes slowly up to CJ =
0.016 wt%. However, above this point the low frequen-
cy shear modulus increases rapidly compared to yield
stress which could be the reason for unusual behaviors
of polymers like MAA/EA, Ultrez 10 and ETD 2050 [26].
The same behavior could be seen for low and high con-
centrations of Carbopol 941.
4 SUMMARY AND CONCLUSIONS
The shear rheology of Carbopol 934 as a model hydrogel
for sealing microcracks in wellbores and stopping leaks
in CO2 storage formations has been studied. These ma-
terials exhibit superior rheological properties compared
to the current oil-field cements for sealing in that they
can be injected at low pH with low viscosity to penetrate
and fill the microcracks and then become solid in the
higher pH environment of the cement. The strength or
yield stress of the hydrogel is more than sufficient to
seal the cracks against the flow of CO2 and prevent leaks.
The flow curve of the shear stress versus shear rate
of the hydrogel is well described by the Herschel-Bulk-
ley equation. All the data can be collapsed onto a single
master flow curve for a range of pHs and polymer con-
centrations allowing one to predict the properties of
other potential formulations and provide a convenient
formula for flow simulations. While such a collapse has
© Appl. Rheol. 27 (2017) 64433 | DOI: 10.3933/ApplRheol-27-64433
Figure 11: Yield stress sy versus low frequency shear modulus
G0 for different hydrogels.
been reported for relatively monodisperse microgels, it
is remarkable that it also works for polydisperse mate-
rials. In part, the collapse occurs because the power-law
exponent of the Herschel-Bulkley fit is approximately
the same for all pHs and polymer concentrations. The
fitted values of these power law exponents are quite
sensitive to the values of the yield stresses. It was thus
critical in this study to use roughened surfaces and mul-
tiple and sometimes time-consuming methods to en-
sure accurate, cross-checked values of the yield stress.
It is possible that the universal flow curve has not been
observed for other Carbopol or polydisperse polyacrylic
acid hydrogels because of the challenge of measuring
the yield stress at low shear rates needed to accurately
fit the power law exponents.
The presence of sodium and calcium ions leaching
from the cement of the wellbore can cause the polymer
to precipitate and prevent the formation of a solid-like
gel to seal the microcracks. Chelating agents included
in the hydrogel formulation can bind these ions and al-
low the hydrogel to form a solid with 30 % of the orig-
inal yield stress restored, sufficient to seal the microc-
rack for formulations identified here. The yield strength
of the material is maintained for at least one year in
brine-filled environment of the microcrack. Thus, hy-
drogels are viable materials for sealing microcracks in
formations for CO2 storage.
ACKNOWLEDGEMENTS
The authors thank the Department of Energy for fund-
ing this work through Award No.: DE-FE0009299 at the
Center for Petroleum Engineering at The University of
Texas at Austin. The help of undergraduate students
Deepali Patel, Valeriy Shakenov, Joulia Nikolaevna Po-
liaeva and Paulami Das with performing some of the
experiments is greatly appreciated. We are grateful to
Dr. Michel Cloitre for his advice on measuring the yield
stress and other discussions.
| 7 |

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