SPE-191822-18ERM-MS

Smart Expandable Polymer Cement Additive to Improve Zonal Isolation

Livio Santos and Arash Dahi Taleghani, Pennsylvania State University; Guoqiang Li, Louisiana State University

Copyright 2018, Society of Petroleum Engineers

This paper was prepared for presentation at the SPE Eastern Regional Meeting held in Pittsburgh, Pennsylvania, USA, 7 - 11 October 2018.

This paper was selected for presentation by an SPE program committee following review of information contained in an abstract submitted by the author(s). Contents
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Abstract
One of the critical issues that might happen in some oil and gas wells is the failure of the cement sheaths and
its debonding from the casing string. Cement shrinkage during setting is regarded as one of the main causes
behind formation of microannulus cracks. In this paper, a new class of polymer-based expandable additives
is presented in the form of fibers to address shrinkage and debonding issues in the subsurface. The proposed
fiber additives are made from shape memory polymers. These fibers expand upon exposure to temperatures
above certain limits; which is selected to be below the temperature of the cementing zone. In this situation,
the expansion occurs before the cement setting but after its placement. If the expansion occurs after cement
setting, it may lead to microfractures. As a result of the controlled expansion of the cement paste, the
creation of channels and fluid migration can be minimized while maintaining the mechanical properties
required for cement integrity. Considering the inert property of the proposed additive, the cement water
ratio and its chemical properties do not change. The cement expansion, fluid loss, gel strength, compressive
strength, and tensile strength of the samples containing these fibers are examined by destructive and non-
destructive methods and presented here. The proposed class of expandable additives can help the operators
reach sustainable well integrity by improving the bonding between the cement and casing.

Introduction
Fluid migration in the annulus can severely compromise well integrity, affecting long term production and
injection efficiency. Annular gas flow outside the casing is usually associated with failure of the cement
sheath. This issue is more common in unconventional reservoirs due to hydraulic fracturing operations. In
these wells, large pressure fluctuations during hydraulic fracturing treatments can happen hundred times
during a single treatment. About 25% of the wells in the Marcellus shale in 2011 were reported for
having sustaining casing pressure (SCP) (Williams et al., 2011). Additionally, cementing is also required
to permanently seal pay zones along the well in the plug and abandonment (P&A) stage. P&A regulations
are very strict and demand an effective barrier against pressurized flow from subsurface after abandonment
(Ferg et al., 2011). Growing environmental concerns regarding methane emissions (Jiang et al., 2011) and
contamination of aquifers (Ingraffea et al., 2014) in few problematic areas have raised some attentions about
new solution for improving integrity of the cement sheaths.
2 SPE-191822-18ERM-MS

The changes in downhole conditions associated with high pressure injections during hydraulic fracturing
leads to variations in the stress state in well cements. Cement failure in tension causes radial cracks and
excessive compressive stresses that can crush the cement sheath (Goodwin and Crook, 1992). An increase
in pressure or temperature inside the wellbore can lead to a slight expansion of the casing, thus, deforming
the cement in a way that creates tangential tensile stress; stretching the cement sheath. Portland cement, in
general, has a much higher resistance to shear failure than to tensile failure (Alqam et al., 2018). In order
to improve zonal isolation, it is important to increase the ductility of the cement sheath, which includes
tensile and flexural strength. A more ductile cement allows more loading cycles and a certain degree of
deformation before it reaches failure, as opposed to a more brittle cement.
Weak bonding between cement and casing or cement and formation may accommodate development of
microannulus, which basically provides a small conducive gap for fluid migration. Improvement of drilling
practices such as more effective mud removal techniques (Choi et al., 2018) and more accurate casing
centralization decrease the chances of cement failure at the rock interface but cannot fully prevent formation
of microannulus cracks at the casing interface (Baumgarte et al., 1999). In addition, cement shrinkage
during setting, casing contraction and inelastic behavior of the formation rock due to thermal- and pressure-
induced stresses increase the chances of formation of microannulus cracks. The cement, reportedly, can
shrink up to 4% in volume after placement in the wellbore, with most of the process occurring when the
cement is in the hardening phase (Chenevert and Shrestha, 1987). Van Eijden et al. (van Eijden et al., 2017)
provide an overview of the advances in standardized procedures to evaluate volumetric changes of the
cement. Exposure of the casing to temperature changes and mud density variations can generate shearing
at the casing-cement interface and lead to failure at this interface (Goodwin and Crook, 1992). Excessive
overburden pressure may also contribute to shear failure (Dahi Taleghani and Wang, 2016).
Logging tools are available to evaluate cement quality qualitatively like cement bond log (CBL) and
ultrasonic imaging tool (USIT). When compared to physical tests, for instance, pressure testing, the cost
is relatively low (Boyd et al., 2006). The logs play an important role to identify failure even when the
fluid does not migrate all the way to the surface and does not show a sustained casing pressure (SCP).
However, microannulus can be so small that they cannot be detected by these techniques (Timonin et al.,
2014). But these are post-failure measurements that show evidence of presence of microannulus cracks in
the subsurface and require the necessity of finding a solution.
When microannulus is detected, it must be corrected by remedial jobs, squeezing cement or cement
plugs. Remedial cementing is considered as challenging technically and operationally as primary cementing
because the wellbore conditions are unknown or out of control (Nelson and Dowell, 1990). Hence, it is not
uncommon for this operation be repeated more than once. Therefore, the cement slurry should be designed
in such a way to avoid subsequent interventions.
Cement additives play a significant role to improve the characteristics of the slurry. More than 40 different
additives are present in the cements for oilfield applications (Bourgoyne et al., 1991). Expansive additives
have been applied in oil well cement systems to prevent shrinkage for more than 50 years (Thomas et al.,
2014). In some cases, the cement expands more towards the rock, particularly, when the shear modulus of the
cement is greater than the surrounding rock (Baumgarte et al., 1999). For that reason, these additives work
best in formations that are capable of resisting the expansive forces, such as hard rock formations. Effective
and permanent expansion of the cement paste in the annulus is required to sustain various conditions during
the well lifetime.
Two main mechanisms are used in the field to compensate for cement shrinkage, involving chemical
reactions and expansion which are based on crystal growth or gas generation. Expansion by gas generation
is achieved by using Mg, Al, or Zn powder as an additive (Nelson and Dowell, 1990). However, they must
be carefully stabilized inside the paste uniformly, if not, gas bubbles may channelize and allow formation
fluid to flow upward. The other mechanism comes from the formation of a crystal known as ettringite. This
SPE-191822-18ERM-MS 3

crystal is formed from the reaction of sulfates with the tricalcium aluminate in the cement compound. The
ettringite crystal replaces the lattice structure of the tricalcium aluminate in the cement due to its larger size.
This crystal replacement generates internal stress that leads to an expansion of the cement mass (Seidel and
Greene, 1985). MgO is one of the most commonly used additives for expansion (along with CaO). In these
systems, the rate of reaction and the products’ stability under downhole conditions are the key parameters to
have a successful sealing downhole. Under high pressure and high temperature (HPHT) conditions, many
of the cited additives, for instance, aluminum powder or crystal-forming products, are showing problems
related to its effectivity, controllability or both due to the expansion mechanism used (Ghofrani and Plack,
1993). If the expansion occurs at early stages of the cementing operation, the cement system will not be able
to sustain the expansive forces. Even under atmospheric conditions, tests with several cement compositions
did not result in any expansion at all, but simply a reduction in volumetric shrinkage (Rubiandini et al.,
2005). In order to improve such deficiencies, nano-MgO was engineered to improve controllability of the
expansive properties (Jafariesfad et al., 2016).
In this paper, a new cement additive is proposed. The additive is made from a shape memory polymer in
the shape of fibers. The material is initially tested in the form of particulates by Dahi Taleghani et al., (2016)
with satisfactory results; however, since the material was in the shape of particles and its large size posed
problems to its application and reduces cement tensile strength. The use of fibers is advantageous because
they keep the expanding properties but in a smaller size and a larger surface area in comparison to the
spherical particles. When exposed to temperatures above a pre-determined temperature, the additive may
expand to close potential microannulus and increase the bond strength between the casing-cement interface
and cement-formation interface. This temperature is achieved before the cement is set in the annulus space.
Additionally, the expansion benefits from the fiber shape due to the large aspect ratio of the material.
Laboratory experiments with an annular expansion ring evaluated the expansion under simulated downhole
conditions.

Shape Memory Polymer

Shape-memory polymers (SMPs) are a class of polymeric smart materials that are able to change from
a temporary shape to their permanent shape when induced by an external stimulus (trigger), such as
heating. The material needs to be programmed in order to change from a temporary shape to the original
shape once exposed to the external stimulus. During the programming, the polymer is set in a form by
conventional methods, then when deformed, the microstructure undergoes a phase change. Therefore,
the polymer undergoes a strain induced phase change. The mechanism for shape recovery relies in the
conformational entropy of the molecular segments by means of micro-Brownian thermal motion. With
temperature increasing, there is a reduction in the viscosity and an increment in the molecule mobility,
which leads to reel of molecules to their original configuration. (Li, 2014). Because of low-cost, and the
fact of being non-toxic and easy to process, SMPs have been considered in the oilfield as lost circulation
materials (Mansour and Dahi Taleghani, 2018) and proppants for hydraulic fracturing operations (Santos et
al., 2018). Preliminary studies with SMP as an expansive additive for cement have shown promising results,
with significant gains in wellbore integrity (Taleghani et al., 2016).
The SMPs used in this study are depicted in Fig. 1, before and after the expansion. These additives were
programmed at room temperature instead of the classical programming method. This process is known as
cold programming (Anthamatten et al., 2016). Cold programming occurs at temperatures below the glass
transition temperature (Tg), when the polymers are in the glassy state. In this process, the temporary shape
is achieved by means of plastic deformation, or pseudo-plastic due to its reversibility. Cold programming
has the advantage of being more time and energy efficient when compared to the classical hot programming
method. The programming includes three steps: pre-stressing, stress relaxation, and unloading (Li, 2014).
The last step, in this case, is the constrained recovery, which is divided in two components: thermal stress,
4 SPE-191822-18ERM-MS

caused by thermal expansion, and entropically stored stress. In a fully constrained recovery test, once Tg is
reached, the shape recovery cannot occur due to confinement, so, the stress is accumulated. Of course, in a
fully free recovery test, after heating for a certain period of time, the material can restore its original shape.

Figure 1—SMP fibers a) Before activation and b) After activation the fibers expanded 40% in volume.

Experimental Procedure
Besides the expansion test, a series of mechanical and rheological tests, described below, were run in
the laboratory to confirm whether the slurry characteristics are acceptable, following the API RP 10B-2
Recommended Practice for Well Cements (API, 2013).
The experiments were conducted using API class-G cement and distilled water. To determine expansion
of the slurry, SMPs fibers were added at three different concentrations by weight of cement (BWOC), 2, 4
and 6%. The fibers were programmed to expand at 150°F. The programming is done for 40% volumetric
compaction of the material in transverse directions rather than the longitudinal direction. The mechanical
properties of the SMP additives are shown in Table 2. Following its preparation, the slurry was conditioned
in a HPHT consistometer.
Due to the low density of the SMP used in this example, these particles tend to float when added to the
slurry. In order to prevent additive floating and maintain a smooth paste, the degree of thixotropy of the
cement needs to be increased by adding bentonite to the slurry. Thixotropic cements have been used for
many years; and mainly applied to reduce cement lost circulation in problematic zones and squeeze problems
(Nelson and Dowell, 1990). A 2% concentration of bentonite is enough to keep the SMPs particles from
floating in the cement paste. The slurry, however, requires a higher amount of water as displayed in Table 1.

Table 1—API Class G cement composition

Water Requirements
% Bentonite
(Gal/sk)

0 5.0
2 6.3

Table 2—Properties of the SMP fibers

Property SMP

Density (g/cm )
3 0.95
Elastic modulus at room temperature (MPa) 260
Tensile strength at room temperature (MPa) 25.5
SPE-191822-18ERM-MS 5

Expansion test
The evaluation of the cement expansion is conducted by following API RP 10B-5 (API, 2005), that provides
the standards to measure expansion of the cement sheath. As the annular ring is fully confined from top to
bottom, the expansion is linear horizontally. Following its preparation, the slurry is placed in the annular
ring expansion test and the mold is taken to a curing chamber for 24 hours to cure under 190°F or 350°F,
and 3000 psi. The circumferential expansion was measured by comparing the distance of the steel balls on
the mold before and after curing, and applying Equation (1).
(1)
where Lf and Li are the final and initial distance, respectively, measured in inches.
Compressive Strength Test. High compressive strength is desirable to prevent formation of cracks. The
cement samples are cured in cubic molds measuring 2 × 2 × 2 in. under 3000 psi and 190°F. Then, the
specimens are evaluated in a hydraulic press for unconfined compressive strength (UCS), a destructive crush
test. The exerted force is applied at a rate of approximately 1000 lbf/min.
Tensile Strength Test. API currently has no procedure to evaluate tensile strength of cement. As mentioned
in this work, tensile strength is an important property to analyze the susceptibility to formation of radial
cracks. This property is also related to the ductility of the set cement. In order to evaluate the tensile strength,
the Splitting Tensile Strength Test (or Brazilian Test) was used. The experiment consists of applying a
diametral compression force to the cylindrical sample (Fig. 2). Failure occurs by separating the specimen
at the diametral plane. This test, however, is an indirect measure of tensile strength and is not considered
uniaxial due to compressive normal stress applied in the sample. The value corresponds to be between 1.5
to 2.5 higher than the ones measured by Direct Uniaxial Tensile Strength Test (Heinold et al., 2003).

Figure 2—Splitting Tensile Strength Test with cylindrical samples before and after failure

The preparation procedure for the samples is similar to the compression test but the mold used is
cylindrical. The specimen has a 2 in. diameter and a 2 in. in height.
Rheology Test. A rotational rheometer was used to measure the slurry's rheological properties. Rheological
measurements can determine the flow characteristics of the cement slurry such as its plastic viscosity, yield
point, frictional properties, and gel strength. These properties determine the quality of the final product and
ensure that the slurry can be pumped into the well with minimum pressure drops. Viscosity is the most
significant property in this regard and it measures the relationship between the shear stress and shear rate.
It also plays a critical role in mud removal.
The gel strength is calculated to verify the susceptibility of the slurry to gas and water migration. Upon
completion of the pumping, the slutty remains in a static state. During the transition time, the cement changes
6 SPE-191822-18ERM-MS

from a fluid with hydraulic pressure capable of holding back flow to a solid material with measurable
compressive strength, is critical. Throughout this interval, there is a high susceptibility to gas migration.
Free Fluid Test. Water may separate from the slurry before setting, which may seriously affect paste
properties. In gas bearing zones, the free water can impair zonal isolation, leaving the annulus susceptible
to gas channelization. The Free Fluid Test measures the potential for this separation. The cement is allowed
to sit for 2 hours, with 0° of inclination, in a 250 ml glass tube. The test temperature is 190°F and the glass
tube is covered to prevent evaporation.
Fluid Loss Test. A fluid loss tester is used to evaluate the fluid loss from the slurry. This apparatus simulates
down-hole conditions where fluid loss can occur. The experiment is conducted at 190°F and 1000 psi. Fluid
loss to the formation has a significant influence on gas migration in the annulus. If a cement slurry loses
too much fluid, its bond strength will be compromised and costly remedial well treatments may be needed.
Additionally, poor fluid loss control in gas bearing zones accelerates the decrease of cement pore pressure

Results and Discussion

The results from the expansion tests are depicted in Fig. 3. The expansion increases linearly with of the
concentration of SMP fibers, reaching 0.61% of circumferential expansion for 6% of additive concentration
BWOC. At higher temperatures, the performance of the expansive additive was not affected significantly
while this is not the case with other commercial solutions in the market as the rate of required chemical
reactions are usually affected with the environment temperature. The SMP fiber has no chemical reaction
with the cement slurry so no significant changes in paste properties are expected at elevated temperatures.

Figure 3—Cement expansion at 190°F and 350°F, represented by

the percent circumference change with the addition of SMP fibers

The concentration of SMPs can have a significant influence on the compressive and tensile strength. Fig.
4 illustrates the relationship between the compressive strength, and tensile strength and concentration of
additive. The samples were also tested with no additives at all and with only 2% of bentonite for comparison
purposes. While the compressive strength is reduced with an increase in SMPs concentration, the tensile
strength shows a slight increase. The weak mechanical properties of the polymeric additive, shown in
Table 1 in comparison to the cement, and its relatively large size can be potential factor for the loss of
compressive strength. A small concentration of SMPs is enough to increase the tensile strength of the
cement but increasing this concentration further does not have a significant influence on increasing tensile
strength. The expansion of the additive closes potential void spaces inside the cement matrix, which may
increase its tensile strength. Commercial expansive additive, available in the market, reduce both tensile
and compressive strength of the cement past (Williams et al., 2011). The additive proposed in this paper,
SPE-191822-18ERM-MS 7

although it decrease the compressive strength of the cement sheath, it improves ductility of the cement
sheath which reduced the chance of brittle failure of the cement in the subsurface conditions.

Figure 4—a) Relationship between compressive strength and concentration of the

additive, b) Relationship between tensile strength and concentration of the additive

As mentioned above, to prevent SMP fiber floating on the top of the cement past, the thixotropy of the
cement needs to be increased and one typical way to reach this goal is by adding bentonite. The increase in
water content due to the use of bentonite lead to changes in the mixture density. As more water was used,
the density decreased by approximately 8% (Fig. 5). The density decreased even further as more additives
were combined. However, the changes do not pose significant variations in density and could be easily
compensated in the slurry design, if needed.

Figure 5—Density of the cement slurry decreases with the use of

additives due to SMP lower density in comparison to the cement.

It is notable that the rheology of the cement can be influenced by the temperature and also adding
bentonite. Bentonite tends to increase the slurry viscosity and gel strength. The addition of SMPs did not
have a significant effect on these properties, as illustrated in Fig. 6.

Figure 6—Plastic viscosity and gel strength increase by using SMP additives
8 SPE-191822-18ERM-MS

Due to the inert nature of the utilized SMP, changes in fluid loss and free fluid content are mainly related
to the addition of bentonite. Fig. 7 shows a slight decrease once the additives are combined but no significant
difference between them.

Figure 7—a) Free fluid content for the different concentrations of additive at 190°F,
b) Fluid loss for the different concentrations of additive at 190°F and 1000 psi

As shown in Fig. 4a, the limiting factor for the use of SMPs fibers, as an expansive additive, is the
compressive strength of the cement. At the highest concentration tested (6%) the compressive strength
decreased by 43%. Although this is a considerable loss, this value is still higher than the minimum
requirements for gas wells. The results also show gains in tensile strength and ductility. It is important to note
that the additive, in the shape of fibers, demonstrated gains above 30% in expansion over the same additive
in the form of particles, reported by Taleghani et al. (2016). This gain can be attributed to the larger surface
area of the fiber. At both temperatures, 190°F and 350°F, the additive demonstrated similar performance
and did not show problems at higher temperatures, as opposed to the other common expansive additives.

Conclusion
A new cement additive in the form of SMP fibers was introduced to reduce the risk of debonding of the
cement sheath and to prevent formation of microannulus cracks. The additive irreversible expansion does
not only compensate for cement shrinkage but it also closes potential microannulus. The proposed additive
increases the tensile strength of the cement paste and improves ductility of the resultant sheaths, which is
crucial to maintain sealing during and after large pressure fluctuations during hydraulic fracturing events.
Experimental results demonstrated that the expansion increases linearly with additive concentration. Tests
performed at 350°F showed that even at high temperatures the additive demonstrate significant expansions.
The improvement in tensile strength by introducing this additive can prevent formation of tensile cracks.
The additive was found to have no chemical reaction with water or cement to affect slurry design.

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