energies

Article
A Novel Experimental Investigation of Cement
Mechanical Properties with Application to
Geothermal Wells
Catalin Teodoriu *, Mi Chin Yi and Saeed Salehi
Mewbourne School of Petroleum and Geological Engineering, The University of Oklahoma, Norman,
OK 73019, USA
* Correspondence: [email protected]; Tel.: +1-405-325-6822




Received: 9 August 2019; Accepted: 30 August 2019; Published: 5 September 2019


Abstract: Geothermal well integrity has proven to be of high importance, especially because the
geothermal life span is expected to be longer than that of conventional oil and gas wells. Recent studies
have demonstrated that cement-casing interfacial bonding is a classical well failure in such wells,
but field measurements do not correlate with the simulations. We believe that this discrepancy is due
to limitations of the simulation itself, which in most cases assumes a free movement of the casing after
the interfacial bonding has been exceeded. Since the casing is cemented using a complex hardware
package such as centralizer and other cementing components, the free movement of the casing is
only possible when no-cement exists behind the casing. This paper proposes a novel experimental
method to understand cement strength properties other than the standardized unconfined cement
strength (UCS). The novel setup allows the measurement of interfacial bonding strength between
cement and casing and the pure cement shear strength. The later becomes an important parameter
as the interaction between casing couplings and cement will show. In the past, standard cement
bending tests were designed to measure cement shear, but the value obtained from such tests is not
relevant for the geothermal in situ casing-cement interaction, and thus the need for a new testing
method arose. The new method is capable to mimic the interaction between the casing connection
edges and the cement. We believe that the results presented within this paper will help engineers to
validate their numerical simulations and to optimize the geothermal well design which will result in
the increase of the well integrity for the life of the geothermal well.

Keywords: geothermal well construction; well cementing; cement shear strength; cement interfacial
bonding strength

1. Introduction
The energy harnessed from geothermal resources is a reliable and well-known resource which can
offer base load power generation. Other renewable energy forms are in general not able to provide
base load power generation without high cost investment in energy storage [1]. Drilling principles in
geothermal and oil and gas are very similar. In fact, geothermal is equivalent with the high-pressure
high temperature well classification of the later. Because of these similarities, technical problems of oil
and gas wells will also apply to geothermal ones, and thus, the engineers will follow same construction
standards and regulations. The loss of well integrity, a major concern which may cause safety issues,
environmental risks, lost time, and additional cost, is considered to be very important and an actual
problem with wells of any age and type. During the production phase, the cement behind the casing is
considered to be an important safety barrier, and therefore, a successful cementing job becomes critical
to achieve the long term well integrity [2].

Energies 2019, 12, 3426; doi:10.3390/en12183426 www.mdpi.com/journal/energies

Energies 2019, 12, 3426 2 of 14

In the work performed by Wehling [3] it has been shown that the wellbore integrity can be
seriously affected by three types of cement mechanical failure: radial cracks, de-bonding cracks or
micro annulus, and shear failure. However, those three types of failure will exist only when the
axial movement of the casing is not restricted by any geometry change of the casing string. When
geometry changes are considered, the intimate interaction between cement and casing must be studied
and considered.
The American Petroleum Institute (API) Specification 10A (API 10A) states the requirements,
properties, and conditions of use for different cement classes, thus we have used class H cement
for the experiments. Table 1 shows the classification of API cements (adapted after [4]). It must be
noted that the dry powder is called cement; however, the hardened product after cement is mixed
with water is still called cement for well construction purposes. Some authors use the term ‘cement
sheath’ to refer to the hardened cement. The cement powder mixed with water is called ‘cement slurry’
and it is very easily pumped down the hole. Once the cement slurry sets or hardens it forms the
‘cement sheath’ or simple called ‘cement’. The use of cement types and their mixtures can vary by well
depth, bottom hole temperature, and pressure as well as sulfate resistance, especially for geothermal
applications. In order to improve cement properties, a small amount of chemicals called additives
are added in order to control and modify the behavior of the cement slurry. The most common
additives can be classified in accelerators, retarders, extenders, and weighting agents. Of course, special
applications will require special developed solutions and additives. The most common cement used
in well cementing, also named oilwell cement, is the Portland cement type which sets and develops
compressive strength through the process of hydration, which is a complex chemical process generated
by the reactions between dry cement constituents and water. The main components that result from the
cement hydration are the generally named C-S-H gels and calcium hydroxide. The hydration process
of the cement primary phases can be illustrated for the different cement components as follows [4]:
during cement setting, the transition from water and anhydrous components to C-S-H gel takes place
to 30% in one day whereas the remaining 70% are completed after 28 days. Although the hydration
starts instantaneously, the process is slow (taking hours and days) and is influenced by the curing
conditions and additives.

Table 1. Portland cement classes [4].

Class Depth (ft) Temperature F Purpose

A 0–6000 80–170 Used when no special needs are required
Used for conditions requiring moderate to high sulfate
B 0–6000 80–170
resistance
C 0–6000 80–170 Used for conditions requiring high early strength
D 6000–10,000 170–290 Used where high temperatures and pressure are found
Used with accelerators and retarders to cover all range
G 0–8000 -
of well depth and temperatures
Used with accelerators and retarders to cover all range
H 0–8000 -
of well depth and temperatures

When it comes to well integrity, every casing that is cemented in place must ensure good isolation
and avoid any fluid migration during the life of the well. Geothermal wells have the same requirements
in terms of well integrity as oil and gas ones. That also implies that the surface casing which should
isolate and protect the fresh water horizons must comply with well integrity conditions and regulations.
Ichim and Teodoriu [5,6] have pointed out the importance of thermal cycles and their inevitable effect
on cement integrity. Although surface casings are not directly exposed to high temperature of the
fluid produced by a geothermal well, the casing and cement temperatures may reach elevated values
up to 100 ◦ C. This hypothesis was considered for the experiments shown in this paper and as such,
Energies 2019, 12, 3426 3 of 14

the maximum temperature used for testing was only 65 ◦ C. The temperature effect is also considered
for the interaction between coupling and cement, and this paper is introducing laboratory test results
achieved through a customized testing setup of a coupling and the surrounding cement.
In both the hydrocarbons and geothermal industry, investigations on compressive strength
of diverse cement samples under various influential factors such as: thermal variation, added
additives, and curing time have been of interest to observe their influence on well integrity issues.
Philippacopoulos et al. [7] pointed out that compressive strength might not be the main factor that
secures zonal isolation in oil, gas, or geothermal wells. Their studies indicated that other mechanical
properties of the cement, such as shear stress, bonding stress, Young’s modulus, and Poisson’s ratio
are important factors to be considered when wellbore integrity is evaluated. Teodoriu [8] introduced
the possibility of cement failure caused by shear failure, but unlike numerous compressive strength
studies of cement, the well integrity issues caused by shear failure have not been spotlighted as much.
This issue had been readdressed by [9] who showed the importance of long-term cement properties and
the need for reference numbers to be used for numerical well integrity studies. For the purpose of this
work, it is important to note that the shear strength is a mechanical property of Portland cement-based
materials analogous to the unconfined compressive strength (UCS) and the tensile strength (UTS).
The interfacial bonding shear strength studied in this paper is an interfacial property that depends on
cement and the contact material (i.e., between casing and cement); therefore, the proper name for this
mechanical property is interfacial bonding shear strength (IBSS). Interfacial can be measured in tension
or through shear, but our focus in this work is shear bonding failure.
Concrete IBSS is a very important mechanical property for the construction industry and as a
result, numerous studies have focused on measuring it. Unlike well cements, the concrete used for
civil engineering is a mix of cement with aggregates of different shapes and sizes such as sand or
gravel. The most used setup to measure the flexure strength in civil engineering is the beam shaped
structure loaded in three points, which can be indirectly used to measure shear strength. However,
this loading is different from the annular shaped cement placed around the casing in a geothermal
well. The results of the civil engineering beam tests are only focused on the cement and neglect the
cement-pipe interaction. Wong et al. [10] have conducted a very detailed experiment to measure the
direct shear strength for concrete in order to understand their shearing behavior under a given range
of confining pressure. Bejar and Rushing [11] examined the shear strength of a cylinder model of Class
H Cement with added silica fume through a finite element analysis approach. However, their main
concern was the accuracy of the cement properties used for the simulation. The first published studies
on cement interfacial bonding were presented by Evans and Carter [12] who obtained shear bonding
strength (equivalent to interfacial bonding strength described in this work) and hydraulic bonding
strength (equivalent to a leak strength) between casing and cement. The shear bonding tests (this was
the official name provided by the authors, which is the equivalent of our proposed IBSS) performed
by [12] consisted of measuring the axial force required to push a cylinder that was previously cemented
inside another cylindrical shape container. The hydraulic shear bond (HSB) was measured by pumping
water in the middle of two concentric cylinders that were cemented in place. [12] experiments were
performed on API Class A cement samples cured inside of a 2 in. pipe (inside diameter) of 10 in. length.
Experimental work on cement IBSS was also performed by [13–15]. Some of their published data will
be used as comparison for this paper and are presented later.
Using Finite Element Method, Kaldal et al. [16] and Teodoriu [8] have shown the importance of
casing coupling—cement interaction, in which the maximum stresses in a temperature loaded well
will always appear between the coupling edges and cement. Figure 1 shows the von Misses stresses
obtained by [16] The results indicate that the failure mode of cement is most likely shear (please note
the high stress concentration around the edge of the coupling). Teodoriu [8] has theoretically stated
that the shear stress will probably propagate vertically or diagonally (see the marked lines in Figure 1).
Due to the thin cement layer (normally between 10 and 30 mm), it is safe to assume that the shear
failure will most likely propagate vertically.
Energies 2019, 12, 3426 4 of 14
Energies 2019, 12, x FOR PEER REVIEW 4 of 14

Figure 1. von Mises stresses [MPa] in the cement around a Buttress type casing coupling (modified
Figure 1. von Mises stresses [MPa] in the cement around a Buttress type casing coupling (modified
after [15]).
after [15]).

The experiments presented in this work simulate the shear bonding strength between cement and
The experiments presented in this work simulate the shear bonding strength between cement
casing coupling, showing which shear failure will appear first and then comparing this with the cement
and casing coupling, showing which shear failure will appear first and then comparing this with the
ultimate compressive strength. To resemble the annular shape that represents casing/coupling, each test
cement ultimate compressive strength. To resemble the annular shape that represents
cell was customized accordingly. A standard API recipe of Class H cement has been used and the
casing/coupling, each test cell was customized accordingly. A standard API recipe of Class H cement
samples were tested for shear/bonding stress at different ages. API class H cement is very commonly
has been used and the samples were tested for shear/bonding stress at different ages. API class H
used in deep wells. The cement composition follows the requirements of API 10A Table 9.3 [17].
cement is very commonly used in deep wells. The cement composition follows the requirements of
API 10A Table 9.3.
2. Experimental Approach
In what follows,
2. Experimental the experimental approach used in this work is shown. First, the sample
Approach
preparation will be described, followed by the measurement and data collection.
In what follows, the experimental approach used in this work is shown. First, the sample
preparation will be described, followed by the measurement and data collection.
2.1. Sample Preparation
The purpose of this work is to obtain accurate mechanical properties of neat set cement only,
2.1. Sample Preparation
since additives may strongly alter the results, and thus, structured and focused research will not be
The without
possible purposeunderstanding
of this work isbasedto obtain
cementaccurate mechanical
properties. For thisproperties of neat
purpose, Class H set
neatcement
cementonly,
was
since additives
considered. may strongly
According to APIalter
10 the results,
A [18], and class
mixing thus, Hstructured and focused
cement requires 38% research
water bywill not be
weight of
possible without understanding based cement properties. For this purpose, Class
well cement. This requirement leads to using 860 g of Class H cement and 327 g of distilled water. H neat cement was
considered. According followed
The mixing procedure to API 10exactly
A (2010), the mixing class H cement
API specifications and wasrequires 38% water
as follows: by weight
the mixing of
speed
well cement. This
was maintained at requirement
4000 RPM while leads thetocement
using 860
wasgadded;
of ClasstheHcement
cementpowder
and 327 wasg of distilled
fully addedwater.
to the
The mixing procedure followed exactly the API specifications and was as follows:
mixer within 15 s during that time. After 15 s, the mixing rate switched automatically to 12,000 RPM the mixing speed
was maintained
and was at 4000
maintained RPM
for 35 while
s. All the cement used
the equipment was foradded;
mixingthe iscement powderand
API certified waswasfully added to
explained in
the
greatmixer
detailwithin 15 s during
by [19,20]. that time.
The cement slurry After
was 15 s, the inspected
visually mixing rate (toswitched
be free ofautomatically
clumps or airto 12,000
bubbles)
RPM andpoured
and then was maintained for molds:
into dedicated 35 s. All forthe
UCS equipment
cube molds used forAPI
as per mixing is API
10A [18] certified
(cubes), andshear
for pure was
explained in great detail
strength a dedicated newly bybuild
[16, 17]. The used,
cell was cement slurry
while forwas visually
interfacial inspected
bonding shear(tostrength
be free cylindrical
of clumps
or air bubbles) and then poured into dedicated molds: for UCS cube molds
pipes were used. When cement-mold bonding had to be reduced, the contact surface was coated as per API 10A (2010)
(cubes), for pure shear strength a dedicated newly build cell was used, while for
with a non-reactive release agent (grease) before the cement mixture was poured. Particularly for the interfacial bonding
shear strength
interfacial cylindrical
bonding pipes were
shear strength samples, used.
no When
grease wascement-mold
used on the bonding
metallichad
molds,to be
andreduced, the
the surfaces
contact surface was coated with a non-reactive release agent (grease) before the cement mixture was
poured. Particularly for the interfacial bonding shear strength samples, no grease was used on the
metallic molds, and the surfaces were carefully cleaned and kept free of any impurities. After a few
Energies 2019, 12, x FOR PEER REVIEW 5 of 14
Energies 2019, 12, 3426 5 of 14

minutes in which the air bubbles were monitored, the molds were placed in water baths with
controlled temperature.
were carefully cleaned andDistilled water
kept free wasimpurities.
of any used for mixing
After aand
fewcuring
minutestheinsamples.
which the Theairpressure
bubbles
was
werealways atmospheric
monitored, pressure,
the molds while in
were placed thewater
selected temperatures
baths for the
with controlled experiments
temperature. presented
Distilled in
water
this paper are room (20 °C) and elevated (65 °C) ones. The samples were cured for
was used for mixing and curing the samples. The pressure was always atmospheric pressure, while 1, 3, 7, and 14
days. Severaltemperatures
the selected room temperature samples were
for the experiments cured for
presented 35 paper
in this and 82aredays
room before the
(20 ◦ C) andshear and
elevated
bonding testsThe
(65 ◦ C) ones. were performed.
samples For reference,
were cured for 1, 3, 7, cube
and 14molds
days. were prepared
Several and used for
room temperature the same
samples were
curing days as shown above.
cured for 35 and 82 days before the shear and bonding tests were performed. For reference, cube molds
were prepared and used for the same curing days as shown above.
2.2. Experimental Setup
2.2. Experimental Setup
The experimental setup consists of an instrumented hydraulic press with a maximum capacity
of 200 The kN (or 20 tons).
experimental The
setup hydraulic
consists of anpress applies hydraulic
instrumented the axial pressload with
to the samples through
a maximum capacity of a
manufactured extension
200 kN (or 20 tons). bar while press
The hydraulic a force gaugethe
applies placed
axialbelow
load tothe thetesting
samples cell measured
through the applied
a manufactured
load. The force
extension gaugea is
bar while connected
force gauge placedto a data acquisition
below the testing system together with
cell measured a displacement
the applied load. The sensor.
force
The
gaugecells (molds) used
is connected to a for
datathese experiments
acquisition systemare placedwith
together in their corresponding
a displacement adapters
sensor. before
The cells the
(molds)
force is only
used for theseapplied to theare
experiments cement
placedused forcorresponding
in their investigations,adapterssee Figure 2. Figure
before the force3 shows a cross
is only applied
sectional
to the cementviewused
of theforshear cell with a see
investigations, similar
Figureshoulder
2. Figure as 3the one generated
shows by theview
a cross sectional casingof coupling
the shear
(Figure
cell with2A) compared
a similar withas
shoulder thetheinterfacial bonding
one generated shear
by the strength
casing couplingcell (Figure
(Figure 2B). The IBSS cell
2A) compared withuses
the
ainterfacial
slightly different
bonding shear strength cell (Figure 2B). The IBSS cell uses a slightly different principle of
principle as the cell presented by other authors. Our cell uses the cement inside as
athe
cylinder with known
cell presented and authors.
by other well measuredOur cell geometry
uses theand thus,inside
cement only oneof acontact
cylinder area
withwith the pipe
known and
exists. A singlegeometry
well measured contact area simplifies
and thus, only onethe contact
processarea andwith alsotheimproves the ability
pipe exists. A singletocontact
accurately
area
measure the interfacial bonding shear strength. The pipe is zinc plated
simplifies the process and also improves the ability to accurately measure the interfacial bonding shear with a slightly higher
roughness
strength. The than regular
pipe is zincblank
platedpipe;with ahowever, a goodroughness
slightly higher bonding than between
regularpipe andpipe;
blank cement was
however,
intended.
a good bondingFuturebetween
tests canpipe
be performed
and cement with
waspipes of different
intended. Futureroughness
tests can be and/or coatings.
performed withThe pure
pipes of
shear strength
different cells (molds)
roughness are madeThe
and/or coatings. of steel
purewith
shear low pipe roughness
strength cells (molds) and,are
asmade
mentioned above,
of steel the
with low
inner surface of the
pipe roughness and,cell was greasedabove,
as mentioned in ordertheto avoid
inner cement
surface of bonding.
the cell wasThegreased
pure shear strength
in order cell
to avoid
has a step
cement diameter
bonding. Thechange at thestrength
pure shear inner diameter,
cell has awhich has the same
step diameter changegeometry as a casing
at the inner diameter,coupling
which
downscaled
has the sametogeometry
the size as of a2 casing
inch. The adapter
coupling used for shear
downscaled to the applies
size of 2the force
inch. Theon a contact
adapter usedarea
for
(circle) that has
shear applies thethe same
force on adiameter
contact area as the smallest
(circle) that hasID ofthethe
samecell. As a result,
diameter as thethe cement
smallest IDisofsheared
the cell.
along this diameter.
As a result, the cement Theisevolution
sheared along of loadthisand displacement
diameter. was measured
The evolution of load and displacement
recorded for later was
analysis.
measured and recorded for later analysis.

(A) (B)
Figure
Figure 2. Views of
of the
the testing
testingcells
cellsmounted
mountedininthe
the press,
press, thethe interfacial
interfacial shear
shear bonding
bonding strength
strength (A)
(A) and
the shear
and strength
the shear (B). (B).
strength
Energies 2019, 12, 3426 6 of 14
Energies 2019, 12, x FOR PEER REVIEW 6 of 14

Bonding
Cement
Cell

ID

(A) (B)
Figure3.3.Shear
Figure Shearstrength (A)(A)
strength and interfacial
and bonding
interfacial shear
bonding strength
shear (B) test
strength (B)cells
testused
cellsinused
the present study.
in the present
study.
Table 2 shows the geometrical details of the constructed cells: length, outer diameter, and inner
diameter (IDA,
Table IDB).the
2 shows The shear strength
geometrical cell
details of has two inner diameters
the constructed in order
cells: length, outertodiameter,
create the square
and inner
shoulder
diameterof(IDA,
an equivalent
IDB). Thecoupling. The values
shear strength shown
cell has twoininner
Tablediameters
2 are usedinfororder
calculation based
to create the on the
square
Equations (1) and (2).
shoulder of an equivalent coupling. The values shown in Table 2 are used for calculation based on
the Equations (1) and (2).
Table 2. Geometries of the shear and bonding cells.
Table 2. Geometries of the shear and bonding cells.
Outer Diameter Inner Diameter Inner Diameter
Item Cell Length (mm)
Cell Length Outer Diameter (mm)Inner Diameter (IDA(ID
) (mm)
A)
(IDB ) (mm)
Inner Diameter (IDB)
Item
Shear Cell (mm) 49.2 (mm) 75.6 (mm) 61 (mm)54
Shear Cell
Bonding Cell 49.2 50 75.6 40 61 35.1 54 -
Bonding Cell 50 40 35.1 -
Figure 4 shows the shear strength specimens before and after testing. The cement behavior for
Figure 4 (1
fresh samples shows the shear
to 3 days strength
curing) versusspecimens
long termbefore
samplesandisafter
verytesting. The cement
interesting. Samples behavior
with lowfor
fresh samples
curing time tend(1totoshow
3 days curing)
a higher versus and
ductility longthus,
termthesamples
cementisisvery interesting.
literally extrudedSamples
from thewith low
sample,
while the long-term samples (cured over 7 days or longer) will crack and fail in a brittle mode. Figurethe
curing time tend to show a higher ductility and thus, the cement is literally extruded from 5
sample, while the long-term samples (cured over 7 days or longer) will crack
shows the shear bonding strength specimens after testing. The same behavior as above was noted. and fail in a brittle
mode.
One Figure 5 of
explanation shows the shearis bonding
this behavior strength specimens
that the incomplete after testing.
cement hydration The affects
strongly same behavior
the cement as
above was noted. One explanation of this behavior is that the incomplete cement
properties. This was particularly observed on the evolution of the cement UCS, which needs time to hydration strongly
affects
reach the cement
a good properties. This was particularly observed on the evolution of the cement UCS,
UCS value.
which needs time to reach a (measured
The pure shear strength good UCS value.
in MPa) is calculated using the following equation:

Fmax
σ= (1)
2π ∗ IDB ∗ SL

where

Fmax is the maximum recorded force, N;

IDB is the inner diameter of the shoulder, m;
SL is the shear length of cement in the cell, m.

The interfacial bonding shear strength (measured in MPa) is calculated as:

Fmax
σ= (2)
2π ∗ IDA ∗ CL

where
(A) (B)
Fmax is the maximum recorded force, N;
Figure 4. Shear strength specimens before testing (A) and after testing (B)—after testing the cement is
pushed outside the mold.
 Bonding Cell 50 40 35.1 -

Figure 4 shows the shear strength specimens before and after testing. The cement behavior for
fresh samples (1 to 3 days curing) versus long term samples is very interesting. Samples with low
curing time12,
Energies 2019, tend
3426 to show a higher ductility and thus, the cement is literally extruded from7 of the
14
sample, while the long-term samples (cured over 7 days or longer) will crack and fail in a brittle
mode. Figure 5 shows the shear bonding strength specimens after testing. The same behavior as
IDA iswas
above the inner
noted.diameter of the cell,
One explanation ofm;
this behavior is that the incomplete cement hydration strongly
CL is the
affects theinterfacial bonding shear
cement properties. This strength cell length,
was particularly m.
observed on the evolution of the cement UCS,
which needs time to reach a good UCS value.

(A) (B)
Figure
Figure4.4.Shear
Shearstrength
strengthspecimens
specimensbefore
beforetesting
testing(A)
(A)and
andafter
aftertesting
testing(B)—after
(B)—aftertesting
testingthe
thecement
cementisis
Energies 2019, 12, x FOR PEER REVIEW 7 of 14
pushed outside the mold.
pushed outside the mold.

(A) (B)
Figure
Figure 5. 5. Interfacial
Interfacialbonding
bondingshear
shear strength
strength specimens
specimens afterafter testing:
testing: (A) shows
(A) shows a cement
a cement samplesample
cured
cured for and
for 1 day 1 day(B)and (B) a long-term
a long-term cured sample).
cured sample). Note
Note that thethat the cement
cement samplesample cured
cured for onefor one
day day in
is still is
still in one whereas
one piece, piece, whereas the long-term
the long-term samplesample suffered
suffered brittle failure.
brittle failure.

To verify
The if the data
pure shear generated
strength within
(measured this research
in MPa) is comparable
is calculated using thewith other equation:
following published results,
we compared our results with previously published data 𝐹 by [12–15,21–24]. However, the published data
𝜎
is limited and allows only a qualitative comparison. (1)
2𝜋 ∗ 𝐼𝐷 ∗ 𝑆𝐿only the interfacial bonding shear strength
Also,
data could be compared since no previous work has proposed a pure shear test comparable with the
where Fmax is the maximum recorded force, N;
ones performed in this work. Also, the literature study we had performed showed that commonly,
IDB is the inner diameter of the shoulder, m;
interfacial bonding shear strength was measured after 1 day (24 h) and therefore, as presented in
SL is the shear length of cement in the cell, m.
Table 3, the results found in this research for 1 day at room temperature show comparable numbers.
The interfacial bonding shear strength (measured in MPa) is calculated as:
𝐹
𝜎 (2)
2𝜋 ∗ 𝐼𝐷 ∗ 𝐶𝐿
where Fmax is the maximum recorded force, N;
IDA is the inner diameter of the cell, m;
CL is the interfacial bonding shear strength cell length, m.
To verify if the data generated within this research is comparable with other published results,
we compared our results with previously published data by [12–14, 19–22]. However, the published
data is limited and allows only a qualitative comparison. Also, only the interfacial bonding shear
strength data could be compared since no previous work has proposed a pure shear test comparable
with the ones performed in this work. Also, the literature study we had performed showed that
Energies 2019, 12, 3426 8 of 14

Table 3. Comparison and validation of the preliminary tests of this work with the literature
published values.

Salehi et al. Lavrov and Zhao et al. Zhao et al.

Author This Work This Work
2016 Torsaer 2016 2015 2015
After 5 days Added sand After 82
Comment After 24 h - After 24 h
mixed temp. to casing days
Interfacial Bonding
81 14.5 to 145 14.5 to 362 362 to 1090 68 1450
Shear Strength (PSI)
Interfacial Bonding
0.56 0.1 to 1.0 1.0 to 2.5 2.5 to 7.5 0.47–1.94 10
Shear Strength (MPa)

As shown in Table 3, the interfacial bonding shear strength values measured after 1 day of curing
are similar to the reported values. The measured interfacial bonding shear strength after 82 days of
curing is higher than that reported by [12] but can be explained by the extended curing time used
for the experiment: 82 versus 5 days curing. All room temperature data points shown in this work
are based on a minimum of 6 experiments that were repeated to enhance the data quality. Elevated
temperature experiments were done using 4 samples for each data point.

2.3. Elevated Curing Temperature Experiments and Results

The effects of elevated temperature on cement mechanical properties were further investigated by
curing the samples for 3 days at elevated temperature set to be 65 ◦ C (±2 ◦ C). For the interfacial bonding
shear strength test, 6 samples were tested at room temperature, while only 4 samples were exposed to
elevated temperature to investigate the thermal effect on the samples. To reduce the measurement
and mixing errors, average values were calculated and used for comparison as shown in Table 4.
The elevated temperature curing affected the measured properties of the cement, specifically samples
cured at high temperature of 65 ◦ C (±2 ◦ C) showed approximately 3 times higher bonding stress in
average, see Table 4.

Table 4. Comparison between 3-day curing room temperature and elevated temperature (ET) bonding
s strength.

1st Attempt 2nd Attempt 3rd Attempt

Bonding Strenght (MPa) Average
#1 #2 #1 #2 #1 #2
3 day 4.44 6.47 6.46 7.66 6.65 9.09 6.79
3 day ET 19.52 18.42 20.54 24.88 - - 20.84

Similarly, the average pure shear strength value after 3 days of curing at room temperature was
7.28 MPa, while at an elevated temperature of 65 ◦ C (±2 ◦ C), a value of 21.04 MPa was obtained.
The measured pure shear strength at elevated temperature shows a large variation between the first and
the second attempt. We assume that this could be a result of curing temperature variance during the
curing process. Later it was also observed that the cement batch of the second samples was different,
showing slight differences from our preliminary experiments [25]. To avoid this, all other samples were
prepared from the same cement batch and the same container, while the temperature was continuously
monitored using a PC based data acquisition. Figure 6 shows the values measured for PSS and IBSS at
elevated temperatures for 3 days curing compared to room temperature at 1, 3, and 7 days of curing.
Figure 7 allows for a better comparison of the values measured at room vs. elevated temperature.
Please note that the accuracy of our measurements is less than 1%, therefore the error bars are not
visible in Figure 6.
To avoid this, all other samples were prepared from the same cement batch and the same container,
while the temperature was continuously monitored using a PC based data acquisition. Figure 6
shows the values measured for PSS and IBSS at elevated temperatures for 3 days curing compared to
room temperature at 1, 3, and 7 days of curing. Figure 7 allows for a better comparison of the values
measured
Energies 2019,at12,
room
3426 vs. elevated temperature. Please note that the accuracy of our measurements
9 ofis
14
less than 1%, therefore the error bars are not visible in Figure 6.

25

20
Shear
Elevated T
Stress (MPa)

15 Bonding
Elevated T
10 Bonding

Shear
5

0
1 2 3 4 5 6 7
Curing Days
Figure 6. Thermal effect on pure shear strength (PSS) and interfacial bond shear strength (IBSS).
Figure
Energies 2019, 12, 6. Thermal
x FOR PEER effect
REVIEW on pure shear strength (PSS) and interfacial bond shear strength (IBSS). 9 of 14

3 day curing bonding and shear

at room/elevated temperature
25
Bonding Shear
20.84 21.04
20
Stress (MPa)

15 Room T Bonding
Elevated T Bonding

10 Room T Shear
6.79 7.28 Elevated T Shear

0
3 days

Figure
Figure 7. Detailed
7. Detailed comparison
comparison of the
of the PSSPSS
andand interfacial
interfacial bondbond shear
shear strength
strength (IBSS)
(IBSS) of class
of class H
H cement.
cement.
3. Discussions
3. Discussions
Figure 8 shows the calculated equivalent PSS and IBSS for the samples used in this work. The PSS
is higher than
Figure the IBSS
8 shows thein calculated
all cases, which impliesPSS
equivalent thatand
theIBSS
cement
for will
the first de-bond
samples usedfrom thework.
in this pipe prior
The
to shear failure. However, at elevated temperatures, the IBSS seems to be affected,
PSS is higher than the IBSS in all cases, which implies that the cement will first de-bond from the showing lower
valuesprior
pipe thantoat room
shear temperature. We believe
failure. However, that this
at elevated is also due tothe
temperatures, different expansion
IBSS seems to be coefficients
affected,
showing lower and
between cement values
steelthan at room
resulting temperature.
in a lower contact. We believe that
Furthermore, this is also
the chemical due process
bonding to different
may
expansion coefficients
be affected by between
the temperature as cement
well. Byand steelatresulting
looking in a lower
the UCS increase due contact. Furthermore,
to temperature, the
we believe
chemical bonding
that the fast process
hydration maywill
process be impede
affectedthe by surface
the temperature
strong bond.as well. By looking
The interfacial at the shear
bonding UCS
increase
strength due
valuesto are
temperature,
shown in Tablewe believe
3. We that
also the fast hydration
observed a decreaseprocess
of shearwill impedeafter
strength the 14
surface
days.
strong bond.
To further The interfacial
understand bonding the
this behavior, shear strength values
unconfined are shown
compressive in Table
strength (UCS) 3. has
We been
also observed
measured. a
decrease of shear strength after 14 days. To further understand this behavior, the unconfined
compressive strength (UCS) has been measured.

25
Pa
 showing lower values than at room temperature. We believe that this is also due to different
expansion coefficients between cement and steel resulting in a lower contact. Furthermore, the
chemical bonding process may be affected by the temperature as well. By looking at the UCS
increase due to temperature, we believe that the fast hydration process will impede the surface
strong bond. The interfacial bonding shear strength values are shown in Table 3. We also observed a
Energies 2019, 12, of
decrease 3426
shear strength after 14 days. To further understand this behavior, the unconfined10 of 14
compressive strength (UCS) has been measured.

25

Pure Shear Strength, MPa

20

15

10

0
3 days 7 days 14 days
Curing Time

Elevated Temperature Room Temperature

Energies 2019, 12, x FOR PEER REVIEW 10 of 14

14
Interfacial Bonding Shear Strength, MPa

12

10

0
3 days 7 days 14 days
Curing Time

Elevated Temperature Room Temperature

Figure
Figure 8. The
8. The measured
measured pure
pure shearstrength
shear strength (PSS)
(PSS) (top)
(top)and
andinterfacial bonding
interfacial shear
bonding strength
shear (IBSS)(IBSS)
strength
(bottom) for class H cement.
(bottom) for class H cement.
The evolution of unconfined compressive strength (UCS) of the cement measured at room and
The evolution of unconfined compressive strength (UCS) of the cement measured at room and
elevated temperature was used as reference for all other measured parameters and it is shown in
elevated temperature was used as reference for all other measured parameters and it is shown in
Figure 9. The measured UCS of the cement (Class H) increases with time, and temperature leads to a
Figure 9. The
higher UCSmeasured UCSday
for the same of the cementwith
compared (Class
roomH) temperature.
increases with time,
This and temperature
behavior is normal andleads has to a
higher
been repeatedly reported in the literature. Also, the room temperature values for UCS are low but been
UCS for the same day compared with room temperature. This behavior is normal and has
repeatedly
they arereported
normal in forthe literature.
neat class H Also,
cement.theThe
room temperature
increase values
of the UCS for UCS
values infersare low
that thebut they are
other
normal for neatlike
properties class H cement.
interfacial The increase
bonding of the and
shear strength UCSpure
values infers
shear that the
strength willother
showproperties
the same like
tendency.
interfacial However,
bonding shearour experiments
strength have shown
and pure that the interfacial
shear strength will showbonding
the sameshear strength However,
tendency. does
not change for samples cured at elevated temperatures, especially day 3 and
our experiments have shown that the interfacial bonding shear strength does not change for samples7. After 14 days of
curing, a small increase of the interfacial bonding shear strength was noted, but the
cured at elevated temperatures, especially day 3 and 7. After 14 days of curing, a small increase of thevalue is lower
than the one obtained at room temperature. Although no similar tests have been found in the
interfacial bonding shear strength was noted, but the value is lower than the one obtained at room
literature, the closest experiments we found were from civil engineering, related to rebar bonding to
temperature. Although no similar tests have been found in the literature, the closest experiments we
the cement, and they also showed a lower value at elevated temperatures.
found were from civil engineering, related to rebar bonding to the cement, and they also showed a
lower value at elevated70 temperatures.
To further understand the behavior of cement pure shear strength and interfacial bonding shear
60
strength, the comparison shown in Figures 10 and 11 is provided. We have compared these properties
with the UCS of cement 50 under same curing conditions. Figure 10 shows a very good linear dependency
UCS [MPa]

between pure shear 40 strength and cement UCS; however, when interfacial bonding shear strength
is compared with UCS, it shows a strong non-linear behavior for elevated temperatures. UCS data
30
are comparable with other published experiments [26,27]. Also as mentioned above, the pure shear
20

10

0
1 3 7 14
Curing Time
 Elevated Temperature Room Temperature

Figure 8. The measured pure shear strength (PSS) (top) and interfacial bonding shear strength (IBSS)
(bottom) for class H cement.
Energies 2019, 12, 3426 11 of 14

The evolution of unconfined compressive strength (UCS) of the cement measured at room and
elevated
strength datatemperature
at elevatedwas used as reference
temperature for all other
shows a decline measured
of shear with theparameters
increase of and it is
curing shown
time. We in
also
Figure 9.the
obtained The measured
same resultsUCS
afterofrepeating
the cement
the(Class H) increases
experiments. with
Figure 11time,
showsand temperature
the behavior ofleads to a
interfacial
higher UCS
bonding shearfor the same
strength. It day
can becompared
observed with
thatroom temperature.
the bonding This has
strength behavior is normal
a nonlinear and has
behavior that
been repeatedly reported in the literature. Also, the room temperature values
is very strong at room temperature. A logarithmic trend line was found to fit very well thisfor UCS are low trend.
but
they
The are normal
elevated for neatvalues
temperature class Harecement. The the
lower than increase of the UCS
ones measured valuestemperature
at room infers that the other
conditions.
properties like interfacial bonding shear strength and pure shear strength will show the same
Consequently, the bonding strength does not evolve continuously with the cement hydration, hence
tendency. However, our experiments have shown that the interfacial bonding shear strength does
curing, but instead reaches a maximum value faster and stays constant. This has strong implications
not change for samples cured at elevated temperatures, especially day 3 and 7. After 14 days of
for the understanding of well integrity and long-term behavior of the well. Our experiments focused
curing, a small increase of the interfacial bonding shear strength was noted, but the value is lower
on 14 days curing time, but longer curing time experiments may prove this concept. Unfortunately,
than the one obtained at room temperature. Although no similar tests have been found in the
there are no similar experiments in the literature that would allow a comparison with the results in
literature, the closest experiments we found were from civil engineering, related to rebar bonding to
this paper.
the cement, and they also showed a lower value at elevated temperatures.
Energies 2019, 12, x FOR PEER REVIEW 11 of 14

70
To further understand the behavior of cement pure shear strength and interfacial bonding shear
60
strength, the comparison shown in Figures 10 and 11 is provided. We have compared these
properties with the 50 UCS of cement under same curing conditions. Figure 10 shows a very good
linear dependency between pure shear strength and cement UCS; however, when interfacial
UCS [MPa]

40
bonding shear strength is compared with UCS, it shows a strong non-linear behavior for elevated
temperatures. Also 30 as mentioned above, the pure shear strength data at elevated temperature shows
a decline of shear20with the increase of curing time. We also obtained the same results after repeating
the experiments. Figure 11 shows the behavior of interfacial bonding shear strength. It can be
observed that the 10 bonding strength has a nonlinear behavior that is very strong at room
temperature. A logarithmic
0 trend line was found to fit very well this trend. The elevated
temperature values are lower 1 than the 3ones measured7 at room temperature 14 conditions.
Consequently, the bonding strength does not evolve continuously
Curing Time with the cement hydration, hence
curing, but instead reaches a maximum value faster and stays constant. This has strong implications
Room Temperature
for the understanding of well integrity and long-termElevated Temperature
behavior of the well. Our experiments focused
on 14 days curing time, but longer curing time experiments may prove this concept. Unfortunately,
areFigure
thereFigure 9. The
no9.similar
The measured unconfined
experiments
measured cement
in thecement
unconfined strength
literature that(UCS)
strength would
(UCS) atatallow
room
roomand elevated
aand
comparisontemperatures
elevated with thefor
results
temperatures for in
this paper.
class H cement. class H cement.

35

30 y = 0.4004x + 0.3523
Pure Shear Strength [MPa]

R² = 0.9917
25

20

15 Room Temperature
Elevated Temperature
10

0
0 20 40 60 80
UCS [MPa]

Figure
Figure 10.
10. Correlation
Correlationbetween
betweenunconfined
unconfinedcement
cementstrength
strength(UCS) and
(UCS) pure
and shear
pure strength
shear of of
strength class H
class
H cement. cement.

14 y = 6.4064ln(x) - 11.271
Strength [MPa]

R² = 0.9997
12

10

8
 0
0 20 40 60 80
UCS [MPa]

Energies 12, 3426

2019, 10.
Figure 12 of 14
Correlation between unconfined cement strength (UCS) and pure shear strength of class H
cement.

14 y = 6.4064ln(x) - 11.271

Interfacial Shear Bond Strength [MPa]

R² = 0.9997
12

10

6 Room Temperature

y = 0.0809x + 3.1213 Elevated Temperature

4
R² = 0.991
2

0
0 20 40 60
UCS [MPa]

Figure 11. Correlation between unconfined cement strength (UCS) and interfacial bonding shear
strength of class H cement.

4. Conclusions
The lack of data for class H cement pure shear strength (PSS) and interfacial bonding shear
strength (IBSS) was the main driver for this paper and the experiments herein. The experiments were
performed for two curing temperatures: room temperature (20 ◦ C) and elevated temperature (~65 ◦ C).
For the first time, a novel setup allows to differentiate between pure shear strength and interfacial
bonding shear strength.
The new proposed method to evaluate cement interfacial bonding shear strength produced
results similar with data published for one day (the only available). However, our unique method to
estimate cement pure shear strength has been proven to be an excellent addition to estimating cement
mechanical properties. Our investigations have shown some scattering of data at elevated temperature,
but low temperature results showed excellent quality.
Long term measurements make this work unique by showing that interfacial bonding shear
strength does not increase linearly. The interfacial bonding shear strength was measured for a curing
time longer that 24 h, as most other papers have shown. The results clearly show the implications and
the need of investigating long term behavior of well cements.
The following observations can be made:

• Pure shear strength for specimens cured at elevated temperature is higher than that for specimens
cured for the same days at room temperature, which was expected.
• The value of interfacial bonding shear strength for specimens cured at elevated temperature
is lower than the one obtained in room temperature conditions and it does not increase as
strongly as we observed for room temperature conditions. This observation is new and has never
been published.
• The measured pure shear strength for specimens cured at elevated temperature was 17.1 MPa
which is 2.1 times greater than it was at room temperature for day 3. After 14 days, a decrease of
the pure shear strength occurs, although the UCS was minimally increasing.

Author Contributions: Conceptualization: C.T.; Methodology: C.T.; Formal Analysis: C.T., S.S.; Experimental
Work: C.T., M.C.Y.; Writing-Original Draft Preparation: C.T.; Writing-Review & Editing: C.T., S.S.; Supervision of
Experiments: C.T.
Funding: This research received no external funding.
Energies 2019, 12, 3426 13 of 14

Acknowledgments: We would like to thank to Central Plains Cement Company for their support with
cement materials.
Conflicts of Interest: The authors declare no conflict of interest.

Nomenclature
A Area, m2
B Correction coefficient for Hashin-Shtrikman 3-phase boundaries
k Thermal conductivity, W/m-K or BTU/hr-ft-◦ F
L Thickness, m
Q Amount of heat transferred through material, W
∆T Temperature gradient, K
m Water fraction inside the pores, -
ϑ Component mass fraction, -
φ Cement porosity, -

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