Powder Technology 342 (2019) 585–593

Contents lists available at ScienceDirect

Powder Technology

journal homepage: www.elsevier.com/locate/powtec

Rheology of a colloidal suspension of carbon nanotube particles in a

water-based drilling fluid
Kanjirakat Anoop a, Reza Sadr b,⁎, Rommel Yrac c, Mahmood Amani c
a
Micro Scale Thermo Fluids (MSTF) Laboratory, Mechanical Engineering Program, Texas A and M University at Qatar, Education City, Doha, Qatar
b
Department of Mechanical Engineering, Texas A and M University, College Station, TX, USA
c
Petroleum Engineering Program, Texas A and M University at Qatar, Education City, Doha, Qatar

a r t i c l e i n f o a b s t r a c t

Article history: High-pressure and high-temperature rheology of a nanomud suspension is studied. The nanomud is prepared by
Received 22 November 2017 dispersing a water-based drilling mud suspension with multi-walled carbon nanotubes (MWCNT). Effect of
Received in revised form 26 September 2018 nanoparticle concentration, shear rate, pressure, and temperature are investigated. The pressure and tempera-
Accepted 10 October 2018
ture are independently varied from ambient conditions to 170 MPa and 180 °C respectively. The results presented
Available online 12 October 2018
show that the addition of CNT increases the viscosity of the drilling mud. A shear thinning non-Newtonian behav-
ior is observed for the basemud and the nanomud samples at all pressures and temperatures. The basemud
showed an increase in viscosity with an increase in pressure. However, with CNT particle addition this trend is
observed to have reversed. For the basemud and the nanomud at lower concentrations, the viscosity values
are observed to have initially increased with the increase in temperature and to have reduced beyond 100 °C.
For a higher particle loading, a consistent decrease in viscosity with temperature is observed. The behavior of
higher concentration nanomud samples with respect to pressure and temperature are seen to follow a similar
trend to that of water. It is reasoned that an adequate addition of CNT nanoparticles helps retain the mud particles
in a more homogenous and stable state, where they are held within the CNT chains. However, with further addi-
tion of CNT nanoparticles, the mud particles become agglomerated with the long chains of CNT, eventually sep-
arating water from the drilling fluid mixture.
© 2018 Elsevier B.V. All rights reserved.

1. Introduction
A proper selection of the drilling fluid, or a drilling mud, is vital in
minimizing the cost and time required for the drilling process. The cir-
culating drilling fluid aids in cooling and lubricating the drilling bit
and in removing the rock cuttings from the drilling well [1,2]. Rheolog-
ical characteristics of the drilling mud are vital as these influence many
processes. Regulating the mud properties would help to reduce prob-
lems during drilling, such as drag, circulation loss, stuck pipes and for-
mation damage, as well as improving wellbore instability.
New ventures for deep-sea drilling at extreme depths encounter
high-temperature and high-pressure (HTHP) conditions. These extreme
conditions result in overheating of drilling equipment and malfunction
due to lost circulation, posing a severe limitation to the drilling fluid
used. Several studies have been conducted to enhance the rheological
and thermal properties of water-based drilling muds under such condi-
tions. Owing to their enhanced thermo-physical properties and stable
nature, it is recommended to use suspensions of nanoparticles along
⁎ Corresponding author at: Department of Mechanical Engineering, Texas A and M
University, College Station, TX 77842, USA.
E-mail address: reza.sadr@tamu.edu (R. Sadr).
with drilling fluids for these conditions [3,4]. Nanofluids, by definition,
are colloidal suspensions containing nano-sized particles (1-100 nm)
in a basefluid. There have been numerous reports showing enhanced
thermo-fluid characteristics for nanofluids [5] with no clear explana-
tions as to the physical reasons for the reported thermal enhancements.
The nanomud suspension can be thus defined as drilling mud suspen-
sion that contains nano-sized particles. The nanoparticles are expected
to improve the mechanical, rheological and thermal properties of the
drilling fluid, according to recent studies [6–10].
Rheological characteristics of nanofluids prepared from various
types of nanoparticles were studied in the past [11]. Anoop and Sadr
[12] provided a work on the nano-Particle Image Velocimetry (nPIV)
measurement in nanofluids that explains the reported viscosity en-
hancement. However, as the present work considers nanomud suspen-
sions prepared by adding multi-walled carbon nanotubes (MWCNT)
into the drilling fluid, only literature relevant to CNT nanoparticle addi-
tion is considered here. CNT based nanofluids is found to be advanta-
geous due to its higher thermal conductivity and efficient mechanical
properties [13,14]. Based on the shape, two categories of CNTs, namely
single-walled CNTs (SWCNT) and multi-walled CNTs are available.
Most of the studies have shown the shear thinning behavior for
MWCNT-based nanofluids prepared in water and ethylene glycol

https://doi.org/10.1016/j.powtec.2018.10.016
0032-5910/© 2018 Elsevier B.V. All rights reserved.
586 K. Anoop et al. / Powder Technology 342 (2019) 585–593
[15–18]. Ponmozhi et al. [19] demonstrated the shear thinning nature of
CNT-water nanofluids and observed that the viscosity increased with an
increase in the particle addition. However, Chen et al. [20] observed
Newtonian behavior for MWCNT suspensions in silicon oil and glycerol.
Halelfadl et al. [21] observed that water-based CNT nanofluids behaved
in a Newtonian manner at low particle concentration. They also ob-
served that the relative viscosity of nanofluids at high shear rate was in-
dependent of the temperature. Singh et al. [22] observed an exponential
decrease in the viscosity of CNT-ethylene glycol nanofluids with an in-
crease in temperature.
Initial studies using nanoparticles in a drilling mud were conducted
by Amanullah et al. [27]. They reported the usage of nanoparticle-based
drilling fluid improved the rheological stability as well as reducing its
differential pipe sticking nature. They observed the nanomud suspen-
sion was superior to the bentonite fluids in reducing mud filtration
and in enhancing rheological characteristics. Based on the low pressure,
low temperature (LPLT) filtration and rheological tests on nano-sized
silica particles into water-based mud samples, Salih et al. [7] observed
that very small concentrations (0.1–0.3 wt%) of the nanoparticles
could enhance the rheological, hydraulic and filtration properties of
the drilling fluid. They suggested that a smart, water-based drilling
fluid that could replace oil-based drilling fluids might be made with
the introduction of these nanoparticles. Samsuri and Hamzah [9] ob-
served the quantity of the lifted cuttings increases when MWCNTs
were added to the drilling mud. The increase in the viscosity of
nanomud results in an increase in the lifting capacity as well as the sta-
bility of the drilling mud. Srivatsa and Ziaja [28] used silica nanoparti-
cles, along with biopolymer and surfactant blend, to reduce filtrate
loss. Ismail et al. [8] demonstrated a reduction in the coefficient of fric-
tion while using MWCNT in drilling fluids when compared with that of
the basemud. Zoveidavianpoor and Samsuri [29] observed that nano-
sized tapioca starch, added to water-based drilling fluid, performed bet-
ter than the micron-sized particles when compared in terms of viscos-
ity, yield point, gel strength and fluid loss. Sedaghatzadeh et al. [30]
experimentally investigated the influence of the addition of carbon
nanotubes (CNT) on the thermal and rheological properties of a drilling
fluid. The thermal conductivity value of the CNT-drilling fluid was ob-
served to have increased by 23% for particle loading of one volume per-
centage. The addition of functionalized multi-walled CNT to water-
based drilling fluid also increased the plastic viscosity, yield point, and
annular viscosity when compared to the base fluid. In another study,
Sedaghatzadeh and Shahbazi [31] investigated the effect of nanoparticle
geometry and particle aggregation on the induced formation damage
for water-based drilling fluid. Nano-sized, CaCO3 SiO2, and multi-
walled CNT particles were considered in that study. Nanoparticles
with tubular shapes (MWCNTs) were observed to create the highest
mud cake quality when compared to spherically shaped particles, thus
imparting the lowest level of formation damage. Fazelabdolabadi et al.
[32] observed that the addition of CNT has enhanced the thermal con-
ductivity of the drilling fluid up to 40.3% along with a reduction in plas-
tic viscosity values in comparison with the basefluid. Hassani et al. [6]
studied the heat transfer properties of drilling mud with nanoparticles
such as zinc oxide, silica MWCNT and a hybrid of CNT with silica nano-
particles. Thermal conductivity was enhanced by 22% and 16.9% for the
2% volume fraction of ZnO and SiO2, respectively. More than two times
improvement in rheological properties, such as apparent viscosity, plas-
tic viscosity, and yield point, was observed for nanomud samples with
0.5 wt% nanoparticle loading. However, rheological characteristics in
both of the above studies were conducted at atmospheric conditions,
and the effect of pressure on viscosity was not investigated. William
et al. [33] investigated the rheology of water-based drilling fluids up
to 10 MPa when CuO and ZnO nanoparticles were added to it and ob-
served that the nanofluids helped to stabilize the viscosity at higher
temperatures. Needaa et al. [10] added sepiolite nanoparticles to ben-
tonite based drilling mud to control filtration loss and rheological prop-
erties. The effect of temperatures up to 180 °C and pressures up to
45 MPa were studied. The addition of nanoparticles was observed to
have improved the stability of the drilling fluids as well as reduce fluid
loss, especially at high temperatures and pressures.
As seen from the literature review, most of the studies with
nanomuds were conducted at low pressure-temperature conditions,
mostly limited to analyzing filtrate and heat transfer performances of
the drilling fluids. In the present work, rheology of water-based drilling
fluids with CNT nanoparticles are studied in detail at high temperature
and high-pressure conditions. The effect of pressure and temperature
are independently studied for the various particle loadings of the nano-
particles at different applied shear rates. Viscosity values are measured
up to a maximum pressure of 170 MPa, with temperatures ranging
from ambient to 180 °C, conditions that are closer to an actual deep
oil-drilling environment. Details of the experimentation and the results
are presented next.
2. Experimentation
2.1. Drilling mud and MWCNT-nanofluid (CNT-nanomud) preparation
Dispersing the nanoparticles into the basefluid is an important step
in the formulation of the nanofluid. Mechanical and chemical methods
are used to disperse the MWCNT into a basefluid. Adding surfactants
and functionalization of CNT surface are the chemical methods used in
stabilizing a CNT-based nanofluid [23]. Surfactants reduce the agglom-
eration of the particles by changing the wetting nature, whereas surface
functionalization uses acids at high temperature to create –COOH and –
OH groups on the surface of the nanotubes. In mechanical dispersion,
ultrasonication is used to disperse the particles in the basefluid. Garg
et al. [24] showed that an increase in time for ultrasonication would re-
sult in breakage of CNT which ultimately changes its aspect ratio. For
1 wt% MWCNT concentration, 40 min of sonication time was found to
be optimal for proper formulation of the dispersion [25]. Derakhshan
et al. [26] prepared MWCNT nanofluid using ultrasonication for 6 h
and without using any surfactant. The suspension was observed to be
stable for 24 h without any agglomeration or sedimentation. They also
observed a time-dependent shear behavior and argued that the time-
dependent agglomeration and de-agglomeration kinetics under shear
changed the structural network of the nanofluid. Hence, for experi-
ments that are performed quickly after preparation, mechanical disper-
sion by ultrasonication seems to be sufficient.
In this work, the CNT-drilling mud mixture (henceforth termed as
CNT-nanomuds) is formulated using a top-down approach. Initially,
the water-based drilling mud (typically called as the basefluid or the
basemud) is prepared. Barium sulfate, also known as barite, is com-
monly used as a weighing agent for drilling mud to subdue the high for-
mation pressure and to achieve a zero-blowout operation. Bentonite,
which is mostly montmorillonite, provides the mud with the viscosity
needed for the removal of rock cuttings. To isolate the effects that
would be brought by other drilling fluid additives, in the present
work, only barite and bentonite are used in the preparation of the dril-
ling mud (basemud). Appropriate amounts of barite and bentonite are
mixed into the drill water to prepare the basemud. The water-based
mud (WBM) prepared in the study contains 1% and 7% of barite and
bentonite by weight, respectively, with a 12.5 ppg (pounds per gallon)
as the final density. The bentonite was initially mixed with the drill
water and aged for approximately 16 h of hydration to form pre-
hydrated bentonite (PHB). The weighing agent was incorporated in
the last 10 min of mixing. The particle size distribution of the barite
and the bentonite particles are measured using a laser-diffraction parti-
cle size analyzer (Beckman Coulter, LS13 320) and is shown in Fig. 1 (a).
The bentonite particles had a wide variation in size with two peaks, one
for lower than a 1 μm diameter and the other having an average value of
10 μm. The barite particles had an average particle diameter of 30 μm.
The CNT-nanomud samples are prepared by adding appropriate
amounts of carbon nanotubes into the drilling fluid (basemud).
 K. Anoop et al. / Powder Technology 342 (2019) 585–593
Fig. 1. (a) Particle size variation for bentonite and barite particles (b) SEM image of the multi-walled carbon nanotubes.
Commercially procured (773,840 Aldrich) multi-walled carbon nano-
tubes (≥98% carbon basis, O.D. × I.D. × L- 10 nm ± 1 nm × 4.5 nm ±
0.5 nm × 3-~6 μm) were used to prepare the nanomuds samples. The
scanning electron microscopy (SEM) image of the nanotubes is shown
in the figure (Fig. 1(b)). A stable dispersion is achieved by using an in-
tensified ultrasonication with a probe-type sonicator (QSonica S-4000,
20 kHz) to deagglomerate particles in the solution. The nanomud sus-
pension was sonicated for 40 min as suggested in the literature for
CNT-based nanofluids [24]. During ultrasonication, the temperature
would increase, resulting in some vaporization of water content from
the drilling mud. To reduce this effect, the sample was kept in a temper-
ature controlled bath (maintained at 15 °C) while applying the sonica-
tion. A qualitative observation of the nanomud samples showed no
significant sedimentation of particles in a stationary vessel, even 6 h
after preparation. Nevertheless, the rheology experiments were con-
ducted immediately after preparing the samples to avoid any sedimen-
tation. Apart from the basemud (drilling mud), four CNT-nanomud
concentrations are studied in this work for their rheological characteris-
tics. CNT concentrations were varied at 0.027%, 0.056%, 0.11% and 0.22%
by mass (henceforth represented as wt%).
2.2. Experimental setup
A high-pressure, high-temperature (HPHT) viscometer, Chandler
Viscometer 7600, was used for the rheological analysis. This state-of-
the-art viscometer is designed for rheological studies of drilling fluids
while subjected to varying well conditions in accordance with ISO
10414-1, 10,414–2 and API 13 recommended practices [34]. The system
is controlled using a computer-based program that provides multi-axis
data display options, automatic instrument control and calibration fea-
tures. It is a Couette type of viscometer with a bob (1.725 cm radius
and 3.805 cm height) and a rotor cylinder configuration. The fluid sam-
ple is kept in and around the annular space between the bob and rotor
cylinders. The shear stress (torque) created between a stationary bob
and the rotating rotor is measured using a precision torsion spring and
a high-resolution encoder in accordance with ISO/API specifications.
Known sample shear rates are created between the bob and rotor
using predefined bob/rotor geometry and a stepper motor subsystem
providing rotational speeds ranging from 0 to 900 rpm (0–1533 s−1).
Suspended solids in the sample are circulated during a test using a heli-
cal screw on the outer side of the rotor. The rotation of the rotor cylinder
at a given shear rate imparts deflection to the bob cylinder. The angular
deflection of the bob is detected and recorded by an encoder. The appar-
ent viscosity is estimated as the ratio of shear stress to shear rate.
587
Further information of the viscometer and its construction could be
seen in our earlier works [35,36].
2.3. Experimental schedule
In the present work, high-pressure and high-temperature experi-
ments are conducted to study the rheological characteristics of the
basemud and the CNT-nanomud suspensions. Effects of temperature
and pressure on the viscosity of the suspension are investigated. As
the variation of both pressure and temperature would influence the
measured viscosity values of the suspension, two independent experi-
mental schedules are performed. Automated measurements are re-
corded once the pressure and temperature values of the sample have
reached the set values. Prior to the actual experimentation, the viscom-
eter was calibrated using a standard fluid (RT100 silicon oil) with a
known viscosity value. Fig. 2 shows the two experimental schedules
used in the present study. Schedule I, where the effects of temperature
on the viscosity of the samples are studied, is depicted in Fig. 2(a).
This Figure shows that after measurements are taken at atmospheric
pressure and temperature, the pressure of the system is ramped to
and maintained at a value of 171 MPa. During the measurements, the
maximum variation in pressure is observed to be within ±0.8 MPa.
While maintaining a steady high pressure at 171 MPa, the temperature
of the sample is increased from 26 °C to 175 °C. For each experimental
point, the shear rate is varied. Shear rates of 5, 10, 51, 102, 170, 340,
511 and 1021 s−1 are used in the present study where the bulk temper-
ature is maintained constant within ±1.2 °C during the measurements.
Fig. 2 (b) shows the schedule II, where the effect of pressure on viscosity
values is investigated. Here, the temperature is kept constant (at room
temperature, 26 °C) and the pressure is ramped in stages. For both
schedules, measurements are recorded for each set point at a sampling
rate of 1 Hz for one minute where the pressure and temperature remain
within the mentioned range. The experimental uncertainties of all the
derived quantities were evaluated using the standard propagation of er-
rors principle and are plotted with a confidence of 95%.
3. Results and discussion
After conducting the initial calibration and repeatability experi-
ments with the basemud, experiments with CNT-nanomud samples
are performed to study the effect of pressure, temperature, shear rate,
and particle loading on the sample viscosity.
Prior to the rheological analysis at high temperatures and pressures,
the viscosity measurements at ambient condition are discussed. Fig. 3
588 K. Anoop et al. / Powder Technology 342 (2019) 585–593
Fig. 2. Experimental schedule used in the present study. (a) Experiment Schedule I: Pressure kept constant (171 MPa) and temperature increased. (b) Experiment Schedule II:
Temperature kept constant (Room temperature) and pressure is increased.
shows the viscosity variation of the basemud and the CNT-nanomud
samples as a function of shear rates for different CNT loading. Only
shear rates of N50 s−1 are considered in the plot, as the viscosity values
of the basemud were below the uncertainty limits at lower shear rates.
This figure shows that the viscosity values increase non-linearly at
lower CNT loading and then decrease slightly with CNT loading beyond
0.05 wt%. However, after 0.1 wt% this trend reverts, and the viscosity
values are again observed to increase with particle loading. The line
shown in Fig. 3 is a cubic fit for the data recorded at the highest shear
rate of 1021s−1. The viscosity variation with CNT particle concentration
is observed to be similar for other shear rates as well. At a given CNT
loading, a lower shear rate condition is observed to generate higher ap-
parent viscosity values than the higher shear rate conditions. This indi-
cates a shear thinning behavior of the CNT mud samples. This trend may
be better understood when the viscosity is presented as a function of
shear rate.
Fig. 4(a) shows the variation of viscosity with shear rate for three dif-
ferent conditions. The effect of shear rate at ambient condition, at room
temperature and elevated pressure, and at elevated temperature and
pressure conditions (as shown in Table 1) are compared. The linear
trend in the log-log plot of viscosity versus shear rate shows the viscos-
ity value reduces with an increase in shear rate following a power law
trend. Shear-thinning nature is observed for both the basemud and
the nanomud samples at all experimental conditions. The lines drawn
on the plot shows the power law fit for the basemud and the nanomud
with 0.11 wt% CNT using the equation given below.
η ¼ Aγ −B ð1Þ
The intercept (A) and slope values (B) for the curve are shown in
Table 1. It is observed that an increase in pressure and temperature in-
creases the slopes of the curve for both the basemud sample and the
nanomud samples. The slope values of the basemud and the nanomud
samples are comparable for a given condition, showing that particle ad-
dition did not have much influence on the shear thinning nature. How-
ever, as the intercept values (values of ‘A’ in Table 1) are observed to
have increased for the nanomud samples when compared to the
basemud, it could be argued that the apparent viscosity values have
substantially increased by CNT particle addition.
 K. Anoop et al. / Powder Technology 342 (2019) 585–593
1000
γ=51 s-1 γ=340 s-1
γ=102 s-1 γ=510 s-1
γ=170 s-1 γ=1021 s-1
100
η[cp]
10
1
0.00 0.05 0.10
CNT loading [wt%]
Fig. 3. Effect of CNT particle loading at ambient conditions (atmospheric pressure and 26 °C).
Fig. 4(b) shows the normalized viscosity variation with shear rate for
the data presented in Fig. 4(a). The viscosity values of the nanomud sam-
ples are normalized with respect to the viscosity values of the basemud
samples. It is observed that, except for lower shear rates, the viscosity
values of the nanomud samples are at least 3 to 5 times higher than
that of the base mud for a given pressure, temperature and shear rate.
It can be noted that both the basemud and the CNT-nanomud sam-
ples are non-Newtonian in nature and highly shear-dependent. Hence,
it is helpful to compare the behavior of the nanomud with that of the
basemud at a selected shear rate. Based on the repetition of experi-
ments, the readings at the highest shear rate (600 RPM) seem to be
more reliable with lower uncertainty values. Hence, viscosity values
measured at this shear rate (1021 s−1) are considered for further com-
parison and analysis in the present work. The effect of an increase in
pressure on viscosity values of the nanomud is analyzed first.
Viscosity variation with pressure at a constant temperature of 26 °C
and for a shear rate of 1021 s−1 is shown in Fig. 5. Viscosity values are
normalized with the corresponding values measured at atmospheric
pressure (ηo,p) as provided in Table 2. This table shows that, at the at-
mospheric conditions, the viscosity values for 0.22 wt% CNT-nanomud
is almost 5 times more than that of the basemud. The trend in Fig. 5
shows an increase in viscosity of the basemud with an increase in pres-
sure. However, with CNT particle addition, this trend is observed to have
reversed. The dashed lines plotted are a cubic fit for the data points to
distinguish these trends. The solid line is the viscosity of water obtained
theoretically at 25 °C [37]. The viscosity increase for a colloidal suspen-
sion with an increase in pressure is an expected trend. A similar trend
was observed in our earlier studies of alumina particles-silicon oil
nanofluids [35]. However, here, the trends for the basemud and the
nanomud with CNT are quite different. With the CNT particle addition
to the basemud, the slope of the curve reduces and eventually becomes
negative. At a particle loading of 0.22 wt% CNT, viscosity values at higher
pressures are observed to be lower than those observed at ambient
pressure. The slightly anomalous trend for the viscosity variation of
water with pressure is included for comparison, showing a very low-
order negative pressure dependence at room temperature [37]. It can
be seen that, as CNT loading is increased, the trend of the basemud
tends towards that of water. Ideally, the basemud has bentonite and
barite particles suspended in water. It may be reasoned that adequate
addition of CNT particles help to form a stable network of CNT chains
589
0.15 0.20 0.25
where the mud particles are held within it. However, the addition of
CNT beyond a certain concentration causes agglomeration of the ben-
tonite and barite particles to the linked network created by the
entangled CNT, separating the water and making a less homogeneous
suspension. In other words, a homogeneous matrix can only be main-
tained at lower CNT concentrations, where the mud particles are
retained within the long chains of CNT particles. This could be a reason
for the observed viscosity trend leaning towards that of water at high
CNT particle concentrations.
Fig. 6 shows the variation of the normalized viscosity for the mud
(by its value at 37 °C and 171 MPa shown in Table 2) at different tem-
peratures and at a shear rate of 1021 s−1. The dotted line shows the
trend (cubic fit) for the basemud and the nanomud samples, whereas
the solid line depicts the variation of viscosity of water at 100 MPa
[37]. Viscosity values should ideally decrease with an increase in tem-
perature. However, for the basemud, the viscosity values are observed
to have initially increased with an increase in temperature beyond
100 °C, and then begin a decreasing trend. A similar trend is observed
for CNT-nanomud samples at lower concentrations, but the trend
changes as the CNT concentration increases. The results presented in
Fig. 6 suggest that, for particle loading of 0.11 wt%, there is a plateau re-
gion of minor viscosity variation for the mud at temperatures below 130
°C, and then, for higher concentrations, a consistent decrease in viscosity
with temperature is observed. Similar to the observation for pressure,
an increase in temperature creates a trend leaning towards that of
water when the CNT concentration is increased. Again, the formation
of the mud particle-CNT chain structure could be reasoned for this
trend. Fig. 7 shows a scanning electron microscope (SEM) image of
the basemud and the basemud with CNT particles added to it. The
SEM images are taken after drying the liquid sample on a carbon sub-
strate. Fig. 7(a) shows the flake-like structure that is normally seen for
bentonite particles. Fig. 7(b) shows the image with the CNT addition.
After CNT particles are added, large agglomerates of bentonite particles
held up by web-like structures are observed. Fig. 7(c) shows a close-up
view of the CNT particles as well. These observations vindicate our rea-
soning that CNT particles help to keep the mud particles in a matrix. This
observation is qualitative in nature as the images are taken on dried
samples and may not accurately reflect the situation in suspension.
Finally, the effect of CNT loading on plastic viscosity (PV) values is
analyzed. Fig. 8(a) shows the variation of relative plastic viscosity with
590 K. Anoop et al. / Powder Technology 342 (2019) 585–593

Fig. 4. (a): Viscosity variation with shear rate at (a) at atmospheric pressure and 26 °C (b) at 171 MPa and 26 °C and (c) 171 MPa and 176 °C. Fig. 4 (b): Viscosity ratio (viscosity of nanomud
to viscosity of the basemud) variation with shear rate at (a) at atmospheric pressure and 26 °C (b) at 171 MPa and 26 °C and (c) 171 MPa and 176 °C.

pressure. The experimental observation is made with a constant tem- Here θ represents the dial reading, and the subscript represents the
perature of 26 °C and pressure increasing from atmospheric to corresponding viscometer rpm.
171 MPa. Relative plastic viscosity is defined as the ratio of the plastic At atmospheric pressure, the PV values of the nanomud are observed
viscosity of CNT-nanomud to that of the basemud. Plastic viscosities to be higher than that of the basemud. Thus, the addition of CNT made
are used in the oil industry and are determined from the dial readings the suspension stiffer. The increase in pressure is observed to
at 600 and 300 rpm from the viscometer as given below [38]. reduce the relative plastic viscosity values. For CNT loading up to
0.056 wt%, the increase in pressure did not have much effect on the rel-
PV ¼ θ600 −θ300 ð2Þ ative increase of PV. However, for higher CNT loading, an increase in
pressure is observed to have reduced the plastic viscosity values. Thus,
at high-pressure applications, CNT addition appears to be beneficial as
it improves the thermal properties require a reasonable increase in
Table 1 pumping power. The concentration of CNT particles needs to be pru-
Intercept and slope values fitted with power-law for basemud and 0.11 wt% nanomud. dently decided based on the intended application.
26 °C & 101 kPa 26 °C & 171 MPa 176 °C & 171 MPa Fig. 8(b) shows the variation of relative plastic viscosity with tem-
A B A B A B
perature. It is observed that the increase in temperature has reduced
the cohesive attraction forces between the molecules of bentonite and
Basemud 93 0.44 902 0.72 1920 0.95
nanoparticles, affecting the overall performance of the fluid sample
0.11 wt% 248 0.40 2731 0.75 5732 0.84
with a gradual decrease in its viscosity. Since the plastic viscosity values
 K. Anoop et al. / Powder Technology 342 (2019) 585–593 591

Fig. 5. Viscosity variation with pressure at 26 °C (measurement shear rate of 1021s−1).

Table 2
Viscosity values used in normalization of Figs. 5 and 6, measured at a shear rate of
1021s−1.

η o,p (cp)@ 26 °C, 101 kPa η o, t (cp) @ 37 °C 171 MPa

Basemud 5.52 4.94

0.027 13.32 19.97
0.056 15.75 19.99
0.11 16.25 25.22
0.22 24.70 35.03

Fig. 6. Viscosity variation with temperature at 171 MPa pressure (measurement shear rate
of 1021s−1).

are a representation of the flow resistance, the graph shows that as tem-
perature is increased from ambient to approximately 125 °C, the sam-
ples containing various percentage of CNT could withstand the effect
of increase in temperature. However, a breakpoint in this trend is ob- Fig. 7. Scanning Electron Microscopy image of (a) basemud and (b) basemud with CNT
particles (0.22 wt%) (c) basemud with CNT particles (0.22 wt%)close up view.
served around 150 °C after which the plastic viscosity values are ob-
served to be fluctuating severely.

4. Conclusions
Rheology of water-based drilling mud suspended with CNT particles
is studied. The following observations are made in this study.
a) Both the basemud and the CNT-nanomud samples showed shear-
thinning behaviors at all experimental conditions.
b) The addition of CNT particles increased the viscosity of the drilling
mud. For a 0.22 wt% CNT loading, viscosity values increased five-
fold when compared to that of the basemud at ambient conditions.
c) The viscosity of the basemud increased with an increase in pressure.
A similar observation is seen for the nanomud at low-concentration
as well. However, for higher CNT loading, viscosity values are ob-
served to decrease with an increase in pressure
592 K. Anoop et al. / Powder Technology 342 (2019) 585–593

Fig. 8. Relative plastic viscosity variation with (a) pressure and (b) temperature.

d) The viscosity of the basemud, as well as the low-concentration Acknowledgments

nanomud, initially increased with an increase in temperature. How-
ever, after 100 °C the trend changes and viscosity values decrease
with further increase in temperature. For higher concentrations of
CNT loading, viscosity values are observed to decrease with an in-
crease in temperature similar to that of water. It is reasoned that
the addition of CNT nanoparticles created an appropriate linkage
system where the mud particles in the drilling fluid are held stable
and homogenous. However, when the concentration of CNT parti-
cles is increased beyond a point, agglomeration of mud particles to
the CNT chain occurs, separating the water from the drilling fluid
mixture.
This publication was made possible by NPRP grant # 08-574-2-239
from the Qatar National Research Fund (a member of the Qatar Founda-
tion). The statements made herein are solely the responsibility of the
authors.
Appendix A. Supplementary data
Supplementary data to this article can be found online at https://doi.
org/10.1016/j.powtec.2018.10.016.
 K. Anoop et al. / Powder Technology 342 (2019) 585–593
References
[1] C. Christiansen, From Oil-based Mud to Water-based Mud, SPE Health, Safety and
Environment in Oil and Gas Exploration and Production Conference, Society of Pe-
troleum Engineers, 1991.
[2] A. Tehrani, S. Young, D. Gerrard, J. Fernandez, Environmentally friendly water based
fluid for HT/HP drilling, SPE International Symposium on Oilfield Chemistry, Society
of Petroleum Engineers, 2009.
[3] S.K. Singh, R.M. Ahmed, F. Growcock, Vital Role of Nanopolymers in Drilling and
Stimulations Fluid Applications, Society of Petroleum Engineers, 2012.
[4] J. Nasser, A. Jesil, T. Mohiuddin, M. Al Ruqeshi, G. Devi, S. Mohataram, Experimental
Investigation of Drilling Fluid Performance as Nanoparticles, World J. Nano Sci. Eng.
3 (2013) 57–61.
[5] S. Iranmanesh, O.H. Chyuan, B.C. Ang, E. Sadeghinezhad, A. Esmaeilzadeh, M.
Mehrali, Thermal performance enhancement of an evacuated tube solar collector
using graphene nanoplatelets nanofluid, J. Clean. Prod. 162 (2017) 121–129.
[6] S.S. Hassani, A. Amrollahi, A. Rashidi, M. Soleymani, S. Rayatdoost, The effect of
nanoparticles on the heat transfer properties of drilling fluids, J. Pet. Sci. Eng. 146
(2016) 183–190.
[7] A.H. Salih, T.A. Elshehabi, H.I. Bilgesu, Impact of nanomaterials on the rheological
and filtration properties of water-based drilling fluids, SPE Eastern Reg. Meet. Soc.
Petrol. Eng. (2016) 14.
[8] A. Ismail, A. Aftab, Z. Ibupoto, N. Zolkifile, The novel approach for the enhancement
of rheological properties of water-based drilling fluids by using multi-walled carbon
nanotube, nanosilica and glass beads, J. Pet. Sci. Eng. 139 (2016) 264–275.
[9] A. Samsuri, A. Hamzah, Water based mud lifting capacity improvement by multiwall
carbon nanotubes additive, J. Petrol. Gas Eng. 5 (2011) 99–107.
[10] A.-M. Needaa, P. Pourafshary, A.-H. Hamoud, A. Jamil, Controlling bentonite-based
drilling mud properties using sepiolite nanoparticles, Pet. Explor. Dev. 43 (2016)
717–723.
[11] A.K. Sharma, A.K. Tiwari, A.R. Dixit, Rheological behaviour of nanofluids: a review,
Renew. Sust. Energ. Rev. 53 (2016) 779–791.
[12] A. Kanjirakat, R. Sadr, Near-wall velocity profile measurement for nanofluids, AIP
Adv. 6 (2016), 015308. .
[13] A. Nasiri, M. Shariaty-Niasar, A. Rashidi, A. Amrollahi, R. Khodafarin, Effect of disper-
sion method on thermal conductivity and stability of nanofluid, Exp. Thermal Fluid
Sci. 35 (2011) 717–723.
[14] M.-F. Yu, B.S. Files, S. Arepalli, R.S. Ruoff, Tensile loading of ropes of single wall car-
bon nanotubes and their mechanical properties, Phys. Rev. Lett. 84 (2000) 5552.
[15] P. Pötschke, T. Fornes, D. Paul, Rheological behavior of multiwalled carbon nano-
tube/polycarbonate composites, Polymer 43 (2002) 3247–3255.
[16] Y. Yang, E.A. Grulke, Z.G. Zhang, G. Wu, Thermal and rheological properties of carbon
nanotube-in-oil dispersions, J. Appl. Phys. 99 (2006), 114307. .
[17] K. Lu, Rheological behavior of carbon nanotube-alumina nanoparticle dispersion
systems, Powder Technol. 177 (2007) 154–161.
[18] B. Wang, X. Wang, W. Lou, J. Hao, Rheological and tribological properties of ionic
liquid-based nanofluids containing functionalized multi-walled carbon nanotubes,
J. Phys. Chem. C 114 (2010) 8749–8754.
[19] J. Ponmozhi, F. Gonçalves, A. Ferreira, I. Fonseca, S. Kanagaraj, N. Martins, M.S.
Oliveira, Thermodynamic and transport properties of CNT-water based nanofluids,
J. Nano Res. (2010) 101–106 Trans Tech Publ.
[20] L. Chen, H. Xie, W. Yu, Y. Li, Rheological behaviors of nanofluids containing multi-
walled carbon nanotube, J. Dispers. Sci. Technol. 32 (2011) 550–554.
[21] S. Halelfadl, P. Estellé, B. Aladag, N. Doner, T. Maré, Viscosity of carbon nanotubes
water-based nanofluids: Influence of concentration and temperature, Int. J. Therm.
Sci. 71 (2013) 111–117.
[22] N. Singh, G. Chand, S. Kanagaraj, Investigation of thermal conductivity and viscosity
of carbon nanotubes–ethylene glycol nanofluids, Heat Transf. Eng. 33 (2012)
821–827.
[23] J. Hilding, E.A. Grulke, Z. George Zhang, F. Lockwood, Dispersion of carbon nanotubes
in liquids, J. Dispers. Sci. Technol. 24 (2003) 1–41.
[24] P. Garg, J.L. Alvarado, C. Marsh, T.A. Carlson, D.A. Kessler, K. Annamalai, An experi-
mental study on the effect of ultrasonication on viscosity and heat transfer perfor-
mance of multi-wall carbon nanotube-based aqueous nanofluids, Int. J. Heat Mass
Transf. 52 (2009) 5090–5101.
[25] B. Ruan, A.M. Jacobi, Ultrasonication effects on thermal and rheological properties of
carbon nanotube suspensions, Nanoscale Res. Lett. 7 (2012) 127.
[26] M.M. Derakhshan, M.A. Akhavan-Behabadi, M. Ghazvini, Rheological Characteristics,
pressure drop, and Skin Friction Coefficient of MWCNT–Oil Nanofluid Flow inside an
Inclined Microfin Tube, Heat Transfer Engineering 36 (2015) 1436–1446.
[27] M. Amanullah, M.K. AlArfaj, Z.A. Al-abdullatif, Preliminary test results of nano-based
drilling fluids for oil and gas field application, SPE/IADC Drill. Conf. Exhibit. Soc. Pet-
rol. Eng. (2011) 9.
[28] J.T. Srivatsa, M.B. Ziaja, An experimental investigation on use of nanoparticles as
fluid loss additives in a surfactant-polymer based drilling fluids, Int. Petrol. Technol.
Conf. Int. Pet. Technol. Conf. (2011) 19.
[29] M. Zoveidavianpoor, A. Samsuri, The use of nano-sized Tapioca starch as a natural
water-soluble polymer for filtration control in water-based drilling muds, J. Nat.
Gas Sci. Eng. 34 (2016) 832–840.
[30] M. Sedaghatzadeh, A. Khodadadi, M.r. Tahmasebi birgani, an improvement in ther-
mal and rheological properties of water-based drilling fluids using multiwall carbon
nanotube (MWCNT), Iran. J. Oil Gas Sci. Technol. 1 (2012) 55–65.
593
[31] M. Sedaghatzadeh, K. Shahbazi, M.H. Ghazanfari, G. Zargar, Experimental Investiga-
tion of Self-Repeating effect of Different Nanoparticles on Internal Mud Cake Forma-
tion by Water-based Drilling Fluid in Directional Wells, IADC/SPE Asia Pac. Drill.
Technol. Conf. Soc. Petrol. Eng. (2016) 17.
[32] B. Fazelabdolabadi, A. Khodadadi, M. Sedaghatzadeh, Thermal and rheological prop-
erties improvement of drilling fluids using functionalized carbon nanotubes, Appl.
Nanosci. 5 (2015) 651–659.
[33] J.K.M. William, S. Ponmani, R. Samuel, R. Nagarajan, J.S. Sangwai, Effect of CuO and
ZnO nanofluids in xanthan gum on thermal, electrical and high pressure rheology
of water-based drilling fluids, J. Pet. Sci. Eng. 117 (2014) 15–27.
[34] Ametek/Chandler Engineering Instructional Manual Model 7600 HTHO Viscometer,
Revision –KOctober 2013 P/N: 7600–1050.
[35] K. Anoop, R. Sadr, R. Yrac, M. Amani, High-pressure rheology of alumina-silicone oil
nanofluids, Powder Technol. 301 (2016) 1025–1031.
[36] K. Anoop, R. Sadr, M. Al-Jubouri, M. Amani, Rheology of mineral oil-SiO 2 nanofluids
at high pressure and high temperatures, Int. J. Therm. Sci. 77 (2014) 108–115.
[37] J.W. Schmelzer, E.D. Zanotto, V.M. Fokin, Pressure dependence of viscosity, J. Chem.
Phys. 122 (2005), 074511.
[38] B. Safi, S. Zarouri, R. Chabane-Chaouache, M. Saidi, A. Benmounah, Physico-chemical
and rheological characterization of water-based mud in the presence of polymers, J.
Pet. Explor. Prod. Technol. 6 (2016) 185–190.
Kanjirakat Anoop is an Assistant Research Scientist in the
mechanical engineering program at Texas A&M University
at Qatar. He received his Ph.D. from Indian Institute of Tech-
nology Madras in 2010. Before joining Texas A&M, he was a
research associate at Helmut Schmidt University in Ham-
burg, Germany as part of his DAAD fellowship. His research
interests include experimental heat transfer, computational
fluid dynamics, micro-fluidics and multi-phase flows.
Reza Sadr is an associate professor in the mechanical engi-
neering program at Texas A&M University at Qatar. He re-
ceived his Ph.D. from University of Utah in 2002. Before
joining Texas A&M in 2008, he moved to Georgia Tech At-
lanta as a research scientist, and then to Georgia Tech Savan-
nah as a visiting assistant professor. His research expertise is
in the experimental methods in thermo-fluid sciences. His
current research addresses microfluidics, droplets and
sprays, environmental fluid mechanics, and supercritical
thermo-fluids. He has beena member of American Physical
Society and American Society of Mechanical Engineering
since 1998.
Rommel Yrac earned his double degree in Chemical Engi-
neering in the Philippines. He started his professional career
in the petrochemical industry as a Chemical Engineer under
the Laboratory and Specialization department of LIEC. Then
he transferred to M-I Swaco, Qatar where he specialized in
drilling laboratory operations from 2005 until 2013 in tech-
nical support to the entire GCC and North Africa. After con-
tinuous collaboration to academic fields, he accepted the
position of first Senior Research Associate of TAMUQ. After
almost 3 years of completion of research with approximately
$4,000,000 QNRF funding on both UREP and NPRP projects,
he's now the newest staff of the program as Technical Lab
Coordinator.
Mahmood Amani is an Associate Professor at Texas A&M
University at Qatar. He received a BS Degree in Mechanical
Engineering from Wichita State University, a MS Degree in
Natural Gas Engineering from Texas A&M University-
Kingsville, and a Ph.D. in Petroleum Engineering from Texas
A&M University. After completion of his Ph.D., Dr. Amani
worked for a few years as a Research Scientist at Texaco Ex-
ploration & Production Technology Department in Houston,
Texas. Dr. Amani joined the faculty of Texas A&M University
in College Station in 2003 and relocated to Texas A&M Uni-
versity in Qatar in 2005.