Journal of Petroleum Science and Engineering 190 (2020) 107006

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Journal of Petroleum Science and Engineering

journal homepage: http://www.elsevier.com/locate/petrol

Experimental evaluation of nanomaterials to improve drilling fluid

properties of water-based muds HP/HT applications
Majid Sajjadian a, Vali Ahmad Sajjadian a, *, Alimorad Rashidi b
a
Department of Chemistry Engineering, Marvdasht Branch, Islamic Azad University, Marvdasht, Iran
b
Nanotechnology Research Center, Research Institute of Petroleum Industry, Tehran, Iran

A R T I C L E I N F O A B S T R A C T

Keywords: These days, significant investigations are carried out on the preparation of high qualified aqueous-based drilling
Nano materials fluid-structure to create the best option compared with oil-base drilling fluid at high-pressure and high-
Rheological characteristics temperature situations utilizing an optimum cost approach. Nanomaterials may have the desirable possibility
Filtration properties
of using their favored utilization documented in many publications. Although high cost, due to more concen­
High-pressure
And high-temperature
tration and side undesirable effects on one or some mud properties, this situation restricts using these materials
in various industries. In this experimental research, an effort was made to enhance the application of water-based
drilling fluids by using three kinds of nanomaterials, called zirconium oxide, multi-walled carbon nanotubes and
titanium dioxide nanohybrids, and functionalized multi-wall carbon nanotubes. Accomplishing some rheological,
filtration characteristics and conductivity experiments on the experimental samples with nanomaterials
mentioned manifested that the hybrids and zirconium oxide efficiently improve the drilling fluid rheological
parameters including plastic viscosity, yield point and gel strength of the mud with a slow influence on the mud
filtrate volume. However, by the multi-walled carbon nanotubes, the filtration properties are remarkably
decreased with no undesirable side effects on rheological characteristics, particularly at the 0.5 wt% concen­
tration. Generally, it could be concluded that using the nanomaterials at concentrations up to 0.5 wt% into the
water-based mud has the possibility of enhancing rheological and filtration characteristics.

1. Introduction
Drilling fluids are discussed as a circulating system in the drilling
industry, which created multiple functions. Their basic roles consist of
suspending/moving drill cuttings, cooling and lubricating the drilling
bits, keeping borehole stability and decreasing the pay zone damage,
removing cutting from the downhole and controlling subsurface for­
mation pressures. Ineffective hole cleaning and creation of beds caused
to serious challenged including, inopportune drill bit erosion, extra
torque and drag, drill pipe sticking and low drilling rates which raises
time and costs of the drilling operation. In vertical wells, as mentioned in
the previous literatures, the appropriate hole cleaning is mainly related
on drilling hydraulics parameters such as; drilling fluid weight/density,
plastic viscosity, yield point, gel strength, etc. (Razali et al., 2018; Zhao
et al., 2017; Xu et al., 2018; Busahmin et al., 2017). Drilling fluids are
often classified into two groups: water-based muds and oil-based muds.
Water-based muds have recognized the most broadly employed muds in
the drilling operations because of their minimum cost and undesirable
influence on the environment (Xie and Liu, 2017; Song et al., 2016).
Reducing of formation of damage among the production zone created by
filtrate invasion is required. Variant studies carried out on the utilization
of nano diameter agents, particularly the Nano silica (Ismail et al.,
2016), Graphite (Mahmoud et al., 2016), Titanium nitride (Vegard and
Belayneh, 2017), and Yttrium Oxide (Elochukwu et al., 2018) to
enhance drilling mud properties. Individual nanomaterials with spher­
ical shape in water-based drilling muds possess several restrictions. The
attractive forces such as van Waals are increased by spherical
morphology because of the very small diameter of nanomaterials. These
attractive forces may create sedimental problems. So, the spherical
nanoparticles could reduce mud drilling efficiency because of hetero­
geneously suspension. The influence of multi-walled carbon nanotubes
and graphene nanoplatelets in aqueous-based drilling mud was evalu­
ated by Ismail et al. It concluded that the use of 0.04 pound per barrel of
multi-walled carbon nanotube enhanced the plastic viscosity nearly 15%
compared with based mud. Also, the mud filtrate volume was reduced
by about 18 and 8% by adding the multi-walled carbon nanotube and

* Corresponding author.
E-mail address: vasajjadian@yahoo.com (V.A. Sajjadian).

https://doi.org/10.1016/j.petrol.2020.107006
Received 18 May 2019; Received in revised form 25 January 2020; Accepted 27 January 2020
Available online 11 February 2020
0920-4105/© 2020 Elsevier B.V. All rights reserved.
M. Sajjadian et al. Journal of Petroleum Science and Engineering 190 (2020) 107006

Table 1 hydrophobic nano-silica was utilized in the drilling mud combination

List of different classes and types of nanoparticles which can be used in drilling and the effect on filtration properties was evaluated in two sections such
mud applications. as mud cake thickness and mud filtrate volume. The mud cake thickness
Type of Subject of study Reference Outcomes and mud filtration volume reduction were measured less than 1 mm and
nanomaterials 44%, respectively. However, the rheological and filtration properties
MWCNTs Plastic Viscosity Ismail et al. Increasing plastic under high-temperature environments were not investigated (Saparti
(2018) viscosity to 15% et al., 2018). Abdo et al. prepared the ZnO-clay nanocomposite for
Graphene Mud Filtrate Reducing mud filtrate mixing in WBDF; it was shown that the mud rheological properties were
Volume volume to 18%
constant under a high-temperature environment. The introduction of
Decreasing mud
filtrate volume to 8% drilling muds with improved rheological and filtration properties at high
Silica Mud Cake Mahmoud et al. Decreasing mud temperatures is still a major problem (Abdo et al., 2014). TiO2-bentonite
(2016) filtrate volume to nanocomposite was made to increase the rheological property of the
43% water-based drilling fluid (Aftab et al., 2017). The experimental results
Iron
Aluminum Oxide Filtrate Volume Anyanwu et al. Control mud filtrate
determined that yield point and 10-min gel strength were improved by
(2016) volume 57 and 40% compared to basic drilling fluid after the addition of 1.0 g at
Iron Oxide Gel Strength Jung et al. Improve the gel 65.56 � C. API and HPHT mud filtrate volumes were decreased by 10%,
(2011) strength and 9.2%. However, the increased amounts in considering used nano­
Zinc Oxide, Rheological Noah et al. Increase in
material concentrations are not significant achievements. Also, the
properties (2017) Rheological
properties application of this mud system is not investigated at ultra-high tem­
Modified Reducing Filtrate perature (Nizamani et al., 2017). Technical literature includes a broad
Calcium Volume area of study subjects about how the different kinds of nanomaterials are
Carbonate using to change particular parameters and properties to improve the
Poly Styrene Mud Filtrate Elochukwu et al. 51 and 61% reduction
drilling fluid performance (Table 1). Oil-based drilling fluid may be
Volume (2018) in mud filtrate
volume under LPLT & chosen for certain demands including HPHT wells, reducing reservoir
HPHT damage and other causes. These days, along with increasing environ­
Hydrophobic Cake Thickness Saparti et al. Cake thickness of less mental worries, the application of oil-based drilling fluid is forbidden
nanosilica Mud filtrate (2018) than 1 mm
and strongly limited in many areas throughout the world. Environ­
Volume Reducing Filtrate
Volume to 44% mental statutes limit and ban the oil-based drilling fluid application due
ZnO-Clay Nano Rheological (Abdo et al., Rheological to contaminating the soil and water aquifers. Hence, to get more success
Composite Properties 2014) Properties were against these limitations and restricts, further investigations and re­
constant under high searches are needed to enhance water-based drilling mud containing
temperature
nanomaterials performance. The water-based mud containing nano­
TiO2-Bentonite Yield point-10- Nizamani et al. Improving YP and 10-
Nano min gel Strength (2017) min gel Strength by particles can be reconditioned and reused during drilling problems is
Composite 57 and 40% compared with oil-based drilling fluid. Moreover, buyback policies for
API and HPHT Decreasing API, the application of this drilling mud may cause them a wonderful
Filtrate Loss HPHT Filtrate Loss
replacement in conditions where the oil-based drilling fluid used.
Volume Volume 10 & 9.2%
MWCNTs Mud filtrate (Ismail et al., Reducing 65% and
Generally, more environmental friendly MWCNTs materials are favor­
volume (2016), Ismail 20% Mud filtrate able mud filtrate reducer agents under the high-temperature condition
et al., (2014) volume as a high performance and more stability suspended (Abduo et al.,
2016). The cost of water-based muds containing nanomaterials exani­
mated is less than oil-based drilling fluid because of fewer chemical
graphene nanoplatelet, respectively (Ismail et al., 2018). Adding higher
materials in proposed mud formulation and low concentration of
silica nanoparticles concentrations illustrated a remarkable decrease in
nanomaterials. By investigation experiments carried out in previous
mud filtrate volume nearly 43% in 0.5 wt% concentration (Mahmoud
sections of this article, it is remarkability clear that functionalized
et al., 2016). The efforts were made to use various diameter of aluminum
multi-wall carbon nanotubes (FMWCNTs) among other nanomaterials
oxide nanoparticles in drilling mud. It was concluded that 2 wt % con­
are the prominent selection to improve water-based drilling fluid
centrations could control the mud filtrate volume during low pressure
properties. The solid control system in the drilling rig is used to remove
and low temperature (LPLT) condition (Anyanwu et al., 2016). The in­
fine particles down to 1–2 μm. So, there is not any degradation and
fluence of iron oxide (Fe2O3) nanoparticles on water-based drilling fluid
destruction of nanomaterials during recycling in the mud refining sys­
properties during the high pressure and high temperature (HPHT)
tem. In conclusion, it could be one of the potentially considerable ben­
environment. It was found that these nanoparticles accidently located in
efits of this water-based drilling fluid containing the nanomaterials
the pore area of bentonite could improve the gel strength of drilling mud
system for application in drilling rig site.
despite not affecting on mud filtrate volume control (Jung et al., 2011).
The main goal of this experimental research is to engineer a
The Zinc oxide (ZnO) and modified calcium carbonate (M-CaCO3)
bentonite drilling mud utilizing several types of nanomaterials such as
nanoparticles were favorably made and mixed to oil-base drilling fluid
zirconium oxide (ZrO2), multi-walled carbon nanotubes and titanium
for investigating mud properties in HPHT. These nanoparticles exhibited
dioxide (MWNT-TiO2) nanohybrids, Functionalized Multi-walled car­
an increment of apparent viscosity, plastic viscosity, and yield point,
bon nanotube as an affordable price along with prominent performance
reduced in mud filtrate volume. However, as mentioned in many pre­
which could control mud filtration volume with enhancing mud rheo­
vious researches, the application of oil-based drilling fluid is strongly
logical properties. Nano-contained experimental samples were investi­
limited throughout the world (Noah et al., 2017). The experimental
gated versus any change in viscosity parameters in comparison with
results Methyl Ester Sulphonate (MES) surfactant and nano polystyrene
nano free sample. Filtration and conductivity experiments were further
in aqueous-based drilling mud displayed about 51 and 61% reduction in
performed to investigate the effect of nanomaterials on drilling effi­
mud filtrate volume under LPLT and HPHT environments, respectively.
ciency at various temperatures.
Although, using auxiliary additives such as surfactant and conventional
polymer in proposed mud composition could cause higher mud cost
compared with oil-based drilling fluids (Elochukwu et al., 2018). The

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M. Sajjadian et al.
2. Experimental section
2.1. Modification of multiwall carbon nanotube
Generally, the more economical procedure to manufacture the major
amount of nanomaterials is named a Two-step method that having
physically excitation to suspend nanomaterials as a dry powder in
related host fluid for procreating nano mixture. This mentioned method
often includes several steps such as bath ultra-sonication method, high-
shear agitator, homogenization procedure (Hoa et al., 2016). Because of
the hydrophobic nature of MWCNTs, aggregate and precipitated of this
nanomaterial often occur into the aqueous phase. So, the hydrophilic
functional groups such as generate hydroxyl ( OH), carbonyl ( C– – O),
or carboxyl groups ( COOH) are embedded in nanotube surfaces via
acid treatment technique. For hydroxyl and carboxyl functionalizing the
MWCNTs surfaces, a mixture of nitric acid and sulfuric acid was pre­
pared. Then, half gram of MWCNTs was exposed to vapor formed of
boiled mixture of H2SO4–HNO3 (1:3 v/v) at 75 � C and reflux system
placed under a ventilating hood during a day, filtered by Whatman
quantitative filter paper (Approximated pore diameter 2.7 μm), and
washed for several times to ensure for reaching a neutral form via acid
removal nanomaterial display excess acidity nature. Various tempera­
tures and method duplication were carried done basing on the surface
treatment quality of MWCNTs. After that, the hot oven was used to dry
this nanomaterial for separating the connected water as a general acid
treatment (Sedaghatzadeh et al., 2016; Kazemi-Beydokhti et al., 2018).
The sedimentation and settlement of nanomaterials happen very negli­
gibly due to having bentonite and thixotropic characteristics of the nano
free based mud. Despite this, each sample of prepared drilling muds
according to Table 2 was blended by Silverson Homogenizer during an
invariant rate of 12,800 RPM for 30 min, continued through a sonicated
bath system utilized LSP-500 Laboratory Scale Ultrasonic Liquid Pro­
cessor during next 1 h to obtain superb suspended nanomaterials. The
suspended mixture was then instantly blended with the FANN Hamilton
beach mixer for further 30 min at a very high RPM.
2.2. Materials and characterization
In this experimental investigation, some NPs types such as MWNT-
TiO2 nano hybrids (100 nm, purity 95%, specific surface area 80–100
m2/g), ZrO2 (4.46 nm, purity 99% and specific surface area 85 m2/g),
FMWCNTs (14 nm, purity 99% and specific surface area 220 m2/g) were
Procured from the Research Institute of Petroleum Industry IRAN. The
NPs crystalline components, morphologies, and sizes were measured by
doing ray-diffraction (XRD, model broker AXS, Germany), transmission
electron microscopy (TEM, model Philips Analytical equipment,
Acc.200.00 kV) and Fourier Transform Infrared Spectroscopy (FTIR,
BRUKER TENSOR 27, Germany) analyses. Sulfuric acid (H2SO4), Nitric
acid (HNO3), titanium chloride (TiCl4), Sodium Hydroxide (NaOH) and
calcium carbonate (CaCO3) were obtained from Merck KGaA (Darm­
stadt, Germany). Sodium bentonite (size 57 μm and density of 2.48 g/
cm3) as the dry powder was obtained from Sun Clay Therapy, Inc.
(Florida, US) and was used without more purification.
2.3. Water-based drilling fluid samples
Water-based drilling mud samples were made for reaching the aim of
this research study containing 10-g bentonite and 350 mL fresh water.
Bentonite was gently added into water by the FANN Multimixer 9B. For
inhibiting of agglomeration of bentonite into the water and forming two-
phase fluids, the blend was mixed for 15 min under the fixed speed of
15,000 RPM. Then, a specific amount of calcium carbonate used to
weigh mud sample density up to 1281.44 kg/m3 171.52-g calcium
carbonate was gently mixed into a blend of water with bentonite and
mixture was blended for 10 min. The water-based drilling fluid sample
was aged in 27 � C for 24 h to ensure of crystallizing bentonite in the
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Journal of Petroleum Science and Engineering 190 (2020) 107006
Table 2
Drilling fluid samples and abbreviated titles.
Sample Abbreviated Title
10 g Bentonite þ350 mL Fresh water þ 171.52 calcium R
carbonate
10 g Bentonite þ350 mL Fresh water þ 171.52 calcium MWNT-TiO2 hybrids -
carbonate þ 0.01 wt% MWNT-TiO2 hybrids 0.01%
10 g Bentonite þ350 mL Fresh water þ 171.52 calcium MWNT-TiO2 hybrids -
carbonate þ 0.05 wt% MWNT-TiO2 hybrids 0.05%
10 g Bentonite þ350 mL Fresh water þ 171.52 calcium MWNT-TiO2 hybrids -
carbonate þ 0.1 wt% MWNT-TiO2 hybrids 0.1%
10 g Bentonite þ350 mL Fresh water þ 171.52 calcium MWNT-TiO2 hybrids -
carbonate þ 0.5 wt% MWNT-TiO2 hybrids 0.5%
10 g Bentonite þ350 mL Freshwater þ 171.52 calcium ZrO2 - 0.01%
carbonate þ 0.01 wt% ZrO2
10 g Bentonite þ350 mL Fresh water þ 171.52 calcium ZrO2- 0.05%
carbonate þ 0.05 wt% ZrO2
10 g Bentonite þ350 mL Fresh water þ 171.52 calcium ZrO2- 0.1%
carbonate þ 0.1 wt% ZrO2
10 g Bentonite þ350 mL Freshwater þ 171.52 calcium ZrO2- 0.5%
carbonate þ 0.5 wt% ZrO2
10 g Bentonite þ350 mL Fresh water þ 171.52 calcium FMWCNTs- 0.01%
carbonate þ 0.01 wt% FMWCNTs
10 g Bentonite þ350 mL Fresh water þ 171.52 calcium FMWCNTs- 0.05%
carbonate þ 0.05 wt% FMWCNTs
10 g Bentonite þ350 mL Fresh water þ 171.52 calcium FMWCNTs- 0.1%
carbonate þ 0.1 wt% FMWCNTs
10 g Bentonite þ350 mL Fresh water þ 171.52 calcium FMWCNTs- 0.5%
carbonate þ 0.5 wt% FMWCNTs
Chemical materials and the number of experimental devices utilized for making
drilling fluid samples and characterizing fluid properties were demonstrated in
Tables 3 and 4.
mixture. After passing this duration of time, the mud sample was
blended more in the Multimixer for 5 min. To homogenize mud struc­
ture. To analysis, the impact of nanoparticles on the drilling fluid
properties, the nanoparticles in mass fractions of 0.01, 0.05, 0.1, 0.5 wt
% were mixed into the reference mud. Next, the experimental samples
were mixed for 2 h. By utilizing an orbital shaker at 1500 RPM and
followed through an ultrasonic bath for half-hour to occur stable
mixture before each experimental analysis. The experimental tests were
precisely carried out according to the 13D API standard procedure. The
drilling fluid formulation and nanoparticles concentrations have been
selected via literature (Kang et al., 2015) and innovation in good per­
formance with low concentrations. The brief of drilling fluid samples
prepared in this research study was demonstrated in Table 2.
2.4. Mud rheology
The experimental samples rheology was obtained by applying the
FANN Model 35-rotational viscometer at various rates basing on the
American Petroleum Institute standard recommended practices (Kang
et al., 2015). The dial reading taken from the viscometer was registered
and applied for more evaluation of the viscosity and thixotropic char­
acteristics. The rheological behavior of water-based drilling fluids is
generally determined with two rheological models named Bingham
plastic and Power-law mathematical models. Between them, the Bing­
ham plastic is major broadly used in the petroleum industry. There are
two parameters for specifying each rheological model such as plastic
viscosity (Avci and Mert, 2019), yield point (Avci and Mert, 2019),
Consistency Index (k) (Elochukwu et al., 2018) and Flow Behavior Index
(n) (Elochukwu et al., 2018) were referred to Bingham plastic and
power-law models, respectively. Plastic viscosity is determined by sub­
tracting 600 from 300 RPM viscometer dial readings. The subtraction of
300 RPM dial reading from plastic viscosity could use to obtain yield
point. The measurements are employed for calculating these parameters
as follows mathematical relations:
PV ¼ Φ600 Φ300 ðmPasÞ (1)
M. Sajjadian et al. Journal of Petroleum Science and Engineering 190 (2020) 107006

Fig. 1. Displays a flowchart with the steps taken in this study to evaluate the designed muds.

Fig. 2. TEM and XRD analyses of nanoparticles: a- ZrO2, b-FMWCNTs, and c- MWNT-TiO2 hybrids.

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M. Sajjadian et al. Journal of Petroleum Science and Engineering 190 (2020) 107006

Table 3 after passing half-hour (Yunita et al., 2016).

Chemical materials utilized for preparing the drilling fluid samples.
Components Purity Brand Function 2.5.1. LPLT situation
FANN Series 300 LPLT Filter Press was utilized by FANN Series 300
Deionized Water - - Host Fluid
Bentonite >80% Sun Clay Therapy Viscosifier LPLT Filter Press in 27 � C as ambient temperature and 689.47 kPa (100
Calcium carbonate >99% Merck Weighting Agent psi) as low pressure according to 13I-API standard procedure. A 10 mL
Sodium Hydroxide >99% Merck PH Controller graduated cylinder was put under the LPLT filter press for half-hour to
(NaOH) accumulate the mud filtrate volume. The mud cake thickness created on
MWNT-TiO2 Research Institute of Potentially
filter paper was gauged at the finish of the experiment.
>95%
hybrids Petroleum Industry Properties Improver
ZrO2 >99% Research Institute of Potentially
Petroleum Industry Properties Improver 2.5.2. HPHT condition
FMWCNTs >99% Research Institute of Potentially FANN Model 175CT HPHT Filter Press was employed for the HPHT
Petroleum Industry Properties Improver
experiments. The test temperature is 93 OC and net pressure was fixed in
3447.37 kPa (500 psi) with controlling regulator and back pressures.
Table 4 The time of the experiment was half-hour by following 13 I - American
All apparatuses used in this research study. Petroleum Institute Recommended Practices. The mud cake thickness
was next gauged for more investigation. Fig. 1 displays a flow diagram
Device Function
with the staged one in this experimental research to analyze the engi­
FANN Multimixer 9B To mix the chemical materials with water for making
neered samples.
experimental samples
FANN Viscometer 35SA To obtain rheological parameters of experimental
samples 3. Results and discussions
FANN Series 300 LPLT To measure the filtrate volume and mud cake
Filter Press thickness
3.1. Nanoparticles characterization
FANN HPHT Filter Press To specify the filtrate volume and mud cake thickness
175CT
Orbital Shaker To blend the suspension of nanoparticles with WBDF The mean sizes of MWNT-TiO2 nanohybrids, ZrO2, and FMWCNTs
to avoid of instability of nanoparticles nanoparticles were determined by X-ray diffraction (XRD) pattern
Bransonic 1.893 liter To sonicate the nanoparticles solution to create a well- below. The XRD analysis from the ZrO2 sample illustrated these nano­
Ultrasonic Bath dispersed solution
particles have a tetragonal structure (Fig. 2(a)). Also, MWNT-TiO2
nanohybrids and FMWCNTs nanoparticles have partial amorphous
(crystalline) structures as seen in (Fig. 2(b) and (c)).
YP ¼ 0:5 ðΦ300 PVÞ ðPaÞ (2)

n ¼ 3:32logðΦ600 = Φ300Þ
Φ600
k¼
1022n
whereas, Φ600 ¼ dial reading at 600 RPM, Φ300 ¼ dial reading at 300
RPM.
The factors k and n are attached to the apparent viscosity and the
deviation of the Newtonian characteristic. Both rheological models were
evaluated in this experimental study.
2.5. Filtration loss properties
The mud cake and filtrate mud volume was gauged for analyzing the
filtration characteristic of the drilling fluid. The LPLT and HPHT filter
press apparatuses were applied for gathering mud filtrate drops at
normal and abnormal conditions such as pressures and temperatures
(3) 3.2. Influence of NP type and concentration on the rheological behavior of
WBDF
(4)
3.2.1. Plastic viscosity
The drilling fluid rheology is specified for investigating muds prop­
erties in the circulating mud system and performs a major function in the
drilling rate, wellbore cleaning, and stability of a good hole. One of the
main factors in the Bingham model is plastic viscosity and it demon­
strates the drilling fluid viscosity while analogizing to the unlimited
shear rate according to the Bingham theory (Rafati et al., 2017). It is
essential that drilling fluid could create an adequate weight to cause
hydrostatic pressure. There is a direct relation between drilling fluid
rheology and hydrostatic pressure. Generally, lower hydrostatic pres­
sure because of less drilling fluid rheology is not desirable. The outcomes
taken of the rheological experiments of the drilling fluid samples
comprising of nanoparticles are shown in Table 5. As could display in the
table, the yield point and plastic viscosity with the increase of NPs

Table 5
Rheological parameters of various experimental samples.
Samples Bingham Plastic Power Law Gel Strength

Plastic Viscosity, mPa s Yield Point, Pa Consistency Index, Pa sn Flow Behavior Index 10 s, Pa 10 min, Pa

R 12 16 6.6553 0.374 2.5 3

MWNT-TiO2 hybrids - 0.01% 13 16 6.5596 0.382 2.5 3.5
MWNT-TiO2 hybrids - 0.05% 14 17 8.1875 0.357 3.1 4
MWNT-TiO2 hybrids - 0.1% 16 19 8.7620 0.366 3.5 4.4
MWNT-TiO2 hybrids - 0.5% 18 19 11.4433 0.333 4 5.1
FMWCNTs- 0.01% 16 19 9.6718 0.349 3 4.2
FMWCNTs- 0.05% 21 25 11.4433 0.367 4 5.5
FMWCNTs- 0.1% 25 34 14.8428 0.365 5 7
FMWCNTs- 0.5% 28 41 19.4872 0.346 7 9
ZrO2 - 0.01% 13 17 7.3735 0.368 2.6 3.2
ZrO2- 0.05% 15 17.5 9.0014 0.349 3 3.8
ZrO2- 0.1% 17.5 18.5 10.5336 0.341 3.6 4.5
ZrO2- 0.5% 21 20 14.8428 0.306 4.5 5

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M. Sajjadian et al.
Fig. 3. The trend of plastic viscosity for experimental samples with various nano materials.
concentration is enhanced. Commonly, there are repulsive forces
applied to any particle in a stability suspending mixture (Tomba �cz et al.,
2001).
The plastic viscosity amount of water-based drilling fluid as a
reference sample is obtained 12 mPa s. As displayed in Fig. 3. Plastic
viscosity is increased because of raising the excretion power among
nanomaterials and other materials in the mud system. Although, the
plastic viscosity value for each kind of nanoparticles at different weight
percent fractions in rage of 0.01–0.5 wt% was varied. Furthermore, the
value of plastic viscosity was almost increased to18 by using ZrO2
nanoparticles from 0.1 to 0.5 wt %. Furthermore, the amount of plastic
viscosity was also enhanced double nearly to 28 mPas by mixing
FMWCNTs at 0.5 wt%. The outcomes for MWNT-TiO2 nanohybrids were
as same as the rest of NPs kinds. By using 0.5 wt% MWNT-TiO2 nano­
hybrids to the reference sample, the plastic viscosity value was obtained
21 mPas. As a reason for increasing mud viscosity due to exist nano­
particles, it should be noted that viscosity is determined as interior
friction in liquid layers. So, the presence of nanoparticles in layers of
liquid could make the viscosity enhancement (Rafati et al., 2017;
Sharma et al., 2016; Sundar et al., 2013). Nanomaterial’s physical
characteristics consist of their shape and density with heat transfer
property performs a required function in mud viscosity behavior. The
enhancement of plastic viscosity was achieved by connecting and
joining nanoparticles with other solid particles especially bentonite
directly or indirectly via special side materials. The nanoparticles and
Bentonite mud may be linked or bonded together directly or through
certain intermediate chemical linkages to increase the plastic viscosity
of Bentonite mud (Kang et al., 2016). The most increase of mud plastic
viscosity is occurred by using 0.5 wt% concentration of FMWCNTs as
Fig. 4. The behavior of YP property for nanomaterials - WBDF at various mass fractions (R, ZrO2 and MWNT-TiO2 hybrids referred to left Y-axis and FMWCNTs
referred to right Y-Axis).
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Journal of Petroleum Science and Engineering 190 (2020) 107006
best choice and MWNT-TiO2 nanohybrids and ZrO2 are other choices,
respectively.
3.2.2. Yield point
The main parameter related to the movement of fluid as the opposite
direction is yield point. This parameter created by electrostatic forces
into a fluid is happened by electrical ions in the area of the active sub­
stance (Ramesh, 2001). Usually, the capability of drilling fluid for taking
away the drilling cuttings from the downhole and moving them to the
ground surface is done by yield point property (Busahmin et al., 2017;
Noah et al., 2017). The sufficient value of the yield point is very
necessary during the drilling operation to carry the drilling cutting as
well as avoiding extra pressure applied to the drilling pump. The in­
crease of mud yield point happens because of the powerful electrostatic
excretion between particles with negative ions (Barry et al., 2015).
These negative ions cause to form a stable homogenous phase without
any coalescence and flocculation. Furthermore, this negative ions sys­
tem results in a rising yield point and viscosity in drilling fluid. The yield
point value of based mud was obtained to 7.5 Pa. The influence of
nanoparticles on the yield point of mud samples are illustrated in Fig. 4.
The yield point amount of mud samples exhibits various effectiveness at
the different nano materials amounts and types. This property for ZrO2
nanoparticles in water-based drilling fluids shows a slow enhancement
tendency at all studied concentrations up to 10 Pa. The highest amount
of mud yield point was measured to 20 Pa at 0.5 wt% fraction of
FMWCNTs. The yield point trend for FMWCNTs in based mud was
strongly increased. This property for MWNT-TiO2 nanohybrids was
nearly maintained about 10.5 Pa at 0.5 wt% concentration. In conclu­
sion, FMWCNTs reveal as the best agent for yield point increaser than
M. Sajjadian et al. Journal of Petroleum Science and Engineering 190 (2020) 107006

Fig. 5. WBDF Gel strength containing different Nanomaterials determined in (A) Initial referred to 10 s duration - and (B) Final referred to 10 min (R, ZrO2 and
MWNT-TiO2 hybrids belonged to left Y-axis and FMWCNTs belonged to right Y-Axis).

other examined nanomaterials, particularly under 0.5 wt % in interaction of the nanoparticles with the matrix and surrounding water-
concentration. based drilling mud (Quintero et al., 2012). The previous researches
As mentioned in some previous researches, it concluded that Nano­ showed that several parameters could play a significant role in the
particles consist of more surface areas per volume could increase the morphology of NPs such as PH, temperature, Zr4þ template and type of

Fig. 6. Mud filtrate volumes of the experimental samples with various Nano Particles (A): The LPLT and (B) the HPHT environments (MWNT-TiO2 hybrids and ZrO2
from left Y-axis and FMWCNTs from right Y-Axis).

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M. Sajjadian et al. Journal of Petroleum Science and Engineering 190 (2020) 107006

Fig. 7. Photographic images of 0.5 wt.% of FMWCNTs, (A) Mud cake formed in HPHT environment (B) Adding in fresh water.

template (Alaei et al., 2014). The ZrO2 Nps used in this experimental
Table 6
research paper were majority spherical in shape, relatively uniform in
Filtration properties of various nanoparticles in low conditions.
size, with specific surface area nearly 85 m2/g. The PV is strongly
dependent on the amount, shape, size, and morphology of solids in Samples Mud Percentage Mud Cake Percentage
Filtrate Changes in Mud Thickness, Change In
drilling fluid composition. Also, PV enhances with some parameters
Volume, Filtrate Volume mm Thickness, %
such as the usage of more concentration, shape, and size of the solids mL respect to
content into the drilling mud (Aftab et al., 2017). Thus, the highest reference mud, %
amount of plastic viscosity was obtained from FMWCNTs due to more R 4.2 – 2.381 –
surface area in comparison with each other basing on experimental re­ MWNT-TiO2 4.1 2.38 2.381 0
sults measured rheological test. On the other hand, using FMWCNTs in hybrids -
drilling fluid composition took apart as (i) a more solid amount and (ii) 0.01%
MWNT-TiO2 3.6 14.29 2.381 0
high surface areas per volume of nanotubes. Between the rest of nano­
hybrids -
materials exanimated in this research study, it is less than the amount 0.05%
measured by the usage of MWCNT-TiO2 nano hybrid due to various MWNT-TiO2 3.3 21.43 2.381 0
shapes and specific surface area despite increasing the PV property by hybrids -
using of more amounts of ZrO2 Nps. The increases in the yield point is 0.1%
MWNT-TiO2 3 28.57 2.381 0
also linked to the strong repulsion force between the negatively charged hybrids -
and the negatively charged bentonite particles. The strong electrostatic 0.5%
repulsion between negatively charged particles prevents coagulation ZrO2 - 0.01% 4 4.76 2.381 0
and hence a strong clay platelet network is formed in the bentonite mud ZrO2- 0.05% 3.7 11.90 2.381 0
ZrO2- 0.1% 3.4 19.05 1.588 33.33
system which increases the viscosity and the yield point. Thus, there is a
ZrO2- 0.5% 3.1 26.19 1.588 33.33
direct relation between Hamaker constant and yield stress in bentonite FMWCNTs- 2.8 33.33 2.381 0
mud system containing nanoparticles (Barry et al., 2015). Analytical 0.01%
calculations of the nanomaterials behavior into a mixture are described FMWCNTs- 2.6 38.10 1.588 33.33
as the Dejaguin–Landau–Verwey–Overbeek (DLVO) theory. Basing on 0.05%
FMWCNTs- 2.3 45.24 1.588 33.33
this theory, two parameters such as net electrostatic charges on the 0.1%
particle surface and Vander Waals force them are affected by the sta­ FMWCNTs- 1.4 66.66 0.794 66.66
bilizing of particles (Hazlina et al., 2018). The yield point amount is 0.5%
enhanced by increasing these two parameters. Yield point appeared in
this research study is strongly increased by the usage of FMWCNTs
strength, respectively. As indicated in Fig. 7, the usage of FMWCNTs of
because of particle bridging effect formed by the interplay of polar
0.01–0.5 wt% in the reference sample caused the increase of gel strength
functional groups such as OH , etc. located in desirable places to operate
amounts nearly 3 times of the reference sample. By using MWNT-TiO2
with interacting attractive layers for having a strong attraction to water,
hybrids in water-based drilling fluid samples, the gel strength tendency
such as sodium.
was increased for all MWNT-TiO2 hybrids concentrations used in this
research study. The amounts of gel strength were obtained 4 and 5.1 Pa
3.2.3. Gel strength
in 0.5 concentration, respectively. The amounts of both gel strength
The other main parameter of drilling fluid rheological properties is
containing initial and final gel strengths with using ZrO2 NPs were
the Gel strength which permits the suspension of drilling cuttings and
slowly increased to 4.5 and 5 Pa in 0.5 wt%. These improvements for Gel
mud solids when the circulating system is stopped in changing of bottom
Strength were obtained about 180% and 200% in comparison with the
hole assembly or work over processes. Generally, the capability of
base sample for 10 s and 10 min, respectively. In conclusion, the best gel
drilling fluid for carrying drilling cuttings while circulation and sus­
strength characteristics are achieved by FMWCNTs compared with other
pending the drilling cutting especially when off mud circulating is very
Nano Materials exanimated in this research at the same weight fraction.
required (Sedaghatzadeh et al., 2012). The experimental results taken of
Generally, inadequate hole cleaning could cause some serious chal­
gel strength experiments in initial referred to 10 s duration and finally
lenges during drilling operations such as filling the bottom hole after a
referred to 10 min are shown in Table 4. Fig. 5 indicates the impact of
trip, reducing drill bit life and partially sticking of the drill string that
nanoparticles on gel strength under different concentrations in order of
spends time and cost for a good drilling. Hole cleaning property as a
10 s and 10 min. The gel strength amounts of reference sample as the
major function of drilling fluid is improved by increasing viscosity and
first experiment were measured in 2.5 and 3 Pa for initial and final gel
yield point of it. Hence, the usage of nanomaterials with increasing hole

8
M. Sajjadian et al. Journal of Petroleum Science and Engineering 190 (2020) 107006

Table 7 Table 8
Filtration characteristics of the drilling fluids with different nanomaterials types Electrical conductivity of experimental samples engineered in this research.
and Concentrations at HPHT conditions (6894.75 kPa and 176.67 � C). Samples Electrical Conductivity, mS/cm
Samples Mud Changes in Mud Mud Cake Change In
R 8.46
Filtrate Filtrate Volume Thickness, Thickness, %
MWNT-TiO2 hybrids - 0.01% 8.32
Volume, respect to mm
MWNT-TiO2 hybrids - 0.05% 8.42
mL reference mud,
MWNT-TiO2 hybrids - 0.1% 8.52
%
MWNT-TiO2 hybrids - 0.5% 8.55
R 14.5 – 4.763 – ZrO2 - 0.01% 8.11
MWNT-TiO2 13 10 4.763 0 ZrO2- 0.05% 7.95
hybrids - ZrO2- 0.1% 7.85
0.01% ZrO2- 0.5% 7.81
MWNT-TiO2 12.2 16 4.763 0 FMWCNTs- 0.01% 8.41
hybrids - FMWCNTs- 0.05% 8.56
0.05% FMWCNTs- 0.1% 8.61
MWNT-TiO2 11 24 3.969 17 FMWCNTs- 0.5% 8.72
hybrids -
0.1%
MWNT-TiO2 10 31 3.969 17 and plural which is named as gelling structure (Daswani and van Herk,
hybrids - 2015). It should be noted that reduction in mud cake thickness (mm)
0.5%
diminishes the possibility of sticking the drill string while drilling
ZrO2 - 0.01% 13.2 9 4.763 0
ZrO2- 0.05% 12.4 14 4.763 0 operation which introduces as other benefits of using FMWCNTs into
ZrO2- 0.1% 11.2 23 4.763 0 WBDF. Most of the reduction in mud cake thickness was obtained up to
ZrO2- 0.5% 10.5 28 3.969 17 67% by using 0.5% of FMWCNTs in comparison with the base sample
FMWCNTs- 12 17 4.763 0 without Nano Materials as seen in Table 6. The experimental results
0.01%
FMWCNTs- 9.8 32 3.969 17
measured from HPHT filtration experiments are illustrated in Table 7
0.05% and Fig. 6-B. Displaying in Table 7, increasing of FMWCNTs concen­
FMWCNTs- 7.8 46 3.175 33.5 trations decrease mud filtration volume of experimental samples
0.1% because of forming the sturdy and stiff structure infiltration cake.
FMWCNTs- 6 59 3.175 33.5
Actually, with increasing FMWCNTs concentrations, mud cake thickness
0.5%
decreases due to an increase in the number of nanoparticles in the
drilling fluid system resulted in blocking very tiny holes and small
cleaning ability of drilling fluid may improve drilling operation per­ cavities (as nanoscale) in mud cake surfaces. Thus, the reduction of mud
formance by reducing significant challenges and problems. filtration volume enhances. These experimental tests were carried out to
show drilling fluid engineered in this research study could tolerate the
3.3. Filtration loss HPHT situation that happened in high depth wells. Also, NPs exani­
mated in this research study illustrated the same trend infiltration test
Filtration properties were evaluated by doing experiment tests in for both LPLT and HPHT situation. It is important to mention that mud
different pressure and temperature situations named LPLT and HPHT cake formation for all the experimental samples using ZrO2 and
situations. Filtration properties were investigated by obtaining some FMWCNTs in a shorter time compared with the reference sample. Mud
parameters such as Filtration loss volume, the thickness of mud cake filtrate volume collected infiltration test of MWNT-TiO2 hybrids is more
after passing a specific period. This property in LPLT for the reference than based mud. In these experimental tests, it was considered that mud
sample was 4.2 mL after half of the hour. The experimental results filtration properties such as filtration volume and cake quality were
measured in LPLT situations are illustrated in Table 6 and Fig. 6-A. As considerably enhanced by using various concentrations of ZrO2 and
shown in Fig. 6-A, it is found that using ZrO2 in various concentrations FMWCNTs. The most desirable quality, thinner mud cake and minimum
gently decrease the filtration loss volume up to 3.1 mL at 0.5 wt% in filtration volume related to FMWCNTs and ZrO2, respectively.
concentration. Also, filtration loss volume is strongly reduced to1.8 mL The nanomaterials got jointed to drilling mud additive to create thin
by adding 0.5 wt % of FMWCNTs. By using 0.01 wt% of MWNT-TiO2 and very low permeable mud cake for avoiding fluid loss entrance.
hybrids into the reference mud sample, the fluid loss amount was ob­ Therefore, all nanomaterials introduced in this research could decrease
tained 4.1 and this property was slowly reduced to 3 mL by 0.5 wt % mud filtration volume (Sadeghalvaad and Sabbaghi, 2015). It probably
concentration of MWNT-TiO2 hybrids. The reason for reducing filtration claimed in several previous types of research that nano diameter agents
loss volume by using FMWCNTs is the enhancement of electrostatic along with modified structures including nano platelets and nanotubes
forces among negative ions of FMWCNTs and other particles that creates blocked nano pore throats of the drilled substructures for stopping fluid
a suitable suspended system with avoiding particle flocculation. invasion (Ismail et al., 2016). Thus, the most reduction of mud filtrate
Deflocculated particles and well-suspended particles into a drilling fluid volume is achieved at a concentration of 0.5 wt % of FMWCNTs. By
system could make to form a thin and low permeable mud cake on the raising the temperature, mud filtration characteristics such as mud
surface of the lost zone (Barry et al., 2015). The usage of FMWCNTs in filtrate volume and mud cake thickness are increased due to several
the WBDF system could be remarkably decreased mud filtration volume. reasons such as reducing mud viscosity and destructing of filtration
It is an indirect relationship between the concentration of FMWCNTs reducer chemical agents. In concentration 0.5 w % of MWCNTs, the mud
and filtration volume decline. So, the mud filtration volume is decreased cake thickness is relatively reduced up 33% compared to the base
with the enhancement of FMWCNTs concentration. It happens because sample during the HPHT environment.
of the electrostatic attractive force among FMWCNTs and other solid
particles such as positive edge bentonite with negative face or edge 3.4. Electrical conductivity
FMWCNTs. The attractive force occurred between FMWCNTs and other
particles that could build a gelling structure which improves mud con­ This part of the experiments was carried out to determine that the
sistency and decrease mud filtration volume. Some factors act in chemical components utilized to prepare mud are matched with sodium
determining force between two particles consists of diameters, chemical bentonite and the alteration of electrical conductivity for experimental
components, and electrical load. These forces cause to form aggregation samples is suitable. It is important to know that logging interpretation

9
M. Sajjadian et al. Journal of Petroleum Science and Engineering 190 (2020) 107006

Table 9
Comparisons of present study data with some recent researches on using Nano Materials in water-based mud.
NPs Concentrations wt.% Mud Type Properties Parameters % Change Reference

CuO SiO2 0.1, 1 WBDF PV þ50 þ33.34 Sharma et al. (2016)

YP 4.76 þ14.29
Mud Filtrate Volume -LPLT 6.35 6.72
CNT 0.14 WBDF PV þ7.14 Sundar et al. (2013)
YP þ19.56
SMA/SiO2a 2.00 WBDF PV þ7.69 Kang et al. (2016)
YP 0
Mud Filtrate Volume -LPLT 21.95
MWCNTs 1 WBDF PV þ60.87 (Ramesh, 2001; Razali et al., 2018)
YP þ20
Mud Filtrate Volume -LPLT 65
MWCNTs 0.057 WBDF PV 0 Barry et al. (2015)
YP þ5.41
Mud Filtrate Volume -LPLT þ4
MWCNTs 0.5 WBDF PV þ133.34 This Research
YP þ156.25
Mud Filtrate Volume -LPLT 67
a
An amphiphilic polymer/nano-silica composite.

may be unreliable and invalid due to the change of electrical conduc­
tivity for experimental samples (Zanten, 2014). Mud should create a
good conductivity causing low and week signals or unsuitable signals for
log information measuring. One of the main reasons for defective elec­
trical infiltration into the subsurface zone is transmission electricity of
drilling fluid. In this experimental research, Conductivity Meter was
utilized to measure electrical conductivity for each sample. The exper­
imental results achieved in this research were documented in Table 8. As
shown in Table 8, it finds that FMWCNTs particle stability is chemically
favorite. Thus, conductive properties for experimental samples exani­
mate illustrate no mark of any discontinuity. Replacing with, upon
expensive-long time treatment, FMWCNTs could enhance the efficiency
of drilling fluid from the view of electrical transmission. The
high-performance drilling fluid, especially with suitable electrical
transmission, could create optimum cost and time in drilling operation
by enhancing drilling bit durability and speed of bit infiltration into the
rock formation.
Comparing to other publications (see Table 9) showed the positive
effects of low concentrations of functionalized MWCNTs for the mud
properties enhancement of water-based drilling fluid. Furthermore, the
very low concentration of the FMWCNTs, other nanomaterials utilized
in this research study for WBDF has proved to be useful and effective.
PV and YP were improved by using FMWCNTs significantly. As seen
in Table 8, the yield point value by using multi-wall carbon nanotubes
was increased nearly from 5 at 0.057 wt% to 20% at 1 wt%. However,
this property is increased by nearly 157% by using just 0.5 wt% of
MWCNTs. The Mud Filtrate volume under LPLT condition was reduced
from 6.7 at 0.1 wt% to 65% at 1 wt% in several studies accomplished on
the WBMs during past years. This property is decreased to 67% at 0.5
wt% of MWCNTs. Particularly, the mud filtrate volume shows the
highest enhancement in this contrast table, which may be affected by the
very effective improvement of the mud properties that stabilized the
borehole under HPHT condition and thus, reduced the formation
damage.
4. Conclusions
In this research, several Nanomaterials were mixed in bentonite mud
to improve drilling fluid characteristics by carrying out a collected of
rheological, filtration loss and conductivity experiments. The experi­
mental results accomplished illustrated that using MWNT-TiO2 hybrids
and ZrO2 could increase the yield point, plastic viscosity and the gel
strength of the drilling muds, although this increasing trend may not
favorable due to side undesirable effects on mud filtrate volume. Plastic
viscosity, yield point and gel strength of the WBDF were strongly
improved by using FMWCNTs from 0.01 to 0.5 wt% concentration
which is desirable. The filtrate loss tests illustrated that the FMWCNTs
makes mud filtrate volume decreases by obtaining firm and taught
structure at LPLT and HPHT situations. The mud cake thickness is
considerably reduced by using FMWCNTs into mud bentonite systems.
The enhancement conduction of experimental samples is another fa­
vorite property that enhances the electrical conduction and drilling
operation performance.
Acknowledgments
The authors would like to thank the Department of Chemistry En­
gineering at Marvdasht Branch, Islamic Azad University (IAU), Iran for
supporting this research such as providing chemicals and testing facil­
ities to do this report.

Appendix A. Supplementary data

Supplementary data to this article can be found online at https://doi.org/10.1016/j.petrol.2020.107006.

Nomenclature

API American Petroleum Institute

YP Yield point
MWCNTs Multi-walled carbon nanotube
HPHT High-pressure High temperature
LPLT Low-pressure low temperature
N Behavior index
K Consistency index

10
M. Sajjadian et al. Journal of Petroleum Science and Engineering 190 (2020) 107006

Φ Dial Reading

Units
Cc Cubic centimeter
Cp Centipoise
Nm Nanometer
o
C Degree of Celsius
Pa s Pascal’s second
mPa s milli Pascal’s second

Units Conversion
1g 1lb
350cc 100ft 2 0.4788 Pa
1 cp 1 mPas

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