Journal of Petroleum Science and Engineering 213 (2022) 110327

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Journal of Petroleum Science and Engineering

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

Evaluation of novel microemulsion-based (O/W) drilling fluid with

nonionic surfactant and shale interaction mechanisms
Raphael R. Silva a, **, Alfredo I.C. Garnica a, b, Giovanna L.R. Leal b, Luara R. Viana a, Júlio C.
O. Freitas c, Alex N. Barros d, Thales L.S. Silva e, João Adauto de S. Neto e, Fabiola D.
S. Curbelo a, b, *
a
Postgraduate Program in Chemical Engineering, Federal University of Paraiba, João Pessoa, 58051-900, Brazil
b
Chemical Engineering Department, Federal University of Paraíba, João Pessoa, 58051-900, Brazil
c
Chemical Institute, Federal University of Rio Grande do Norte, Natal, 59078-970, Brazil
d
Baker Hughes, Brazil
e
Postgraduate Program in Geoscience, Federal University of Pernambuco, Recife, 50670-901, Brazil

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

Keywords: The increasing production of hydrocarbons from unconventional reservoirs, particularly water-sensitive for­
Rock-drilling fluid interaction mations, has led to the emergence of technologies necessary to maintain wellbore stability. The drilling fluid
Reactive formations must always be adequate to the needs presented by such formations since serious problems may be generated due
Shales
to inadequate drilling fluid planning. Microemulsions appear in this scenario with advantages over the tradi­
Nonionic surfactants
Swelling inhibition
tional fluids already used by the industry due to their thermodynamic stability, ease of preparation, and is
environmentally acceptable. This work aimed to evaluate the inhibition capacity of microemulsion-based drilling
fluids comprised of nonionic surfactants and pine oil, environmentally friendly components, and never before
assessed in the laboratory. Initially, a shale sample from a sedimentary basin in Northeastern Brazil was char­
acterized using XRF, XRD, TGA, and DTA. The microemulsions, base of the drilling fluids, were formulated from
a ternary phase diagram, in which a water/glycerol solution (1:1 by mass) was used as the aqueous phase, pine
vegetable oil as the oil phase, and two nonionic surfactants, Ultranex NP100 and Alkest Tween 80 were used
separately in the formulated systems. Potassium citrate (INIB1) and potassium sulfate (INIB2) were also used to
inhibit the swelling of reactive formations. In order to evaluate the behavior of drilling fluids, rheology tests,
filtrate loss, filtercake thickness, and permeability were considered. Finally, drilling fluid systems were tested for
shale inhibition and dispersion capability. In addition to systems composed of INIB1 and INIB2, potassium
chloride (KCl) (INIB3) was evaluated, and a system without a swelling inhibitor (SI). It was observed that the
shale samples presented clay minerals from the smectite group, which represent a more significant interaction
with water for swelling of hydratable formations. Drilling fluids showed rheological behavior following the
Herschel-Bulkley model. There is a variability of interactions in the fluids concerning the concentrations of
surfactant, oil phase, and swelling inhibitor, with more significant responses associated with increased surfactant
concentration in the microemulsion. The drilling fluids showed a significant swelling inhibition, especially the
fluid formulated from the surfactant Ultranex NP100 and INIB2, with a 6.9% swelling variation. Excellent results
concerning dispersibility were also achieved, with the NP100_INIB1 fluid being the lowest dispersion of cuttings
(0.075% and 0.215%). In general, the microemulsion-based drilling fluids efficiently inhibited swelling of the
shale sample, showing good rheological and filtration behavior.

1. Introduction process of exploratory oil and gas wells. They must present physico­
chemical characteristics compatible with the types of drilled formations.
Drilling fluids are an essential and usual element in the drilling Incompatibility of drilling fluid may significantly increase the total cost

* Corresponding author. Postgraduate Program in Chemical Engineering, Federal University of Paraiba, João Pessoa, 58051-900, Brazil.
** Corresponding author.
E-mail addresses: ribeiro.rse@gmail.com (R.R. Silva), fabioladias@yahoo.com (F.D.S. Curbelo).

https://doi.org/10.1016/j.petrol.2022.110327
Received 3 August 2021; Received in revised form 26 January 2022; Accepted 20 February 2022
Available online 9 March 2022
0920-4105/© 2022 Elsevier B.V. All rights reserved.
R.R. Silva et al.
of drilling, causing a reduction in wellbore efficiency and, thus, low
productivity (Reed, 1989; Bennion et al., 1994, 1996; Zhou et al., 1996;
Tare et al., 1999; Knox and Jiang, 2005; Qiansheng et al., 2010; Khodja
et al., 2010; Denney, 2011; Qiu et al., 2011; Qutob and Byrne, 2015;
Elkatatny et al., 2019; Zhao et al., 2019). Wellbore instability problems
due to swelling of shales are widely known in the industry as the primary
source of increased operating cost, both during drilling and completion
of oil wells (Nesbitt et al., 1985). It is estimated that this type of for­
mation represents about 75% of all drilled formations. The interaction
between an inadequate fluid and shales accounts for 90% of all drilling
problems (Berry et al., 2008; Farrokhrouz and Asef, 2013; Aghdam et al.,
2021), mainly owing to recent discoveries of non-conventional reser­
voirs (Zhao et al., 2019). However, it is reported that this aspect is not
fully understood (Zendehboudi and Bahadori, 2017; Koteeswaran et al.,
2018; Hazra et al., 2019).
Shale consists of a fine-grained sedimentary rock containing a
considerable amount of clay minerals (Huang et al., 1998; Ahmed and
Meehan, 2016). Commonly, the clay minerals found in shales are illite,
montmorillonite, smectite, calcite, and kaolinite, and each plays a
different impact on the physicochemical behavior of the shale. For
instance, in the presence of free water, clay minerals of the montmo­
rillonite type present a high swelling tendency, increasing their initial
volume due to water absorption between the individual clay unitary
layers. In contrast, those of the kaolinite type will remain essentially
unchanged. Thus, the behavior of shales is directly related to the amount
of clay minerals present in the sample (Koteeswaran et al., 2018).
The drilling fluids are in constant contact with the formations, so it is
expected they inhibit or delay the phenomenon of swelling in reactive
formations essentially caused by the interaction between the two. Oil-
based drilling fluids (OBDF) present an excellent inhibiting property,
showing greater stability in high-temperature environments. Nonethe­
less, this drilling fluid is restricted due to environmental regulations and
high costs. Water-based drilling fluids (WBDF) are increasingly used
because they are considered more environmentally acceptable and
present good rheological properties (Van Oort, 2003; Kamal et al., 2015;
Aftab et al., 2017). However, when finding hydratable formations, the
choice for this fluid may not be as suitable as OBDF. When in contact
with WBDF, the shale may promptly take up water from the drilling
fluid, causing swelling or degrading the shale (Patel et al., 2007),
resulting in wellbore instability. Problems related to instability include
bit balling, caving, sloughing, stuck pipe, and even the wellbore collapse
(Zhao et al., 2019; Murtaza et al., 2020).
Several studies are found in the literature on swelling inhibitors for
application in WBDF (e.g., An and Yu, 2018; Chu et al., 2019; Liu et al.,
2021; Ahmad et al., 2021a,b; Quainoo et al., 2021; Su et al., 2022)
Swelling inhibitors must not only address the hydration reduction of
formations, but they also must be environmentally acceptable and have
a low total cost to the drilling process. Among the chemical additives for
swelling inhibition found in the literature, surfactants have gained
prominence due to their excellent inhibition potential.
Surfactants, natural or synthetic amphiphilic structures, play an
essential role in inhibiting hydratable formations. These molecules sta­
bilize two-phase mixtures by reducing interfacial tensions between oil
and water. In drilling fluids, the addition of these molecules can control
problems related to wellbore instability, differential sticking, in addition
to serving as detergents for the cuttings in the drill bit (Quintero, 2002).
The most applied surfactants as swelling inhibitors are the cationic
and nonionic types (Ahmed et al., 2019). Cationic and nonionic sur­
factants are adsorbed on the surfaces of hydratable clays, primarily due
to the silanol group and negative charges present in the interlayers (Cui
and van Duijneveldt, 2010). The adsorbed surfactant, which generally
has a long chain (Muhammed et al., 2021), suppresses the swelling effect
of clays and uses the molecule’s hydrophobic chain to repel water ab­
sorption. Liu et al. (2019) evaluated that the mixture of nonionic sur­
factants Span 20 and Tween 60 can increase the hydrophobicity of the
shale, forming a hydrophobic membrane on the surface of the formation,
2
Journal of Petroleum Science and Engineering 213 (2022) 110327
which reduced and weakened the number of hydrogen bonds between
the water and the formation, significantly reducing the amount of water
entering the shale. Murtaza et al. (2020) evaluated the quaternary
ammonium dicationic surfactant with phenyl linkers, evaluating that
the base surfactant formulations presented a high reduction rate in
bentonite swelling a maximum decrease in the linear swelling rate.
Kamal et al. (2020) proposed a drilling fluid formulation from Gemini
surfactants, organophilic clay, and polyacrylamide. They observed that
the formulation demonstrated efficient shale swelling inhibition, as the
Gemini surfactant changed the rock wettability, with a linear swelling
rate on the order of 10% compared to 18% swelling when the shale
sample was immersed in water. Besides, the proposed drilling fluid
showed improved rheology properties at elevated temperatures.
Huang et al. (2017) developed a novel method to measure the
wettability of shale power by determining the real contact angle, using a
series of surfactants in the drilling fluids formulation. The tests revealed
that the mix of 0.05% of polyamine (PA) and 0.1% of twelve alkyl two
hydroxyethyl amine oxide (THAO) showed a 10.11% linear expansion
rate. Oseh et al. (2020) used the nonionic surfactant
polyethylene-block-poly (ethylene glycol) (PE-b-PEG) and a series of
other cationic, anionic and nonionic surfactants to synthesize the
(3–Aminopropyl) triethoxysilane polypropylene-nanosilica composite
(PNSC + NH2) and apply it in a water-based drilling fluid. The author
also tested drilling fluids formulated with KCl and a mixture of KCl and
partially hydrolyzed polyacrylamide (HPAM). It was observed that after
60 h of the linear swelling test, samples in contact with PNSC + NH2
showed 29% free swelling, compared to 40% with the KCl + HPAM
mixture and 44% with KCl.
Other works using surfactants to inhibit shale swelling can be found
in the literature, such as in Yue et al. (2018), who used an optimized
surfactants combination of 0.2 wt% CTAB and 0.1 wt% SDBS, and found
that the surfactant combination effectively reduced the surface tension
of the WBM and increased the contact angle with shale, hence opti­
mizing the inhibition. Rana et al. (2019) reported the effect of sodium
dodecyl sulfate modified graphene (SDS-Gr) in WBM and found that the
surfactant improved the shale inhibition characteristics and enhanced
the rheological features. Xu et al. (2019) studied the 1-Octyl-3-methyli­
midazolium bromide (OMB), which chemical structure contains an
amphiphilic structure, thus behaving as a surfactant, as a promising
shale inhibitor; the authors reported that OMB could effectively reduce
the surface tension of rock formations at low concentrations, hence
becoming a good candidate as an additive for drilling shale formations.
Ahmad et al., 2021a,b assessed two Gemini surfactants at different
concentrations on rheology, filtration, and inhibition characteristics.
The authors showed a significant improvement in the swelling shale
inhibition at concentrations of 0.2% in the drilling fluid.
Natural surfactants and extract leaves have also been investigated by
Shadizadeh et al. (2015), who used Zizyphus spina-christi extract (ZSCE),
a novel nonionic surfactant, and found that ZSCE had a better perfor­
mance compared to KCl and PA. Aggrey et al. (2019), who used a novel
nonionic surfactant extract derived from Chromolaena odarata (CO),
concluded that the degree of inhibition is comparable to industrial KCl;
however, the CO presented a lower filtrate volume compared to the
latter. Aghdam et al. (2019) used a natural surfactant (quillaja saponin)
as a shale inhibitor and investigated its compatibility with other addi­
tives, showing that it was compatible. Ghasemi et al. (2019) assessed the
use of Korean red ginseng root extract, which is rich in nonionic sur­
factant, as a shale inhibitor and concluded that inhibition property was
comparable to CTAB and KCl. However, little attention has been given to
microemulsions inhibiting the swelling phenomenon in shales.
Microemulsions are thermodynamically stable and transparent
mixtures, comprised of at least three components: an oil phase, an
aqueous phase, and a surfactant (Tartaro et al., 2020). Depending on the
components’ proportions, the microstructure of microemulsions ranges
from tiny water droplets dispersed in the oil phase (W/O micro­
emulsion) to oil droplets dispersed in the aqueous phase (O/W
R.R. Silva et al.
microemulsion).
Microemulsions, both water-in-oil (W/O) and oil-in-water (O/W),
have been investigated in the formulation of drilling fluids. Hayes et al.
(1977) have addressed the applicability of water-in-oil micro­
emulsion-based drilling fluids (MEDFs) comprised of water, sodium
petroleum sulfonate, hydrocarbon, and bentonite. The drilling fluids
showed suitable viscosity, gel strength, and low fluid loss characteris­
tics, varying from 1 to 14 mL. Besides being more economical than
conventional W/O emulsion muds, the drilling fluids showed desirable
lubricity characteristics, primarily due to the surfactant.
Davies et al. (1997) investigated the usage of a microemulsion as an
additive to water-based drilling fluids to minimize the tendency of dif­
ferential sticking of the fluid and mud cake, using a series of surfactants
and vegetable and mineral oils. Anionic surfactants presented better
results when compared to cationic and nonionic surfactants, providing
the required properties without affecting mud rheology. Quintero et al.
(2009) evaluated a multi-functional treatment fluid comprised of a
microemulsion formulated with surfactants, cosurfactants, brine, a sol­
vent, and an acid. The fluid was effective in reducing skin damage and
improving productivity.
Another critical factor to be considered is the environmentally
acceptable character promoted by microemulsions, as they are usually
formulated with vegetable oil, water, and low environmental impact
surfactants. Junior et al. (2021) applied nonionic surfactant NP100 and
pine oil to formulate microemulsion-based drilling fluids and investi­
gated their impact on the filtrate volume and filtercake thickness. The
surfactant at a concentration of 45% in the microemulsion resulted in
the lowest filtrate volume, being 1.3 mL, and a reduction in the pine oil
concentration showed a lower filtercake thickness and permeability.
Sousa et al. (2021) considered the nonionic surfactant Tween 80 and
pine oil to develop a novel environmentally friendly
microemulsion-based drilling fluid. The authors reported a drilling fluid
with high lubricity (0.07638), thermal stability, and low fluid loss (4.0
mL). Besides, the formulated ME-based drilling fluid was considered
non-toxic, as it was presented with a toxicity test. Paswan and Mahto
(2020) evaluated the application of sunflower oil and an anionic sur­
factant, sodium methyl ester sulfonate (SMES), in oil-in-water emul­
sion-based drilling fluids. The evaluated drilling mud presented a low
friction coefficient and a reduction in the contact angle and interfacial
tension, thus encouraging wetting characteristics of the developed
drilling fluid.
In this paper, for the first time, a novel drilling fluid formulation was
proposed based on microemulsions as the continuous phase of the mud,
and the mechanism of interaction with shale was investigated. Two
nonionic surfactants were used in different formulations of
microemulsion-based drilling fluids, being the Ultranex NP100 and
Alkest Tween 80, associated with two potassium salts (potassium sulfate
and citrate) to investigate the inhibition potential in shale swelling.
Blank samples of drilling muds without inhibitors were also used to
evaluate the inhibition potential of the ME-based drilling muds per se. A
shale sample was characterized regarding its chemical and mineralog­
ical composition, as well as its thermal behavior. The shale inhibition
performance of the microemulsion-based drilling fluids was investigated
through the linear swelling test and hot-rolling dispersion test. The
rheological and filtration performances of the drilling fluids were also
investigated through API-Recommended Practice tests.
2. Materials and methods
2.1. Materials
A shale sample from the Rio do Peixe sedimentary basin, located in
the Northeast of Brazil, was characterized regarding its chemical and
mineralogical composition. This sedimentary basin was formed during
the separation and disaggregation of the African and South American
continents. The basin comprises three sub-basins, representing three
3
Journal of Petroleum Science and Engineering 213 (2022) 110327
mid-grabens named west to east, sub-basins Brejo das Feiras, Sousa, and
Pombal, separated by basement uplift.
The microemulsion-based drilling fluids were prepared using, as the
continuous phase, a microemulsion comprised of a water/glycerol (1:1)
solution, as the aqueous phase; pine oil as oil phase; and nonionic sur­
factants, these being Ultranex NP100 and Alkest Tween 80 (provided by
Oxiteno). Solid additives such as bridging agent, fluid-loss control, and
viscosifying and weighting material were used. Chemical additives to
inhibit shale swelling were also used, these being potassium salts: po­
tassium citrate (INIB1), potassium sulfate (INIB2), and potassium chlo­
ride (INIB3), the latter being the most commonly used in well drilling of
oil and natural gas (Table 1). Tests were also carried out using two blank
drilling fluid samples with surfactants Ultranex NP 100 and Alkest
Tween 80 in order to compare the flow and inhibiting behaviors.
For characterizations regarding rheology, filtration, and swelling
inhibition, a total of eight drilling fluids were formulated, varying the
nonionic surfactant used in their formulations and the swelling shale
inhibitor. Two of the drilling fluids mentioned above were not prepared
with swelling inhibitors to visualize the drilling fluids’ inhibitory
capacity.
2.2. Methods
The experimental procedure flow chart of the present study is shown
in Fig. 1.
2.2.1. X-ray diffraction (XRD)
In order to identify the crystalline phases of the shale sample, a
SHIMADZU Model LabXRD-6000 diffractometer was used, using Kα
radiation of Cu (40 kV/30 mA), with a θ-2θ type goniometer rotating at a
speed of 2◦ /min and step 0.02◦ , in the range of 5–60◦ .
2.2.2. X-ray fluorescence (XRF)
In order to quantitatively map the chemical elements of the shale
sample, a SHIMADZU Model EDX-720 energy dispersive spectrometer
was used. The generation of X-rays was performed employing a tube
with an Rh target.
The X-ray fluorescence (XRF) technique is an advanced tool that
reveals the chemical composition of shale samples in a short measure­
ment time, which makes analysis possible and cost-effective (Gromet
et al., 1984; Baig and Urbancic, 2010; Lentz et al., 2014). Numerous
studies have been conducted and indicate that FRX may reflect a higher
resolution of variability in shale composition than other standard tech­
niques such as X-ray diffraction (XRD). It may be due to a shorter
measuring range and more available element candidates for a compre­
hensive analysis (Tjallingii et al., 2007; Turner et al., 2015, 2016).
2.2.3. Thermogravimetric analysis (TGA) and differential thermal analysis
(DTA)
To evaluate the thermal behavior of the shale sample, simultaneous
equipment (TGA/DTA) SHIMADZU Model DTG-60H was used, condi­
tioning the sample in a dynamic nitrogen atmosphere, with a heating
rate of 10 ◦ C/min and a flow of 50 mL/min in an alumina crucible,
obeying the temperature range varying from 28 ◦ C to 1000 ◦ C.
2.2.4. Ternary phase diagram and drilling fluids preparation
Initially, two ternary phase diagrams were elaborated using the same
aqueous phase, water/glycerol solution (1:1), and oil phase, pine oil.
Two nonionic surfactants were used in different formulations, Ultranex
NP100 and Alkest Tween 80. The diagrams were obtained by titration.
The surfactant was added to a mixture of the aqueous and oil phases
with the initially known mass composition to form a single clear phase
featuring the microemulsion.
The titration took place until the solubility of the ternary mixtures in
the entire region of the diagram was verified, observing the formation or
disappearance of the microemulsion region (single-phase system) or of
R.R. Silva et al. Journal of Petroleum Science and Engineering 213 (2022) 110327

Table 1
Formulations of microemulsion-based drilling fluids.
Additives NP100 T80

INIB1 INIB2 INIB3 SI INIB1 INIB2 INIB3 SI

Water/Glicerol (1:1) (g) 175 175 175 175 175 175 175 175
Pine oil (g) 17.5 17.5 17.5 17.5 17.5 17.5 17.5 17.5
Ultranex NP100 (g) 157.5 157.5 157.5 157.5 – – – –
Alkest Tween 80 (g) – – – – 157.5 157.5 157.5 157.5
Calcitea (g) 11.7 11.7 11.7 11.7 11.7 11.7 11.7 11.7
HP-starcha (g) 1.2 1.2 1.2 1.2 1.2 1.2 1.2 1.2
Cloisite 20 Aa (g) 4.7 4.7 4.7 4.7 4.7 4.7 4.7 4.7
Xanthan guma (g) 0.6 0.6 0.6 0.6 0.6 0.6 0.6 0.6
Potassium citratea (g) 20 – – – 20 – – –
Potassium sulfatea (g) – 20 – – – 20 – –
Potassium chloridea (g) – – 20 – – – 20 –
Baritinea 58.3 58.3 58.3 58.3 58.3 58.3 58.3 58.3
Water (mL) 250 250 250 250 250 250 250 250
a
Drilling fluids’ additives amounts for g/350 mL of microemulsion.

Fig. 1. Experimental flowchart.

other system’s phases. Visual observation of the macroscopic properties
of the samples, such as the number of phases and physical state, makes it
possible to determine the limits between the microemulsion and two and
three phases’ regions. A centrifuge for phase separation, an analytical
balance, and magnetic stirrers for mixing the components were used in
these experiments. The temperature of the experiments was 28 ◦ C. From
the diagrams elaborated, one point was chosen in the microemulsion
region (oil-in-water region) and used as the continuous phase of the
drilling fluids.
The drilling fluids were then formulated as the continuous phase the
microemulsions prepared above, and the solid additives shown in
Table 1 were added following the order of addition presented therein.
The mixtures were stirred on a Fann Hamilton Beach mixer, with 10-min
intervals between each addition.
2.2.5. Rheological properties
The rheology of drilling fluids is an important parameter to be
analyzed since the behavior of the fluid in the wellbore depends strongly
on viscosities, gel strengths, and thixotropy. The microemulsion and
chemical swelling inhibitor effects on the drilling fluids’ rheology were
investigated through rheological analysis of the formulated drilling
fluids.
For this purpose, the Fann rotational viscometer, model 35 A, was
used, and the measurements consisted of measuring the shear stress at
six different speeds, namely: 3, 6, 100, 200, 300, and 600 rpm, following
the standard API 13B-1 at room temperature. The rheological parame­
ters plastic viscosity, PV (cP), apparent viscosity, AV (cP), and yield
point, YP (lb/100 ft2) were then calculated following Equations (1)–(3).
PV = θ600 − θ300 (cP), (1)
AV = θ600 /2 (cP), (2)
( / )
YP = θ300 – PV lb 100ft2 , (3)
where: θ600 is the reading at 600 rpm; θ300 is the reading at 300 rpm.

4
R.R. Silva et al.
With the shear stress and shear rate data, it was possible to plot the
flow curves of the microemulsion-based drilling fluids. The Herschel-
Bulkley parameters, the flow behavior index, n (dimensionless), con­
sistency index, k (cP), and low-shear yield point, τy (lb/100 ft2) were
calculated following the API standards RP13-D.
The parameter n, flow behavior index, physically indicates the dis­
tance of the drilling fluid from the Newtonian model. The parameter K,
consistency index, is a rheological property related to the cohesion of the
individual particles of the fluid, their capacity to deform, and their
resistance to flow. This parameter describes the degree of resistance of
the fluid to flow and is given in cP.
2.2.6. Filtration test
After the rheology test, low-pressure and low-temperature fluid loss
(LPLT) tests were performed by static filtration to estimate the volume of
filtrate (filtrate loss) that tends to invade permeable formations. Ac­
cording to Burgoyne et al. (1988), this test is indicative of the rate at
which permeable formations are sealed by filtercake deposition after
being penetrated by the drill bit.
For this purpose, the drilling fluids were previously stirred in a
Hamilton Beach mixer. The test followed API standards (API Recom­
mended Practice 13B-1). API filter press was used to determine the
filtration rate, and Whatman filter paper n◦ 50 was used as the filter
medium. The fluid was subjected to the pressure of 100 psi at 28 ◦ C for
1800 s. After the determined time, the volumes of filtrate (mL) collected
in a beaker were measured.
2.2.7. Filtercake thickness and permeability
The thickness of the filtercake, ε (mm), formed after the filtration
test, was measured using the scheme shown in Fig. 2. Two glass plates of
known thicknesses were used. The filter papers, collected after the
filtration tests, were placed between the two plates and, with the aid of a
caliper, the total thickness was measured, then the filtercake thickness
was subtracted (Farias et al., 2006). Two measurements were taken on
each side of the set of glass plates, using the arithmetic mean of the two
measurements.
The filtrate viscosity was measured using Brookfield DVIII Ultra
rheometer with a CPE52 spindle. The rheometer was coupled to a
thermostatic bath and a computer, controlled by Rheocalc 32 software.
Two temperatures were used in the measurements, being 30 and 55 ◦ C,
to establish a relationship with the different temperatures of the oil
wells.
The filtercake permeability was evaluated under the conditions of
100 psi, 30 min, and filter paper area of 45 cm2 (Numkam and Akbari,
2019), based on Darcy’s equation for axial flow (Foust et al., 1982).
k = 8.95 ∗ 10− 5 ∗ FL ∗ ε ∗ μf , (4)
Fig. 2. Schematic representation of filtercake thickness measurement, ε.
5
Journal of Petroleum Science and Engineering 213 (2022) 110327
where: k is the permeability of the filtercake formed after the static
filtration test (mD); FL is the filtrate loss (mL); ε, the filtercake thickness
(mm); and μf, the viscosity of the filtrate (cP).
2.2.8. Hot rolling dispersion test
The shale cuttings dispersibility test was conducted to measure the
tendency of the shale sample to disintegrate in the presence of the
formulated drilling fluid. The test was carried out in a stainless-steel cell
in an oven at high temperature and continuous rotation. The degree of
dispersion experienced by shale cuttings directly indicates the inhibiting
capabilities of a drilling fluid (Aramendiz and Imqam, 2019). The dis­
persibility test compares the initial and final masses of formation sam­
ples after continuous contact with drilling fluids at constant temperature
and rotation.
In order to carry out the test, 20 g of a shale sample was initially
ground between ABNT sieves n◦ 4 and n◦ 8, with openings 4.75 mm and
2.36 mm, respectively. A Roller Oven rotary oven, Fann model 705 ES,
was used and stainless-steel cells with a capacity of 400 mL each. Then,
the shale sample was added to 350 mL of microemulsion-based drilling
fluids and gently mixed using a spatula. The cells were then rotated at
50 rpm and heated to 66 ◦ C constantly for 16 h.
At the end of the tests, the cells were cooled to 28 ◦ C, and the cell
contents were filtered through an ABNT No. 100 sieve, with an opening
of 0.150 mm, with a freshwater flow of 2 L/min. The shale samples with
less than 100 mesh were considered dispersed, then dried in an oven at
60 ◦ C until a constant weight was measured. The dispersibility of the
samples was obtained using Equation (5).
D = (ΔW / W0 ) x 100 (%), (5)
where: D is the percentage of dispersibility (%); W0 is the initial weight
of the shale sample (g); ΔW is the difference between the final and initial
shale weight (g).
After the calculation of dispersibility, XRD tests were performed on
the shale samples to verify the differences in the basal spacing, d, of the
samples. The dispersed samples were previously ground in mesh sieve
No. 200. The XRD analysis setup was the same used in the initial sample
analyses.
2.2.9. Linear swelling test
Due to direct exposure to drilling fluids, shale swelling was measured
using the linear swelling test of a bentonite clay sample without
confinement stress. This test measures the interaction between drilling
fluids and clay inserts as a function of the time the samples are exposed
to the fluids. For this purpose, the Fann model 2000 Linear Swell-Meter
(LSM) equipment with four channels was used.
This equipment is designed to test and study the reactivity of shales
found in oil well drilling. In the field, the objective is to apply the in­
formation found in order to anticipate and/or correct problematic en­
counters of hydratable formations, minimizing the risks and drilling
costs caused by these so-called unpredictable materials. Initially, 20 g of
dry clay, previously sieved in 200 mesh, were compacted (reconstituted)
using the two-cell hydraulic compactor that complements the equip­
ment. The pulverized sample was placed in a cylindrical mold, and then
a compaction pressure of 10,000 psi was applied and maintained while
compaction was taking place. Tests indicated that this constant pressure
for 90 min resulted in satisfactory sample plugs, with 28.6 mm in
diameter and 12.7 mm in thickness.
The selected clay plug was placed in the LSM equipment to start the
test. An expansion indicator connected to a high-precision linear vari­
able differential transformer was contacted with the Teflon piece on top
of the sample. 250 mL of tested drilling fluid was then poured into the
device to completely cover the clay plug, maintaining the immersion for
1440 min. A computer connected to the equipment automatically
recorded the vertical swelling of the sample with time.
R.R. Silva et al. Journal of Petroleum Science and Engineering 213 (2022) 110327

3. Results and discussion

3.1. X-ray fluorescence

Table 2 presents the XRF results for the shale sample.

Based on the chemical analysis presented in Table 2, it can be
inferred that SiO2 is seen in a more significant proportion in the shale
sample (49.82%), indicating the possible presence of quartz. Moreover,
the high amounts of Al2O3 (18.03%) and CaO (12.65%) indicate the
possible presence of smectitic clay minerals and calcite, respectively.
Minerals with appreciable SiO2 and Al2O3 contents above 46% are
classified as aluminosilicates (Rodrigues et al., 2004). It is also observed
that considerable MgO contents indicate the presence of the clay mineral
smectite. For Motta et al. (2008), silica or silicon oxide (SiO2) is related
to clay minerals feldspar and quartz. Therefore, a sample with high
contents of SiO2 and Al2O3 and appreciable contents of MgO and CaO
probably indicates the presence of clay mineral smectite.
The low content of alkaline oxides and the high concentrations of Fig. 3. Diffraction pattern of the Rio do Peixe basin shale.
aluminum and silicon oxides existing in some samples can be attributed
to kaolinite’s presence, which naturally has a low percentage of alkaline (CaCO3, PDF#83–0577), anorthite (CaAl2Si2O8, PDF#70–0287), and
oxides. The concentrations of MgO, Na2O, K2O found in the shale sample albite (Na(AlSi3O8), PDF#72–1245), consistent with the oxides of
were 3.09%, 2.57%, and 3.41%, respectively. The analyzed sample also aluminum, calcium, silicon and sodium present in the chemical
presented iron oxide, Fe2O3, in its composition, 8.55%. composition of the sample.
The shale sample from the Rio do Peixe Sedimentary Basin, due to As the XRD equipment generates the angle data in 2θ, for the
the presence of calcium and magnesium (alkaline earth oxides), may application of Bragg’s Law, all selected angles were divided by 2, and
present polycationic behavior, in addition to indicating the possible Table 3 presents the calculated values according to Bragg’s Law, for each
existence of carbonates in the sample (Lucena et al., 2013). Further­ characteristic interplanar distance, adopting λ = 1.5406 Å (character­
more, the presence of K2O (3.41%) and Na2O (2.57%) in the sample is istic of copper).
another indication that the sample presents polycationic behavior, and
Lucena et al. (2013) reports that this character may be associated with
the presence of these alkaline oxides. 3.3. Thermogravimetric analysis and differential thermal analysis

To perform the thermogravimetric analysis and differential thermal

3.2. X-ray diffraction analysis tests, the simultaneous equipment (TGA/DTA) SHIMADZU
Model DTG-60H was used, conditioning the shale sample in a dynamic
Clay minerals were identified using the Jade 5.0 software with an nitrogen atmosphere, with a heating rate of 10 ◦ C/min and flow of 50
ICDD database, and the basal interplanar distance for each identified mL/min in an alumina crucible, obeying the temperature range varying
peak was calculated according to Bragg’s Law (Equation (6)). Fig. 3 from 28 ◦ C to 1000 ◦ C. Fig. 4 presents the TGA and DTG for the Rio do
shows the diffraction pattern of the shale sample. Peixe basin shale, and Fig. 5 the DTA curve.
nλ = 2dsinθ, (6) It is possible to observe, through Fig. 4, that for the shale of the Rio
do Peixe basin, its total mass loss was 14.89%, and it occurred in 3
where: λ is the wavelength of the incident radiation, (Å); n, the order of thermal decomposition events. The first weight-loss event occurred in
diffraction; d, the distance between the atomic planes, (Å); and θ, the the range of 36.16 ◦ C–108.88 ◦ C, corresponding to a loss of 2.60%
angle of incidence, (◦ ). associated with free water present in the sample, represented by the
From Fig. 3, the shale diffractogram of the Rio do Peixe basin pre­ endothermic inflection in the DTA curve of the shale, observed in Fig. 5,
sents the highest intensity peak corresponding to quartz (SiO2, in the same temperature range.
PDF#85–0798), being the majority mineralogical phase of the sample,
which is in accordance with the high percentage of silica observed in the Table 3
XRF analysis. The accessory clay minerals of the sample correspond to Interplanar basal distances for the Rio do Peixe basin shale sample.
the other peaks of lower intensity, being observed the presence of calcite Peaks Observed angle Calculated angle Basal interplanar distance
(2θ) (θ) (Å)
Table 2 T 15.89 7.94 5.57
XRF result of Rio do Peixe basin shale. Q 20.85 10.42 4.25
B 22.05 11.02 4.02
Elements Shale sample (%)
T 25.93 12.96 3.43
CaO 12.65 Q 26.63 13.31 3.34
SiO2 49.82 B 27.96 13.98 3.18
SO3 0.15 C 29.40 14.70 3.03
Al2O3 18.03 B 30.50 15.25 2.92
Fe2O3 8.55 T 33.30 16.65 2.68
MgO 3.09 T 35.40 17.70 2.53
K2O 3.41 Q 36.54 18.27 2.45
TiO2 1.00 Q 39.46 19.73 2.28
MnO 0.16 C 43.16 21.58 2.09
SrO – C 47.52 23.76 1.91
Na2O 2.57 C 48.51 24.25 1.87
P2O5 0.43 B 50.09 25.04 1.81
Others 0.14 C 57.40 28.70 1.60

6
R.R. Silva et al.
Fig. 4. TGA and DTG for the shale sample obtained under N2 atmosphere and
rate of 10 ◦ C.min− 1.
Fig. 5. DTA curve for shale sample from Rio do Peixe basin obtained under N2
atmosphere and rate of 10 ◦ C.min− 1.
The second weight-loss event occurred in the range of
342.50 ◦ C–554.59 ◦ C, which corresponds to a loss of 2.08%, associated
with the combustion of organic matter, represented by the exothermic
band in the DTA curve (Fig. 5). In addition, the slight endothermic in­
flection observed at 519.76 ◦ C may be associated with chemically
combined or coordinated water release by calcium or sodium oxides
present in the sample and related to the presence of iron-rich clays.
The third weight-loss event occurred in the range of
554.59 ◦ C–743.52 ◦ C, which corresponds to the maximum loss of 7.53%
related to the decarbonation reaction of calcite, an accessory clay min­
eral from the Rio do Peixe basin shale, releasing CO2, which is repre­
sented by the endothermic peak in the DTA curve in Fig. 4.
3.4. Microemulsion-based drilling fluids
3.4.1. Ternary phase diagram
Fig. 6 presents the ternary diagram obtained using both nonionic
surfactants Ultranex NP100 and Alkest Tween 80. Through visual in­
spection of the points for constructing the diagram in Fig. 5, different
results were obtained in color, texture, and transparency, thus, showing
the phase separation (Winsor I, II, and IV). Above the curves is the
microemulsion region, from which the point indicated for the formula­
tion of the microemulsions that served as the continuous phase for the
7
Journal of Petroleum Science and Engineering 213 (2022) 110327
Fig. 6. Ternary phase diagram.
drilling fluids was chosen. This point comprises 45% surfactant, 50%
glycerol/water (G/W 1:1) solution, and 5% pine oil. This point was
selected to reduce the cost of the drilling fluid by reducing the pro­
portions of the oil phase and surfactant, hence, increasing the proportion
of the aqueous phase.
The difference in the hydrophilic-lipophilic balance (HLB) of the
surfactants Ultranex NP100 and Alkest Tween 80 may explain the dif­
ference observed in the microemulsion regions (Winsor IV) in the phase
diagram since both surfactants present a nonionic character. This semi-
empirical scale, developed by Griffin (1949), uses the relative percent­
age of hydrophilic to lipophilic (hydrophobic) groups in the surfactant
molecule(s) as its base. Concerning an oil-in-water microemulsion, the
hydrophobic tail is directed towards the oil phase, while the hydrophilic
head group resides in the aqueous phase (Tadros, 2014). The HLB values
for both surfactants used in the formulation of the microemulsions may
favor the stabilization of oil-in-water mixtures. Due to short-range
repulsive forces, the nonionic surfactants provide stability to the
microemulsion, which prevents droplets aggregations (Silva et al., 2015;
Raman and Aichele, 2020).
The hydrophobic portion of the nonionic surfactant Ultranex NP100
comes from nonylphenol, while the hydrophilic portion from the
ethylene oxide chain. The degree of ethoxylation of this surfactant af­
fects the HLB value, which is 13.3. On the other hand, the nonionic
surfactant Alkest Tween 80 presents a slightly higher HLB value of 15.0.
This surface-active agent is hydrophilic in nature and soluble in water,
thus lowering the interfacial tension between the continuous and
dispersed phases of the microemulsion (Foo et al., 2020). The micro­
emulsions presented a homogeneous appearance for both mixtures,
which indicated a single phase.
3.4.2. Rheological study
The fine particles of drilled formations and rheology control addi­
tives may directly or indirectly control the drilling fluid rheological
properties (Saasen and Løklingholm, 2002; Gamal et al., 2019). Sur­
factants have also been used to control these properties added in
water-based muds, invert emulsion drilling fluids, and oil-based muds.
These properties, among other factors, present high significance for a
successful drilling operation. They ensure that the drilling fluid suspends
and carries away the drill cuttings, clean the downhole and the borehole,
and drill safely and quickly (Luo et al., 2017; Xu et al., 2018). The effect
of the microemulsions and the potassium salt adding on the rheological
behavior of the formulated drilling muds were investigated using
viscometer Fann 35 A in 6-speed readings.
Fluid flow curves for the microemulsion-based drilling fluids
formulated with both surfactants Ultranex NP100 and Alkest Tween 80
are depicted in Fig. 7. Table 4 presents the yield stress results, τy (lb/100
ft2), obtained according to the API Recommended Practice 13D, along
with the coefficient of determination, R2. Flow behavior index, n
R.R. Silva et al. Journal of Petroleum Science and Engineering 213 (2022) 110327

Fig. 7. Flow curves for drilling muds formulated with surfactant: (a)Ultranex NP100; (b) Alkest Tween 80.

rheological behavior following the Herschel-Bulkley model since n

Table 4
varied between 0 and 1. The Herschel-Bulkley model includes the two-
Rheological parameters for microemulsion-based drilling fluids.
parameter models of Bingham Plastic (BP) and Power Law (PL) as
Mud sample τy (lb/100 ft2) R2 n (dimensionless) k (cP) particular cases (Guo and Liu, 2011). When n is equal to one, the drilling
NP100_INIB1 0.7 0.9984 0.72 0.70 fluid can be defined as BP, and it becomes PL when τy is equal to zero. It
NP100_INIB2 0.8 0.9915 0.65 1.34 is worth noting that K is directly proportional to the fluid’s effective
NP100_INIB3 1.4 0.9992 0.91 0.26 viscosity (μ0). Therefore, drill cuttings will travel less in low-K fluids
NP100_SI 1.0 0.994 0.85 0.41
T80_INIB1 3.0 0.9929 0.57 1.05
with low effective viscosity, as cuttings tend to settle faster at the bottom
T80_INIB2 1.2 0.9856 0.66 1.16 of the annular space due to gravity. Whereas in high-K fluids, having
T80_INIB3 0.2 0.9756 0.81 0.32 high effective viscosity, cuttings will be suspended for a more extended
T80_SI 0.9 0.9975 0.89 0.22 period, presenting a superior transport velocity (Caenn et al., 2017).
Currently, the Herschel-Bulkley model, also known as the modified
(dimensionless) and consistency index, K (cP), likewise obtained ac­ Power Law, is considered more accurate in predicting the behavior of
cording to the API Recommended Practice 13D, are presented in Table 3. the vast majority of drilling fluids compared to the two-parameter
Fig. 7a shows an increase in shear stress at a higher shear rate for models that are widely accepted in the oil industry (Muherei, 2016;
drilling fluids NP100_INIB3 and NP100_SI, where the first presented Hemphill et al., 1993; Zamora and Power, 2002).
shear stress of 147.9 Pa compared to 145.35 Pa of the latter. This fact The eight formulated drilling fluids have, in general, similar flow
may be due to the particle size of the KCl, as it directly influences the behavior. The drilling mud T80_INIB1 presented the highest result for τy
rheological behavior of drilling fluids, also observed in the viscosity (3.0 lb/100 ft2), which may influence the cutting removal efficiency of
curve depicted in Fig. 8a. However, it can be seen that all drilling muds the drilling fluid. The consistency index varied from 0.22 to 1.34 cP
presented a similar flow behavior. As for the drilling fluids formulated (drilling muds T80_SI and NP100_INIB2, respectively).
with the surfactant Alkest Tween 80 (Fig. 7b), the swelling inhibitor The drilling fluid viscosity significantly impacts its performance
INIB2 showed a greater influence, presenting a more significant change. during the drilling process. It must be high enough under low shear
The behavior of the fluid formulated with the inhibitor INIB1 showed conditions in order to suspend and carry cuttings from beneath the drill
the slightest change in shear stress with an increase in the shear rate for bit to the surface, and under high shear rates, it should be low enough for
both surfactants (119.85 Pa and 66.3 Pa for surfactants Ultranex NP100 adequate flow (Arabloo et al., 2013). Drilling fluids are usually designed
and Alkest Tween 80, respectively). to suspend barite and drill cuttings under static conditions. For this to be
Table 4 shows that all formulated fluids presented non-Newtonian possible, drilling fluids must exhibit yield-stress behavior or a very high

Fig. 8. Plot of viscosity vs. shear rate for drilling fluids with (a) Ultranex NP100; (b) Alkest Tween 80.

8
R.R. Silva et al.
zero-shear-rate viscosity (Power and Zamora, 2003; Saasen, 2014). One
of the reasons for the importance of accurate modeling of drilling fluid
rheology lies in the pump pressure needed to resume circulation after a
static period and how the fluid rheology evolves with time while in static
or near-static conditions Skadsem et al. (2019).
From Fig. 8a, for the drilling fluids formulated with the nonionic
surfactant Ultranex NP100, the INIB2 presented a higher viscosity value
at a low shear rate and a higher shear rate; the samples presented a
similar behavior. As for the drilling fluids formulated with Alkest Tween
80 (Fig. 8b), it may be seen that the INIB1 influenced the most, pre­
senting both a higher viscosity at a lower shear rate and a lower viscosity
at a higher shear rate.
Table 5 presents the results of plastic viscosity, PV (cP), apparent
viscosity, AV (cP), yield point, YP (lb/100 ft2).
Based on the results presented, it is possible to observe that the
presence of the solid additive to inhibit clay swelling and the type of
nonionic surfactant present in the microemulsion influenced the rheo­
logical properties of the formulated fluids. Plastic viscosity is defined as
the flow resistance above the yield point in plastic material. Its strength
is affected by the concentration and size of solids and the continuous
phase viscosity (Caenn et al., 2017; Razi et al., 2013). This property
plays an essential role in the cuttings carrying capacity of drilling fluids
(Murtaza et al., 2020). Ultranex NP100 surfactant provided an increase
in this property, especially in the fluid formulated with potassium
chloride, KCl (INIB3). It may directly affect the equivalent circulating
density, ECD, as it increases proportionally with this property (Irawan
et al., 2017; Al-Hameedi et al., 2019). Drilling fluids formulated with the
nonionic surfactant Alkest Tween 80 had lower PV results. The drilling
fluid with the swelling inhibitor potassium citrate (INIB1) showed the
lowest result (52.5 cP). This fact may be associated with a better inter­
action of this additive with the continuous phase of the drilling fluid.
Apparent viscosity (AV) was also maximized in the drilling fluids
using Ultranex NP100. The fluid NP100_INIB3 showed the highest value
of AV, 145 cP, whereas the fluid T80_INIB1 presented 65 cP. The yield
point, YP, directly influences the transport of drilled cutting from the
bottom hole to the surface. A higher value of YP suggests a better ca­
pacity for transporting cuttings when compared to low-YP fluids.
However, an increase in costs of the drilling operations due to high
pump power may occur when YP is too high. From Table 4, both drilling
fluids added with potassium sulfate showed a higher value of YP, 50 lb/
100 ft2, while a lower result was found in NP100_INIB3, 16 lb/100 ft2.
3.4.3. Filtration and filtercake properties
Filtrate loss and filtercake thickness are essential parameters to
evaluate a drilling mud formulation (Murtaza et al., 2020). The filtrate
invasion into permeable zones of formations can cause, among other
problems, the swelling of hydratable rocks (Van Oort, 2003; Gholami
et al., 2021). The invasion into the reservoir will increase water satu­
ration in zones near the wellbore, thus decreasing oil saturation in this
zone. Consequently, the effective permeability of the formation will
decrease (Windarto et al., 2011). As a result, the resistance to oil flow
into the wellbore will increase. Therefore, a minor filtrate loss implies
more excellent stability of the drilled wellbore and less degradation of
Table 5
Rheological parameters (PV, AV, and YP) of the microemulsion-based drilling
fluids.
Mud sample PV (cP) AV (cP) YP (lb/100 ft2)
NP100_INIB1 107.5 117.5 20
NP100_INIB2 110 135 50
NP100_INIB3 137 145 16
NP100_SI 122.5 142.5 40
T80_INIB1 52.5 65 25
T80_INIB2 95 120 50
T80_INIB3 60 80 40
T80_SI 92.5 102.5 20
9
Journal of Petroleum Science and Engineering 213 (2022) 110327
the drilling fluid by the formation mud. Fig. 9a and b shows the effects of
the swelling inhibitors and the microemulsions on filtrate loss.
It is observed that the drilling fluids prepared without swelling in­
hibitors, NP100_SI and T80_SI, had lower filtrate loss values, 3.4 and 0.6,
respectively. This shows that microemulsions alone can significantly
decrease the invasion of filtrate into permeable formations. The drilling
fluid prepared with the surfactant Alkest Tween 80 showed the lowest
result of filtrate loss, which could be explained by the higher viscosity
presented by this surfactant, which influences the pore plugging effect.
The other microemulsion-based drilling fluids added with potassium
salts, despite showing slightly higher results than those mentioned
above, still gave low values of filtrate loss, all being within the specifi­
cations established by API-Standard 13B-1.
Fig. 10 shows the filtercake thickness measured after the filtration
experiments, following the arrangement in Fig. 2. Both drilling fluids
formulated with INIB2 showed the lowest filtercake thickness, 0.61 and
0.51 mm, for microemulsions with Ultranex NP100 and Alkest Tween
80, respectively. A thin filtercake is desirable while drilling since it may
directly affect tripping operation in the wellbore. Swelling inhibitor
INIB3 showed the highest results among all drilling fluids tested but still
considered low compared to other filtercake thicknesses found in the
literature. Junior et al. (2021) evaluated the effect of NP100 on the
filtercake thickness and found similar results, ranging from 0.64 to 1.24
mm. Higher HLB values for surfactants are associated with smaller fluid
loss and thinner mudcakes (Numkam and Akbari, 2019). The difference
among the results both with Ultranex NP100 and Alkest Tween 80,
associated or not with the swelling inhibitors, may be directly related to
the dispersed phase volume fraction of the drilling fluids.
Table 6 shows the results of filtercake permeability at 30 ◦ C and
55 C. All filtercakes showed low permeability, which is desired in the
◦
field, allowing for less infiltration of the filtrate. The filtercakes formed
by drilling fluids with Alkest Tween 80 surfactant showed lower
permeability, ranging from 0.0004 to 0.0033 mD at 30 ◦ C and 0.0003 to
0.0019 at 55 ◦ C. However, an unexpected behavior was observed in the
T80_INIB3 fluid, where at 55 ◦ C, the filtercake permeability was higher
than at 30 ◦ C. The synergy of the KCl inhibitor and the surfactant Alkest
Tween 80 must be taken into account, in which at high temperature the
properties may behave differently. As Caenn et al. (2017) reported, the
filtercake permeability may increase with a decrease in the width of the
particles’ size range. The authors have also pointed out a series of ex­
periments carried out throughout the years, showing that the filtercake
permeability usually lies on the order of 10− 3 mD, being the results
found in this work compatible with what is mentioned.
3.5. Linear swelling
Linear swelling tests of bentonite clay samples in contact with dril­
ling fluids were carried out to analyze the swelling inhibiting properties
of microemulsion-based drilling fluids with added potassium salts and a
blank sample. In addition to the eight drilling muds mentioned, the clay
plugs were also subjected to tests with distilled water. In general, most
swell versus time graphs show different behavior compared to each
other. The time required for the systems to reach equilibrium may be
directly linked to the chemical nature of each inhibitor, as well as the
size of the surfactant’s hydrophobic chain.
Fig. 11 shows the linear swelling results for microemulsion-based
drilling fluids formulated with Ultranex NP100 and the swelling curve
of the bentonite clay sample with distilled water.
Initial results indicated that the clay plug immersed in distilled water
had the most substantial linear swelling influence, reaching a volume
variation of 108% after test time. The clay sample undergoes rapid
growth, noted at 50 min after the start of the test. This rapid growth is
due to the absorption of polar ions from water in the basal spacing of the
sample, thus causing rapid osmotic swelling. The growth continued until
reaching an equilibrium 900 min after the start of the test when it
reached a plateau.
R.R. Silva et al. Journal of Petroleum Science and Engineering 213 (2022) 110327

Fig. 9. Filtrate loss of microemulsion-based drilling fluids formulated with (a) Ultranex NP100; (b) Alkest Tween 80.

Fig. 10. Filtercake thickness of microemulsion-based drilling fluids formulated with (a) Ultranex NP100, (b) Alkest Tween 80.

Table 6
Filtercake permeabilities at 30 ◦ C and 55 ◦ C.
MEDF sample NP100_INIB1 NP100_INIB2 NP100_INIB3 NP100_SI T80_INIB1 T80_INIB2 T80_INIB3 T80_SI

k 30 ◦ Ca 0.0023 0.0220 0.0950 0.0077 0.0033 0.0004 0.0004 0.0013

k 55 ◦ Ca 0.0004 0.0020 0.0137 0.0028 0.0005 0.0003 0.0019 0.0006
a
Unit: mD.

The clay sample’s linear swelling, which was put into contact with
the drilling fluid NP100_INIB2, presented the lowest result, reaching a
swelling variation of 6.9%. It can be said that the swelling inhibitor
potassium sulfate showed better synergy with the microemulsion, thus
presenting a greater inhibition capacity. Besides the performance of the
inhibitor per se, the hydrophobic chain of the nonionic surfactant also
acts on competing with the water’s oxygen atoms. The fluids formulated
with the inhibitors INIB3 and INIB1 and the drilling fluid without the
swelling inhibitor, NP100_SI, showed 8.5%, 11.3%, and 22.8%. It is
observed that, even without presenting swelling inhibitors,
microemulsion-based drilling fluids achieved results considered satis­
factory when compared to water-based drilling fluids and other fluids
with the addition of surfactants. However, the swelling curve of drilling
fluid without inhibitor shows an increasing behavior, not reaching ionic
balance at the end of the test.
The Ultranex NP100 surfactant has, in its hydrophilic part, molecules
from ethylene oxide and, as well as other simple additives such as
ethylene glycol and polyethylene, show a tendency to destabilize ionic
reactions within clay structures (Quintero, 2002). According to Aston
and Elliott (1994), one aspect of the behavior of nonionic surfactants is

10
R.R. Silva et al.
Fig. 11. Swelling (%) as a function of time for a bentonite clay sample
immersed in microemulsion-based drilling fluid systems with Ultranex
NP100 surfactant.
that they interfere with the hydrogen bond between water and shale
surfaces. Shale swelling involves forming hydrogen (H–O) bonds be­
tween water and silica or aluminum groups on the surface of the shale.
Since the glycol group also forms this type of bond, there is competition
with water molecules, thus interrupting the hydrogen-bonded networks.
Ultranex NP100 also competed with the water of hydration around
the adsorbed cations in the samples. This fact also favored changing the
strength of hydrogen bonds. It is also noted, by the results obtained for
the fluids with that surfactant, that there was a good synergy of the
surfactant molecules used with the potassium salts, especially with the
potassium sulfate (INIB2) showed a lower result. This caused a hard­
ening of the structures, preventing or retracting water uptake in the
bentonite clay interlayers.
Fig. 12 presents the linear swelling results for drilling fluids formu­
lated with the nonionic surfactant Alkest Tween 80. The swelling curve
of the clay sample with distilled water was also added to this figure for
comparison.
Among the results, the microemulsion-based drilling fluid added
with INIB1 (potassium citrate) presented the lowest clay expansion
value, 15.6%. This result may be associated with a better chemical
interaction between the ethoxylated sorbitan esters present in the hy­
drophobic chain of the surfactant Alkest Tween 80 with potassium cit­
rate. The interaction between the exchangeable ions of the clay surfaces
and the portion of the adsorbed molecules of the surfactant favor this
inhibition reaction. However, comparing the result of INIB1 with that of
Fig. 12. Swelling (%) as a function of time for a bentonite clay sample
immersed in microemulsion-based drilling fluid systems with Alkest Tween
80 surfactant.
11
Journal of Petroleum Science and Engineering 213 (2022) 110327
the previous system, this one presented a slightly higher result. Drilling
fluids with INIB3 (KCl), INIB2 (K2SO4), and the fluid without inhibitor
(T80_SI) showed results of 16.3%, 20.3%, and 40.6%, respectively. All
results were also slightly higher than those with Ultranex NP100.
The K+ cation present in the swelling inhibitors was responsible for
inducing a solid osmotic consolidation in the post-swelling region in the
studied drilling fluids, that is, when the cation exchange between fluids
and clay particles found equilibrium. These ions’ low degree of hydra­
tion in a polar medium shows the effectiveness of reducing swelling
pressures in clayey formations. This fact results in a low ionic repulsion,
which is responsible for lowering the hydration influence of these ions
between the basal spacing (Christenson et al., 1987; Israelachvili and
Wennerstroem, 1992; Van Oort, 1997; Andagoya Carrillo et al., 2015).
Furthermore, nonionic surfactants are adsorbed on clay surfaces due
to the hydrophilic group of molecules, which interact with the nega­
tively charged surface of clay layers. (Cui and van Duijneveldt, 2010).
The surfactant Ultranex NP100, due to its longer hydrophobic chain
(resulting from the reaction of nonylphenol with ethylene oxides),
showed better results than Alkest Tween 80, which hydrophobic portion
comes from the reaction of polyethoxylated esters of 3,6-sorbitan. The
interaction between the surfactant molecule and the negatively charged
clay layer, as well as the cationic substitution in the interlayers of the
clay structure, are schematically represented in Fig. 13.
3.6. Hot roll/dispersion test
The hot roll/dispersion test was carried out in order to verify the
interaction of the shale sample with the drilling fluids and the capacity
of the microemulsified systems to maintain the sample with integrity
after the test. Reactive shales can be problematic during drilling oper­
ations due, among other factors, to their tendency to disperse when
exposed to aqueous media such as aqueous-based drilling fluids.
Dispersion involves the degradation of shale rock when exposed to water
and is caused by stresses in the well, the extent to which the rock is
hydrated, the drilling fluid velocity in the annular space, and the degree
of the brittleness of the shale (Al-Arfaj et al., 2018).
Shales’ degradation may also directly affect the equivalent circu­
lating density, ECD, which, in general, is influenced by the total amount
of solids in the system. Therefore, maintaining a proper density is
essential when a wellbore is being drilled and presents a tight tolerance
between the weight of drilling fluid needed to control the formation
pressure and the weight that will cause formation fracture. In such cir­
cumstances, minimizing the degradation of these formations generally
provides improved control of drilling fluid density (Janjua et al., 2011,
Andagoya Carrillo et al., 2015).
Regarding the tests performed with the drilling fluids formulated
with the surfactant Ultranex NP100, the fluid NP100_INIB1 showed the
lowest results, 0.215% of shale dispersion (Fig. 14). These results show
Fig. 13. Schematic representation of the surfactant inhibition mechanism and
potassium cation substitution.
R.R. Silva et al.
Fig. 14. Results of hot roll dispersibility tests for Ultranex NP100 dril­
ling fluids.
the efficiency of this drilling mud in maintaining the integrity of the
analyzed shale sample. In addition, the hydrophobic part of the Ultranex
NP100 surfactant contributed to the formation of bonding bridges be­
tween the platelets in the samples’ interlayers, providing more excellent
stability. The drilling fluid NP100_INIB2 also showed a low degree of
dispersibility in the shale sample, being 3.95%. The fluids NP100_INIB3
and NP100_SI, with chloride potassium and without inhibitor, respec­
tively, presented 4.85% and 5.15% dispersibility.
Fig. 15. XRD characterization of samples before and after the dispersibility test with Ultranex NP100 fluids. (a) NP100_INIB1; (b)NP100_INIB2; (c) NP100_INIB3;
(d) NP100_SI.
12
Journal of Petroleum Science and Engineering 213 (2022) 110327
It can be said that even without the presence of swelling inhibitors,
the microemulsion-based drilling fluid is able to maintain the integrity
of the shale sample. This fact may be associated with the hydrophobic
part of the surfactant, which, as shown in the previous test, is capable of
repelling the absorption of molecules from the aqueous phase. Fig. 15a,
b, c, and d show the diffraction patterns of the shale sample after the
dispersibility test using microemulsion-based drilling fluids with the
surfactant Ultranex NP100. As can be seen, little or practically no change
is observed in the peaks, followed by the θ differences on the x-axis of
each graph, showing that the basal spacing, d, of the samples were kept
practically unchanged.
A change in the behavior comparing the starting and ending pattern
is also noticed at the beginning of each chart. This change in the crys­
tallinity of the sample may be associated with a slight change in the
behavior from amorphous to crystalline due to potassium salts, which
promoted greater ease of reorganization in the samples’ crystalline re­
ticulum. The same pattern is not observed in the sample tested with
drilling fluid without the potassium salt.
Drilling fluids formulated with the nonionic surfactant Alkest Tween
80, system 2, showed good dispersibility results but a little higher when
compared to the previous muds. As with the first system, the fluid
formulated with the inhibitor INIB1 presented a lower result, desired as
this test’s outcome (1.25%). The exchangeable cations present on the
surface of the formation samples interacted well with the inhibitor and
the hydrophilic part of the surfactant molecule, with a low interaction
with the free water of the system.
The dispersion tests with drilling fluid T80_INIB2 showed values
similar to those of fluid T80_INIB1. The result was 1.25% for the shale
sample, similar to that observed for T80_INIB1. This may suggest that
both inhibitors have similar inhibition mechanisms. The T80_INIB3 and
T80_SI fluids showed dispersibility values, respectively, 2.5% and 3.15%
for the used shale sample. The results are shown in Fig. 16.
Fig. 17 shows the results of XRD characterization of the shale sample
R.R. Silva et al.
Fig. 16. Results of hot roll dispersibility tests for Alkest Tween 80 dril­
ling fluids.
using the fluids T80_INIB1, T80_INIB2, T80_INIB3, and T80_SI.
As in the previous results, there is little difference between the initial
and final basal spacing, which indicates that the shale samples were kept
intact. It may imply that the formulated drilling muds provide a better
cleaning capacity of the wellbore.
It is noteworthy that even without the presence of a swelling
Fig. 17. XRD characterization of samples before and after the dispersibility test with Alkest Tween 80 fluids. (a) T80_INIB1; (b) T80_INIB2; (c) T80_INIB3; (d) T80_SI.
13
Journal of Petroleum Science and Engineering 213 (2022) 110327
inhibitor, microemulsion-based drilling fluids presented low dis­
persibility values, both with the surfactant Ultranex NP100 and with
Alkest Tween 80. The fluids can maintain the integrity of the cuttings of
shale, showing little cation exchange with ions from the sample surfaces.
When compared to results from water-based drilling fluids,
microemulsion-based drilling fluids can maintain the integrity of sam­
ples more efficiently (Al-Awad and Smart, 1996; Lucena et al., 2013;
Al-Arfaj et al., 2018).
4. Conclusions
This study investigated a novel drilling mud approach using a
microemulsion as the drilling fluid’s continuous phase, and the inter­
action with a shale sample was assessed. Two nonionic surfactants were
used in different formulations of microemulsion-based drilling fluids
associated with potassium salts to investigate the inhibition of shale
swelling. A shale sample was characterized regarding its chemical and
mineralogical composition, as well as its thermal behavior. The shale
inhibition performance of the microemulsion-based drilling fluids was
investigated through the linear swelling test and hot roll dispersibility
test. The rheological and filtration performances of the drilling fluids
were also investigated through API-Recommended Practice tests. The
following observations and conclusions may be drawn.
• The studied shale sample presented a considerable proportion of
aluminosilicates, presenting a higher reactivity with the aqueous
medium.
• All formulated drilling fluids followed the Herchel-Buckley rheo­
logical behavior, having the flow behavior index varying from 0.65
to 0.91. Thus, both nonionic surfactants did not seem to influence
R.R. Silva et al.
much the rheological behavior of the drilling muds since all fluids
showed similar results concerning the rheological parameters.
• The plastic and apparent viscosities were higher in the drilling fluid
with the Ultranex NP100 as the surfactant and the chloride potas­
sium (INIB3) in its formulation (137 cP and 145 cP, respectively).
However, the same drilling fluid presented the lowest yield point (16
lb/100 ft2).
• The linear swelling (%) of drilling fluid NP100_INIB2 was 6.9%,
which was the lowest result found. The other drilling muds with
citrate potassium, chloride potassium, and without inhibitor also
showed good inhibition results, both with the Ultranex NP100 and
Alkest Tween 80.
• The drilling fluids formulated with both the Ultranex NP100 and
Alkest Tween 80 presented low results of dispersibility on the shale
sample, being the fluid NP100_INIB1 the lowest (0.215%).
• The shale sample did not show significant expansion after the dis­
persibility test, showed through the DRX analysis, which represents
an essential factor during drilling operations since the shale cuttings
may degrade and make the equivalent density, ECD, higher.
Credit author statement
Raphael R. Silva: Conceptualization, Methodology, Validation,
Investigation, Data curation, Writing – original draft, Writing – review &
editing. Fabiola D. S. Curbelo: Conceptualization, Methodology,
Writing – review & editing, Supervision, Project administration, Fund­
ing acquisition. Alfredo I. C. Garnica: Conceptualization, Methodology,
Supervision, Project administration, Funding acquisition. Giovanna L.
R. Leal: Validation, Investigation, Data curation. Luara R. Viana:
Validation, Investigation, Data curation. Júlio C. O. Freitas: Resources,
Supervision. Alex N. Barros: Methodology, Investigation, Data cura­
tion. Thales L. S. Silva: Investigation. João Adauto de S. Neto: Re­
sources, Supervision.
Declaration of competing interest
The authors declare that they have no known competing financial
interests or personal relationships that could have appeared to influence
the work reported in this paper.
Acknowledgments
The authors thank CNPq and PIBIC/CNPq/UFPB for the scholarship
granted, Postgraduate Program of Chemical Engineering, Federal Uni­
versity of Paraiba (UFPB), Postgraduate Program in Geoscience, Federal
University of Pernambuco (UFPE), and Baker Hughes, Brazil.
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