j o u r n a l o f m a t e r i a l s r e s e a r c h a n d t e c h n o l o g y 2 0 2 3 ; 2 4 : 4 1 4 3 e4 1 5 2

Available online at www.sciencedirect.com

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

Original Article

Synthesis and characterization of silica-based

nanofluids for enhanced oil recovery

Mariana Schneider a, Karina Cesca a, Su
elen Maria de Amorim b,

n c, Regina F.P.M. Moreira a,*
Dachamir Hotza a, Enrique Rodrı́guez-Castello
a
Department of Chemical Engineering and Food Engineering, Federal University of Santa Catarina, 88040-900

polis, SC, Brazil
Floriano
b

,
Faculty of Mining and Environmental Engineering e Federal University of the South and Southeast of Para
Maraba
, PA, Brazil
c

laga, Spain
Department of Inorganic Chemistry, Faculty of Sciences, University of Ma

article info abstract

Article history: The use of nanofluids in enhanced oil recovery processes has gained attention due to the
Received 25 August 2022 possibility to intensify oil recovery from mature oil fields. When nanofluids are injected
Accepted 6 April 2023 into oil wells, different mechanisms are involved such as wettability alteration, reduction
Available online 12 April 2023 of interfacial surface tension, increase in the viscosity of the aqueous solution, and
decrease in oil viscosity. Silica nanoparticles are extensively used for nanofluid formula-
Keywords: tions but there are important obstacles to the use of nanofluids in enhanced oil recovery.
Nanoparticles Stability is the most evident, in addition to environmental and economic aspects, and the
Silica need to design suitable large-scale production processes for nanoparticle synthesis with
Smart nanofluids the required characteristics. Thus, the present study aims to evaluate oil recovery using
Rice husk silica-based nanofluids from various sources (natural rice husk ash, sol-gel synthesis, and
Enhanced oil recovery commercial nanosilica) under different operational conditions. Silica nanoparticles were
characterized by XRF, XRD, TEM, FTIR, specific surface area, and XPS. Nanofluids with
different nanoparticles concentration were characterized by their viscosity, surface ten-
sion, zeta potential, and stability. Oil recovery from an oil-saturated sand-packed bed
increased due to the nanofluid injection after secondary recovery. An additional 5e10% oil
recovery is achieved after flooding due to the injection of nanofluids, proving that silica
from rice husk ash has comparable efficiency to other synthetic silica nanoparticles that
are used in enhanced oil recovery.
© 2023 The Author(s). Published by Elsevier B.V. This is an open access article under the CC
BY-NC-ND license (http://creativecommons.org/licenses/by-nc-nd/4.0/).

the technology of materials at the nanoscale [1]. Because of

1. Introduction this characteristic, nanotechnology has applications in
different knowledge areas, such as engineering, chemistry,
Nanotechnology is the area of science devoted to under- physics, biology, and medicine.
standing the fundamental physics, chemistry, biology, and

* Corresponding author.
E-mail address: regina.moreira@ufsc.br (R.F.P.M. Moreira).
https://doi.org/10.1016/j.jmrt.2023.04.049
2238-7854/© 2023 The Author(s). Published by Elsevier B.V. This is an open access article under the CC BY-NC-ND license (http://
creativecommons.org/licenses/by-nc-nd/4.0/).
4144 j o u r n a l o f m a t e r i a l s r e s e a r c h a n d t e c h n o l o g y 2 0 2 3 ; 2 4 : 4 1 4 3 e4 1 5 2
Nanoparticles can be dispersed in fluid bases (like ethylene
glycol, oil, water, brine, and surfactants) to prepare nanofluids
[2e4]. Depending on the nanoparticle characteristics and the
fluid base, the thermal, optical, electrical, rheological, and
magnetic properties, and the nanofluid stability can be
adjusted for different applications [5e7]. Particularly in the
petroleum industry, nanoparticles have been applied in dril-
ling operations, wastewater treatment, corrosion inhibition,
production development, heat transfer, and enhanced oil re-
covery [8e11].
Oil recovery occurs in three steps: primary, secondary, and
tertiary recovery; the latter is also known as enhanced oil re-
covery (EOR). In primary recovery, the natural energy present
in the reservoir is utilized, although only about 5e10% of the
oil present in the reservoir is recovered. Water and gas are
injected into the reservoir for the secondary recovery, and the
oil recovery is 10e55%. Thus, after the primary and secondary
recovery, a large amount of oil remains in the pores of the
reservoir, due to the high capillary pressure of the water.
Considering the large amount of oil that can still be extracted
from a reservoir, tertiary recovery techniques are applicable.
To increase efficiency, biological, physical, and chemical
methods are applied. In those cases, the ratio of mobility of
the injected fluids is reduced, decreasing the interfacial ten-
sion between the fluid injected and the oil, reducing capillary
forces, and changing the wettability of the reservoir [12,13].
EOR allows an additional 5e15% of the oil from the reservoir to
be recovered [14].
In the chemical method, the association between nano-
particles and surfactants to prepare nanofluids for applica-
tions in EOR has been proposed by several authors in recent
years [4,8,9,11,15e18]. According to Mittal [11], the application
of nanomaterials has the potential to achieve outstanding
results in the oil industry.
Surfactants are applied to reduce the surface tension be-
tween oil and water, facilitating the displacement of oil
throughout the production pool, and can be added to nano-
fluids to improve their characteristics and properties [13].
Although the studies related to the application of nanofluids
in enhanced oil recovery are relatively recent, their utilization
can improve the economy of mature fields, because nano-
fluids can change the wettability of the rock surface, reduce
interfacial tension and the viscosity of the oil phase [6,19].
Numerous studies have reported the use of nanoparticles
of silica (SiO2), titanium dioxide (TiO2), graphene oxide (GO),
and aluminum oxide (Al2O3) to improve the rheological
properties of nanofluids [4]. The preparation method of
nanoparticles can play a key role in controlling their physi-
cochemical properties, such as size, morphology, and point of
zero charge, influencing the stability of nanofluid [18]. Some
examples of widely accepted preparation methods for nano-
particle synthesis are hydrothermal [20], co-precipitation [21],
sol-gel [22], chemical vapor deposition [5], and biosynthesis
[23]. Other less common methods are also applied, such as
milling [15], and the Sto € ber process [24].
Silica nanoparticles are extensively used in enhanced oil
recovery because they can be easily adjusted to have the
desired characteristics [11,25,26]. Nevertheless, the EOR
mechanism of nanoparticles is extremely complex and in-
cludes several aspects such as wettability, injection fluid
viscosity, surface tension alterations, and separation pressure
[27]. Despite extensive investigation on SiO2 nanoparticles for
EOR application, there are still challenges in the field owing to
cost and huge environmental problems [26].
Recently, Agi et al. [15] reported the application of silica
nanoparticles from rice husks for chemically enhanced oil
recovery and concluded that rice husk ash is a promising and
cost-effective source to produce silica nanoparticles. Howev-
er, deeper studies are required to formulate nanofluids to
avoid nanoparticle agglomeration and increase oil recovery by
adjusting operational conditions such as the nanoparticles
concentration and nanofluid composition. Thus, this study
aims to compare the efficiency of silica produced from rice
husk ash and other silica-based nanofluids in the enhanced oil
recovery process and to evaluate the effect of silica nano-
particle characteristics and their concentration in the tertiary
oil recovery.
2. Experimental
2.1. Materials
Sodium dodecyl sulfate (SDS, purity 96.44%, Neon), sodium
silicate ((Na2O)x$(SiO2)y) (3.3:1), 40e50 wt% in water, Quimi-
drol), aqueous ammonia (analytical grade, Biotech), and so-
dium chloride (NaCl, 99% purity, Vetec) were used without
prior treatment or purification. Mineral oil (MO) SAE 90 GL-5
with a density of 0.90 g cm
3 was applied in the flooding
tests since it presents comparable properties with petroleum
from Campos Basin (Brazil) [28]. Moreover, the use of this oil in
laboratory-scale tests has advantages such as easy cleaning
procedures.
Three different silica nanoparticles were used in the
nanofluid formulation. Commercial silica nanoparticles (SC)
with a hydrophobic characteristic were purchased (Sigma-
Aldrich). Two other samples were synthesized in this study,
the first from rice husk (Fumacence Foods, Santa Catarina,
Brazil) and the second using neutral sodium silicate.
2.2. Synthesis of silica nanoparticles from rice husk
The methodology for synthesizing silica from rice husk ash
(RH) was adapted from Agi et al. [15]. To remove organic
matter, the rice husks were calcined at 800  C for 7 h in a
muffle oven (F2-DM, Fornitec). Then, the material was washed
with distilled water, filtered using a vacuum pump (820,
Fisatom), and dried in an oven (DeLeo) at 100  C for 15 h.
Finally, to obtain the particles on a nanometric scale, two
consecutive milling steps were applied. The first milling step
was conducted in a ball mill (CT 242, Servitech), for 4 h. Then,
the material was milled in a micro-processed digital jar mill
(CE-500/D, Cienlab), with a controlled velocity of 300 rpm for
5 h. Finally, the material was dried in an oven at 80  C for 24 h.
2.3. Synthesis of silica nanoparticles by sol-gel
The procedure for obtaining silica nanoparticles using the sol-
gel method was based on Maaref et al. [2], Zulfiqar et al. [25],
and Chaturvedi and Sharma [29]. First, 100 mL of sodium
 j o u r n a l o f m a t e r i a l s r e s e a r c h a n d t e c h n o l o g y 2 0 2 3 ; 2 4 : 4 1 4 3 e4 1 5 2 4145

silicate were added to a beaker and kept in an ultrasonic bath synthesized by the sol-gel method (SS) were used in a similar
(USC-1650A, Unique) for 15 min. Then, 60 mL of aqueous formulation, as displayed in Table 1. For the enhanced oil re-
ammonia were added dropwise and kept in an ultrasound covery tests, 14 different formulations were used: brine (B),
bath for 1 h, followed by a standing time of 20 min. Then, brine with surfactant (BS), and 12 nanofluids (NF) prepared
200 mL of distilled water were added, and the solution was left with brine, surfactant, and different concentrations of nano-
to stand for 1 h. The precipitated solid was filtered and particles (Table 1).
exhaustively washed with ethanol and distilled water to Brine was prepared by adding NaCl to distilled water; then,
remove the ammonia residues to obtain silica by the sol-gel the solution was kept under magnetic stirring for 10 min. For
method (SS silica). Finally, the silica produced was dried in the BS solution containing surfactant, SDS was initially added
an oven at 250  C for 30 h. to distilled water and the solution was kept under magnetic
stirring for 30 min. Then, NaCl was added, and the solution
2.4. Characterization of nanoparticles was kept under stirring for another 10 min. The same pro-
cedure used for preparing BS was made for the nanofluids.
The synthesized, precipitated, and commercial silica were However, after the second agitation, the percentage of nano-
analyzed by X-Ray Fluorescence (XRF, Thermo Fisher), to particles was added to the solution (according to Table 1), and
determine the chemical composition of nanoparticles. The the solution was kept under magnetic stirring for 30 min. After
crystalline structure of the samples was evaluated by X-Ray that, the nanofluids were sonicated for 1 h (USC-1650A,
Diffraction (XRD, MiniFlex600, Rigaku), at a scanning speed of Unique).
10 min
1 with a step size of 0.05 .
A Transmission Electron Microscope (TEM, JEM 1011, JEOL) 2.6. Characterization of nanofluids
was used to analyze the inner structure of the samples, like
the crystal structure, morphology, and stress state informa- A particle size analyzer (Zetasizer Nano Series ZS, Malvern)
tion. Magnifications of 5000 to 300,000 were applied, with was utilized to measure the particle size and zeta potential by
point and line image resolution of 0.23 nm and 0.14 nm, Dynamic Light Scattering (DLS). The procedure was performed
respectively, and a goniometric stage with a dual tilt module at 25  C and the powder samples were dispersed in distilled
of ±30 . water (0.1 wt%) using an ultrasound bath for 1 h. To measure
Fourier-Transform Infrared Spectroscopy (FTIR, Cary 660, the size and zeta potential of the particles in the presence of
Agilent) was used to identify the functional groups present on NaCl and surfactant, components present in nanofluids, the
the surface of the samples. Dry nanoparticles were added to samples were prepared with a concentration of 0.75 wt%
potassium bromide (KBr) before it was placed in a sample nanoparticles, 3.0 wt% sodium chloride, and 0.12 wt%
bearer. surfactant.
The surface chemistry of the nanoparticles was deter- The relative viscosity of nanofluids was analyzed in
mined by X-Ray Photoelectron Spectroscopy (XPS), using a PHI the function of the shear rate using a rotatory rheometer
Versa-Pro II spectrometer utilizing a monochromatic Al Ka (Haake Mars, Thermo). The following parameters were
source (hn ¼ 1486.6 eV, 150 W) and the pressure in the analysis selected for the analysis: geometry with a diameter of 60 mm;
during data acquisition was sustained below 1  10
9 Torr. shear rate from 0 to 50 s
1, gap of 150 mm, and room
The binding energy (BE) scale was corrected utilizing the po- temperature.
sition of the peaks for the C 1s (284.8 eV) of the adventitious
carbon. The powder samples were mounted on a holder uti-
lizing double-sided adhesive tape. Narrow spectral regions
were recorded in addition to the survey photoelectron spectra.
The pass energy during the analysis was 25 eV for the narrow Table 1 e The concentration of silica nanoparticles, salt,
scans and 160 eV for the survey spectra. The individual and surfactant on solutions.
spectral regions were analyzed to calculate the relative ratios Silica Fluid Concentration (wt%)
of the surface of the solid, identify the chemical state of the nanoparticles formulations
NaCl Nanoparticle SDS
elements and determine the BE of the peaks. The obtained
spectra were analyzed after applying Shirley's background e Brine (B) 3.00 0.00 0.00
e Brine þ 3.00 0.00 0.12
subtraction and Gaussian (30%)eLorentzian (70%) decompo-
sition parameters using the Multipak software. surfactant (BS)
The analysis of the surface area and the pore size distri- Commercial Silica CS-NF0.10 3.00 0.10 0.12
bution were conducted using a gas sorption analyzer (Auto- (CS) CS-NF0.25 3.00 0.25 0.12
sorb, Quantachrome) with BrunauereEmmetteTeller (BET) CS-NF0.50 3.00 0.50 0.12
and BarretteJoynereHalenda (BJH) methods, respectively. The CS-NF0.75 3.00 0.75 0.12
Rice Husk Silica RH-NF0.10 3.00 0.10 0.12
N2 adsorption-desorption isotherms measurement at 196  C
(RH) RH-NF0.25 3.00 0.25 0.12
was performed after degassing at 300  C for 24 h.
RH-NF0.50 3.00 0.50 0.12
RH-NF0.75 3.00 0.75 0.12
2.5. Preparation of nanofluids Sol-Gel Silica (SS) SS-NF0.10 3.00 0.10 0.12
SS-NF0.25 3.00 0.25 0.12
For the preparation of nanofluids, commercial silica nano- SS-NF0.50 3.00 0.50 0.12
particles (CS), rice husk ash-derived silica (RH), and silica SS-NF0.75 3.00 0.75 0.12
4146 j o u r n a l o f m a t e r i a l s r e s e a r c h a n d t e c h n o l o g y 2 0 2 3 ; 2 4 : 4 1 4 3 e4 1 5 2

The turbidity of nanofluids was measured six times

(before the sonicator bath; 1 h, 2 h, and 24 h after the bath;
and the last was after the flooding tests) using a turbidimeter
properly calibrated with a 0.1 to 1000 NTU pattern scale.
Finally, the interfacial tension (IFT) of nanofluids was
measured using a goniometer (250, Rame
-Hart). In these an-
alyses, 3 mL drops of fluids (oil, water, solutions, or nanofluids)
at room temperature were deposited over a clean borosilicate
glass surface. Measurements of interfacial tension were per-
formed in triplicate and the results were determined by the
mean of the values obtained.
2.7. Oil recovery tests
The experimental apparatus used in the oil recovery tests is
shown in Fig. 1. A fixed-bed column (7.5 cm in diameter and
35.5 cm in height) with ascending flow was employed to
simulate an oil reservoir, as proposed by Rangel et al. [28] and
Son et al. [30]. The column bed, prepared before starting each
recovery test, was comprised of a mixture containing 950 mL
of mineral oil and 1.058 kg of sand (950 mL).
The sand used as a porous medium was purchased from a
local market (Santa Catarina, Brazil). It was sieved to obtain a
size between 300 and 600 mm and then washed for 3 h with
distilled water according to the same experimental system as
the flooding tests. Subsequently, the sand was dried in an
oven (DeLeo) at 80  C for 24 h.
Oil recovery was initially performed using 4 L of saline
solution (B) injected into the system for 5 h using a rotary
pump (75211-15, Cole-Parmer). Afterward, the enhanced re-
covery of residual oil from the bed begins by feeding 4 L of the
BS solution for 5 h (flow rate: 0.8 L h
1), followed by feeding 4 L
of nanofluid through the column (0.8 L h
1). At this stage, a
certain amount of oil is recovered, and another amount re-
mains in the reservoir. The amount of oil recovered was
measured in a graduated cylinder (Fig. 1), for the B, BS, and
each nanofluid sample, and the amount of oil recovered is
expressed as a percentage (%). The mixture of oil and water
collected from the porous cell was kept at rest for 24 h and
then the fluids are separated, using a density separator, and
each volume is measured [28].
3. Results and discussion
3.1. Characterization of silica particles
The chemical compositions of particles are shown in Table 2,
as determined by XRF. The silica obtained from rice husk (RH)
presented the highest purity among the three samples with
94.01 ± 0.26 wt% of SiO2 and about 5.99 wt% of impurity that
includes K, Ca, P, Mg, Al, Mn, Fe, Zn, S, Zr, and Ti.
The crystalline structure of all silica nanoparticles was
evaluated by XRD (Fig. 2). The commercial and sol-gel silica
nanoparticles are amorphous materials, and a broad signal
can be observed at about 2q ¼ 23 corresponding to the (002)
reflection of amorphous silica in CS and SS silica [31]. As
previously reported by Zulfiqar et al. [25], the synthesis of
silica nanoparticles from sodium silicate under alkaline con-
ditions produces only amorphous nanoparticles.
On the other hand, RH silica is crystalline and shows a
dominant peak in the XRD pattern at 22 due to the presence
of crystalline SiO2 in RH. The sharp narrow peaks at 22, 26, 31,
and 36 are attributed to cristobalite, tridymite, and quartz as
polymorphs of crystalline silica that were formed due to the
high temperature and time employed during the rice husk
treatment [32]. With the help of relevant equations and XRD
results, the crystallite size of RH can be estimated as 27 nm.
TEM was used to determine the geometry and shape of the
nanoparticles (Fig. 3). The images reveal the spheroidal
structure of nanoparticles, presenting a respective size of ~27,
~44, and 2453 nm for CS, RH, and SS nanoparticles, respec-
tively. The electron diffraction patterns obtained by TEM
(Fig. 3c, f, and 3i) confirmed that commercial and SS silica
particles are in an amorphous phase, while RH silica presents
higher crystallinity.
The textural characterization of silica nanoparticles is
shown in Table 3. Lower surface area and pore volume were
measured for RH and SS nanoparticles, while CS appears as a
mesoporous solid (Fig. S1).
The FTIR spectra of the silica nanoparticles are shown in
Fig. S2. The peaks at 3436 and 953 cm
1 can be attributed to the

Table 2 e Chemical composition by X-ray fluorescence of

commercial nanosilica, RH silica, and SS silica.
Commercial silica (wt RH silica SS silica
%) (wt%) (wt%)
SiO2 89.87 ± 0.33 94.01 ± 0.26 69.29 ± 0.51
K2O 0.04 ± 0.00 1.33 ± 0.05 0.04 ± 0.00
CaO 0.01 ± 0.00 0.83 ± 0.08 0.01 ± 0.00
P2O5 e 0.52 ± 0.02 e
MgO e 0.44 ± 0.05 e
Al2O3 1.07 ± 0.09 0.27 ± 0.02 0.11 ± 0.01
MnO e 0.22 ± 0.01 e
Fe2O3 0.12 ± 0.01 0.18 ± 0.02 0.07 ± 0.01
ZnO e 0.04 ± 0.00 e
SO3 0.04 ± 0.00 0.02 ± 0.00 e
ZrO2 0.02 ± 0.00 0.01 ± 0.00 0.04 ± 0.00
TiO2 0.05 ± 0.00 0.01 ± 0.00 0.09 ± 0.00
Fig. 1 e Experimental scheme of the system for oil recovery Na2O 0.94 ± 0.05 e 26.79 ± 0.24
tests: (I) magnetic stirrer; (II) fluid reservoir; (III) rotary Loss on 7.39 2.12 0.56
ignition
pump; (IV) fixed-bed column; and (V) graduated cylinder.
 j o u r n a l o f m a t e r i a l s r e s e a r c h a n d t e c h n o l o g y 2 0 2 3 ; 2 4 : 4 1 4 3 e4 1 5 2
Fig. 2 e XRD Diffractogram of (a) SS, (b) CS, and (c) RH
samples.
stretching vibrations of the OeH groups of silanol groups
(SieOH). The deformation of water molecules absorbed on the
SiO2 surface appears at 1635 cm
1. The peaks at 2920 and
2856 cm
1 are associated with symmetric and antisymmetric
elongations in eCH2 groups, respectively. The peaks at 1225,
1105, 804, 619, and 484 cm
1 are characteristic of silica and can
be related to different modes of SieO vibration [15,33,34]. The
FT-IR spectra did not show the significant presence of organic
Fig. 3 e TEM analysis of the samples: (a) CS structure in 100.000 £ ; (b) CS structure in 300.000 £ ; (c) CS crystal structure;
(d) SS structure in 5.000 £ ; (e) SS structure in 50.000 £ ; (f) SS crystal structure; (g) RH structure in 100.000 £ ; (h) RH structure
in 300.000 £ ; and (i) RH crystal structure.
4147
and inorganic impurities, which confirms the high purity
observed for the RH and commercial samples in the XRF
analysis.
XPS analysis (Fig. 4) was performed to obtain the compo-
sition and chemical states of the silica surface, and the results
are presented in Table 4. The XPS spectra with the corre-
sponding deconvolutions are illustrated in Figs. S3, S4, and S5
for commercial silica, RH silica, and SS silica, respectively.
The high-resolution core level spectra were corrected
considering the C 1s signal of adventitious carbon contami-
nation at 284.8 eV (Figs. S3, S4, and S5). Subsequently, the C 1s
core level spectra were decomposed into peaks that corre-
sponded to the hydrocarbon (CeC) at 284.8 eV (commercial
silica) or 284.9 eV (RH and SS silica); ethoxy (CeO) at 285.8 eV
(commercial silica), and carbonate at 289.3 eV (SS silica)
[35e37]. The CeO chemical bonds could be CeOeC or CeOeH
[36]. It can be seen that the eCH2e bond was presented on the
surface of all SiO2 nanoparticles, which was in good agree-
ment with the FTIR analysis. The Si 2p core level spectra of the
silica samples showed a main peak at ~103 eV which corre-
sponds to SieO bonds [38e40]. Sodium (Na 1s) is present in all
surface samples at ~1071e1072 eV [41], especially in SS
nanosilica, as also measured by XRF.
In all O 1s core level spectra (Figs. S3, S4, and S5) it is
possible to verify that most of the oxygen on the surface of the
nanomaterials is related to the siloxane group SieOeSi
(~532e533 eV) [41]. Total surface oxygen follows the order
CS > SS > RH (Table 4). These amounts are related to different
4148 j o u r n a l o f m a t e r i a l s r e s e a r c h a n d t e c h n o l o g y 2 0 2 3 ; 2 4 : 4 1 4 3 e4 1 5 2

of the silica nanoparticles in RH-NF0.10 grew visibly in the

Table 3 e Characteristics of silica samples.
nanofluids (Tables 5 and 6). The main reason for this change
Samples Specific surface Average pore Pore volume may be the aggregation of the nanoparticles, which can be
area (m2 g
1) size (
A) (cm3 g
1)
confirmed by the observed change in the zeta potential values
CS 100 317.5 0.793 [42]. On the other hand, SS-nanoparticles remain non-
RH 8.8 252.6 0.056 agglomerated and well-dispersed in the nanofluid [25].
SS 1.1 216.8 0.003
The stability of nanofluids was also evaluated by
measuring their turbidity after different standing times of
dispersion after sonication (Table 6). This technique is useful
synthesis processes that can lead to different degrees of water for nanoparticle stability studies and can reveal nanoparticle
chemisorption on the surface of nanoparticles, which is agglomeration and sedimentation as well as quantify nano-
closely related to the presence of oxygen-containing groups particle stability. As expected, Table 6 shows that the increase
on the surfaces. in the solid content leads to an increase in the light back-
scattering. On increasing the solid content, the agglomerate
3.2. Characterization of nanofluids size increases, and the turbidity is also increased, but remains
nearly constant after 24 h and indicates the stability of
To quantify the stability of nanofluids their zeta-potential was nanofluids [45].
measured after different standing times, as shown in Table 5. To achieve high oil recovery, it has been proposed that the
High zeta potential values indicate that the particles are nanofluid viscosity should be of the same order of magnitude
electrically stable due to electrostatic repulsion [15]. The as the viscosity of the oil. When the viscosity of the nanofluid
repulsive and attractive forces determine the stability of sus- is much lower than the viscosity of the oil, the nanofluid flows
pensions when solid particles collide with each other in a more easily between the pores in the direction of the pro-
liquid medium [29,42,43]. According to Setia et al. [44], a duction pools, without removing the oil from the pores,
nanofluid exhibiting a value of zeta potential greater than resulting in a low recovery factor. It is known that the viscosity
30 mV and lower than
30 mV is stable and resists agglom- of nanofluid can be altered by altering concentration, particle
eration. As shown in Table 5, CS-NF0.10 and SS-NF0.10 are size, shape, hydrophobic-hydrophilic character, and Newto-
stable, while RH-NF0.10 has limited stability. nian or non-Newtonian behavior [46].
The RH-nanoparticles tend to agglomerate over time (Table In the present study, the viscosity at different concentra-
5) because of inter-particle adhesion forces. The average size tions showed that shear stress increases linearly with an

Fig. 4 e XPS survey spectra for silica nanoparticles: (a) commercial; (b) RH; and (c) SS.
 j o u r n a l o f m a t e r i a l s r e s e a r c h a n d t e c h n o l o g y 2 0 2 3 ; 2 4 : 4 1 4 3 e4 1 5 2 4149

Table 4 e XPS analysis and quantification for commercial, RH, and SS silica.
Element Composition (Atomic %)
Commercial SiO2 RH SiO2 SS SiO2
Elemental analysis C 12.0 18.3 23.7
O 59.4 57.1 48.0
Na 0.6 0.2 15.2
Si 30.0 21.9 11.9
Mg e 1.3 e
K e 1.2 e
Cl e e 1.2
C 1s e 284.8 eV (85%) 284.9 eV (100%) 284.9 eV (79%)
e 285.8 eV (15%) e 289.3 eV (21%)
O 1s e e e 531.0 eV (27%)
e 533.0 (100%) 532.7 eV (100%) 532.5 eV (62%)
e e e 536.0 eV (11%)
Na 1s e 1072.7 eV (100%) 1071.5 eV (100%) 1071.6 eV (100%)
Si 2p e 103.5 eV (100%) 103.5 eV (100%) 103.1 eV (100%)

Table 5 e Average particle size and zeta potential (ZP) of Table 6 e Turbidity of the nanofluids after different
the nanofluids after different standing times. standing times.
Samples 1st day 30th day Nanofluid Turbidity (NTU) Images of NF after
24 h of sonication
Size (nm) ZP (mV) Size (nm) ZP (mV) Standing time of
dispersion after
CS-NF0.10 3772
31.1 1331
34.9
sonication
RH-NF0.10 1370
25.8 3939
19.5
SS-NF0.10 1863
19.2 1082
41.7 0h 1h 24 h
CeNF0.10 167 181 165
CeNF0.25 291 344 310

increase in shear rate, indicating Newtonian behavior for the

nanofluids. The particle size has a direct relationship with the
nanofluid viscosity [42,47] and large particles usually form
highly viscous nanofluids [48]. Although nanoparticles are
agglomerated in CS and RH-nanofluids, the nanofluid viscos-
ity decreases in the order SS-NF > RH-NF ~ CS-NF, which fol-
lows a similar order of nanoparticle sizes (SS >> RH > CS).
RH-NF0.10 167 169 139
Moreover, Table 7 shows a tendency to increase the viscosity
RH-NF0.25 169 172 161
of all nanofluids with the nanoparticle concentration, even at
a low concentration [46,48].
The interfacial tension of the oil and the injected nanofluid
is one of the main characteristics to determine the movement
and the distribution of fluids in porous media [9,49]. As shown
in Table 7, considering the small variation in the results, the
interfacial tension showed no relevant difference between the
different types of nanoparticles in the nanofluids and is nearly SS- NF0.10 8.8 5.2 55
early independent of nanoparticle concentration for CS and SS- NF0.25 25.0 15.3 88
SS-nanofluids (0.10e0.75 wt% range) and increases with
nanoparticle concentration for RH-nanofluid.

3.3. Flooding tests

Table 8 shows the oil recovery from each oil recovery step
using different nanofluids. Tests with solutions B and BS were
also conducted to evaluate the effect of salt and surfactant on
oil removal, respectively. After oil recovery in the primary and
secondary oil recovery, around 58% of oil is recovered. Yousefvand et al. [45] using HPAM as an additive in their
The nanofluid-enhanced oil recovery in this study is higher silica-based nanofluid.
than that reported by Chaturvedi and Sharma [29] with In general, the tertiary oil recovery using CS-NF increases
nanofluids containing 0.10 to 0.75 wt% silica nanoparticles. On as the nanoparticles concentration increases, due to the
the other hand, 13.37%e20.87% of oil recovery was reached by increase in viscosity, as also reported by Lashari and Ganat
4150 j o u r n a l o f m a t e r i a l s r e s e a r c h a n d t e c h n o l o g y 2 0 2 3 ; 2 4 : 4 1 4 3 e4 1 5 2

Table 7 e Viscosity and surface tension of the solutions.

Viscosity (mPa$s) Interfacial tension (mN$m
1)
Oil 473.13 22.4 ± 0.2
Water 1.37 70.9 ± 0.6
B 0.73 66.9 ± 0.5
BS 0.75 37.3 ± 0.0
CS-NF0.10 0.60 29.2 ± 0.1
CS-NF0.25 0.68 29.5 ± 0.1
CS-NF0.50 0.89 26.6 ± 0.1
CS-NF0.75 0.81 28.4 ± 0.1
RH-NF0.10 0.77 28.1 ± 0.1
RH-NF0.25 0.69 30.4 ± 0.1
RH-NF0.50 0.81 30.1 ± 0.1
RH-NF0.75 0.63 30.2 ± 0.1
SS-NF0.50 1.10 27.5 ± 0.1 Fig. 5 e Turbidity of different nanofluids before and after
SS-NF0.75 1.70 26.7 ± 0.1 flooding tests.

Table 8 e Oil recovery after flooding tests using B, BS, and
different nanofluids.
Solution Recovery Factor (%)
B 47.8 ± 5.9
BS 10.1 ± 1.5
Nanofluids CS-NF RH-NF
NF0.10 4.7 4.7
NF0.25 5.3 8.9
NF0.50 5.8 5.8
NF0.75 7.9 5.8
[50]. Others studies indicated that silica-based nanoparticles
have a promising ability to change wettability and reduce
IFT [1]. However, in our work, the concentration of surfac-
tant was kept constant for all nanofluids, and the IFT did not
show a large variation. Thus, no significant effect of inter-
facial tension in the oil recoveries was observed for all
nanofluids.
Additionally, CS-NF and RH-NF result in similar recovery
factors, indicating that rice husk ash is a promising material to
produce nanofluids. It is known that the increment in the NPs
concentration could reduce the reservoir IFT, accompanied by
a substantial change in the wettability of the rocky surfaces.
Repulsive forces between nanoparticles increase the viscosity
of the nanofluids [51], which contributes to the enhancement
of displacement efficiency (Table 8).
The SS nanoparticles are retained in the sand bed,
causing a decrease in the SS-NF0.10 and SS-NF0.25 turbidity,
as shown in Fig. 5, which becomes more important as the
nanoparticles concentration increases. Thus, increasing the
SS nanoparticle concentration could decrease the perme-
ability of reservoir rock with high clogging coefficients [53].
However, the CS and RH nanoparticles do not seem to be
retained in the sand bed since the nanofluid turbidity showed
a slight increase after the flooding test. This may have
occurred due to the deagglomeration of the nanoparticles
when passing through the bed, allowing their passage through
the reservoir [52], though further analysis would be needed to
establish what happened.
4. Conclusions
The current study was an experimental investigation of various
sources of silica nanoparticles to produce nanofluids applicable
in enhanced oil recovery (EOR). Rice husk ash proved to be a
suitable raw material to produce crystalline and nanosized
material useful in EOR. With a nanoparticles concentration in
SS-NF
the range of 0.10e0.75 wt%, stable nanofluids were prepared
6.8 using rice husk ash silica and sol-gel silica with similar vis-
7.4 cosity and interfacial tension as nanofluids formulated using a
10.0
commercial nanosilica. Although the nanoparticles can be
7.9
agglomerated after 24 h-standing time, the stability of the
nanofluids is guaranteed by a suitable repulsive force and zeta
potential lesser than
30 mV. Oil recovery in the tertiary step is
affected by the nanofluid viscosity, which increases as the
nanoparticles concentration increases. An additional 5e10% oil
recovery is achieved after flooding due to the injection of
nanofluids, proving that silica from rice husk ash has compa-
rable efficiency to other synthetic silica nanoparticles for
application in enhanced oil recovery.
Funding
This work was supported by the Human Resources Program of
the National Agency for Petroleum, Natural Gas and Biofuels e
PRH/ANP, supported by resources from the investment of oil
companies qualified in Clause P, D&I of ANP Resolution No. 50/
2015; Brazilian Coordination for the Improvement of Higher
Education Personnel (CAPES) e Project Number 88881.142487/
2017-01; CNPq e Grant number 150.164/2020-3 and 405.223/
2018-8, and Consejerı́a de Transformacio
n Econo
mica,
Industria, Conocimiento y Universidades (Project P20_00375)
and FEDER funds.
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.
 j o u r n a l o f m a t e r i a l s r e s e a r c h a n d t e c h n o l o g y 2 0 2 3 ; 2 4 : 4 1 4 3 e4 1 5 2 4151

[13] Kumar RS, Chaturvedi KR, Iglauer S, Trivedi J, Sharma T.

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