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Surfactants: Recent advances and their applications

Samy M. Shaban, Joohoon Kang, Dong-Hwan Kim

PII: S2452-2139(20)30265-5
DOI: https://doi.org/10.1016/j.coco.2020.100537
Reference: COCO 100537

To appear in: Composites Communications

Received Date: 24 August 2020

Revised Date: 15 October 2020
Accepted Date: 16 October 2020

Please cite this article as: S.M. Shaban, J. Kang, D.-H. Kim, Surfactants: Recent advances and their
applications, Composites Communications (2020), doi: https://doi.org/10.1016/j.coco.2020.100537.

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 Mini-Review

Surfactants: Recent Advances and Their Applications

Samy M. Shaban1,2,3, Joohoon Kang4,*, and Dong-Hwan Kim1,2,*
1. School of Chemical Engineering, Sungkyunkwan University (SKKU), Suwon 16419,
Republic of Korea
2. Biomedical Institute for Convergence at SKKU (BICS), Sungkyunkwan University
(SKKU), Suwon 16419, Republic of Korea
3. Petrochemicals Department, Egyptian Petroleum Research Institute, Egypt
4. School of Advanced Materials Science and Engineering, Sungkyunkwan University

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(SKKU), Suwon 16419, Republic of Korea

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E-mail: dhkim1@skku.edu (D.-H. K.) and joohoon@skku.edu (J.K.)
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Abstract
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Surfactants have been widely used in many industrial products such as detergents,
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medicines, and anti-corrosive treatments due to their unique structures consisted

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of two different molecular parts and the broad range of selection. Surfactants
have also contributed significantly to many research fields, especially in
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nanotechnology. For example, the amphiphilic nature of surfactants has been

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exploited to stabilize hydrophobic nanomaterials in water, affording access to a

plethora of solution-processed nanomaterial-based scalable applications.
Surfactants are also a key additive in the production of well-controlled
nanoparticles. Surfactant-assisted metallic nanoparticle production has enabled
the realization of colorimetric sensors, which are of massive interest in numerous
interdisciplinary applications owing to their simplicity, practical applicability,
cost-effective production, high stability, and high selectivity. Surfactants added
during nanoparticle synthesis play a critical role in optimizing the sensor
sensitivity and selectivity because they directly affect the nanoparticle properties.

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 Mini-Review

Further, a new category of surfactants with magnetic properties has been

introduced for drug delivery applications. In this short review, we provide an
overview of the fundamentals of surfactants and their applications for the
development of nanotechnology.

Keywords: Surfactant; amphiphilic; stabilizer; nanoparticle synthesis; nano-

sensors; magneto surfactants

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 Mini-Review

1. Introduction

Surfactants are organic compounds composed of two chemical parts with

different polarities, a head group with affinity for polar phases, and a tail group
that is attracted to nonpolar phases [1-7]. Due to their structural uniqueness,
surfactants can be widely used to reduce the surface and interfacial tension
between two or more phases [8-11]. Their tendency to generate self-assembled
structures in solution can also lead to the formation of micelles with diameters

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ranging from nanometers to microns [12, 13]. The amphiphilic nature of

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surfactants makes them suitable for use in numerous industrial products,
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including medicines [14-16], corrosion inhibitors for protecting steel and other
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corrosive metals [17-20], detergents [21-23], de-emulsifiers [24, 25], wetting
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agents [26, 27], oil recovery enhancers [28-31], pour-point depressants [32-34],
pharmaceutical formulations [35-37], and drug delivery [38-40].
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In addition to industrial applications, surfactants have great potential to

overcome the current limitations in nanotechnology [41-46]. For example,
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amphiphilic surfactants have been reported as stabilizers for the preparation of

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stable dispersions of hydrophobic inorganic nanomaterials such as carbon

nanotubes [47-49], graphene [50], transition metal dichalcogenides [51], and
black phosphorus [52]. Since the first graphene exfoliation method,
micromechanical exfoliation, was discovered in 2004 [53], researchers have
attempted scale-up of the process by stabilizing exfoliated graphene in solvents.
Considering the accessibility and environmental toxicity of organic solvents [48],
water may be an ideal solvent system for preparing nanomaterial dispersions, but
most inorganic nanomaterials have hydrophobic surfaces and thus exhibit
repellent behavior in water. To overcome this limitation, various organic solvents

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 Mini-Review

have been exploited for stabilizing nanomaterials, such as N-methyl-pyrrolidone

and dimethylformamide [54-58]. Although these organic solvents can
successfully disperse nanomaterials, their high boiling points leads to the
requirement for additional high-temperature annealing to remove the solvent,
which may induce chemical degradation of the nanomaterials and obscure their
toxicity limits for use in biological applications [48]. This hurdle was overcome
by adding amphiphilic surfactants to water, together with inorganic nanomaterials.

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The hydrophobic parts of the surfactants interact with the surfaces of the

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nanomaterials, and the hydrophilic parts stabilize the surfactant-nanomaterial
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composite in water. Furthermore, the buoyant densities of nanomaterials can be
controlled based on the type of surfactants, which enables the separation of
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nanomaterials in the structure via isopycnic density gradient ultracentrifugation
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[59]. The resulting structurally sorted nanomaterials have contributed

significantly to many research fields in nanotechnology, especially electronics
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[60-62], optoelectronics [57, 63, 64], energy [58, 65, 66], biology [48], and
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catalysis [54].
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Due to the potential advantage of surfactants for tuning the surface/interface

tensions between solid/liquid interfaces and further improving the dispersion
stability, surfactants may be a key agent in the synthesis of nanoparticles with
well-controlled geometries. Recently, researchers have focused on nanoparticle-
based sensors that detect organic and inorganic pollutants and biomolecular
compounds in serum or urine samples as biomarkers for the early diagnosis of
diseases. One approach is to use localized surface plasmon resonance phenomena
on a nanoparticle array, where the nanoparticle size and shape, degree of
aggregation, and refractive index affect the sensitivity of the sensors [67, 68].
Furthermore, advanced sensing systems have been developed for enhancing both

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the identification and transduction processes by using many novel nanoparticles

rather than conventional organic dye-based sensing assays, where the former
offer advantages in sensitivity, selectivity, stability, reusability, and practical
applicability [69-75]. Among the available methods, colorimetric methods are
simple, highly efficient, and exhibit great potential for point-of-care diagnosis
because the detection process is facile as responses can be discerned by the naked
eyes or via simple instrumental techniques [76-81]. For colorimetric applications,

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the unique physical and chemical properties (size, shape, large active surface

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area, and higher activity) of nanoparticles afford tremendous catalytic activities
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that differ from those of their bulk counterparts due to size-induced quantum
confinement effects in the former [80, 82-85]. For example, colloidal plasmonic
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gold and silver nanoparticles have been most intensively studied as they produce
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rapid and vivid responses to incident light, and can be efficiently used for the
sensitive detection of target analytes through visible color changes in the solution
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phase [86-91].
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In this short review, we provide an overview of surfactants for nanoparticle

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synthesis and discuss the detailed relationships between the molecular structure of
the surfactant and the resulting particle structure distributions for optimizing
ultrasensitive detection in sensing application devices. We also discuss a new
category of surfactants that have magnetic properties for drug delivery, protein
separation, DNA extraction and catalyst applications.

2. Surfactant structure dependent synthesis and properties

2.1 Surfactant modification for nanoparticle synthesis

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 Mini-Review

The amphiphilic characteristics of surfactants play an important role in

nanoparticle synthesis by preventing aggregation of the synthesized nanoparticles
and providing more stability in colloidal systems [43, 92-97].
Surfactant-assisted nanoparticle synthesis has attracted considerable
attention in the development of nanoscale sensors for detecting toxic materials
[98-100], biomaterials, and biomarkers [101-103]. Because nanoscale sensors
should distinguish a trace amount of material, it is necessary to achieve high

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sensitivity and selectivity for a specific analyte. The sensitivity and selectivity are

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strongly related to the structural parameters of the nanoparticles, including the
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precise size distribution. Consequently, controlling the size by modifying the
molecular structure of the surfactant can provide a new strategy for maximizing
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the sensitivity enhancement. One such approach in which the tail length of the
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surfactant was altered to control the nanoparticle size, growth, and colloidal
stability was recently reported [95, 96, 104].
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The colloidal stability of surfactant-nanoparticle hybrid systems can be

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described by the thermodynamic Gibbs free energy changes (ΔG°), which

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strongly depend on the free energy for surfactant micellization (ΔG°mic) and
adsorption (ΔG°ads), surface tension, and critical micelle concentration. Such
factors are highly correlated to the molecular structure of surfactants, from head
to tail [105]. To understand the impact of the molecular structure of the surfactant
on the stability of the synthesized nanoparticles in the colloidal state, we must
first understand the behavior of surfactants in solution systems.
Surfactants consist of two parts with opposing polarities, which makes the
surfactant solution thermodynamically unstable due to the repulsive force
between the hydrophobic tail of the surfactant and the polar medium in which the
surfactant is dissolved. This repulsion forces the surfactant to be adsorbed on the

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nanoparticle and undergo micellization to stabilize the system by lowering the

free energy. In the surfactant-nanoparticle hybrid system, the surfactant
monomers direct themselves toward the surface of the nanoparticles through
interaction of the hydrophobic surfactant tail with the nanoparticles via
electrostatic interaction or van der Waals forces during the synthesis process,
while the hydrophilic surfactant head is in contact with the polar solvent,
consequently reducing the interfacial tension between the nanoparticles and

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solvent. This arrangement decreases the free energy of the surfactant-nanoparticle

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hybrid system and enhances stabilization of the nanoparticles in the surfactant
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solution [104, 106-110]. Thus, increasing the surfactant hydrophobicity by
chemical structure modification will enhance both the adsorption and self-
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assembly of the surfactant on the nanoparticle surface, and greater stability in
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solution can be attained.

Ordóñez et al. reported the effects of nonionic (polyvinyl pyrrolidone,
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PVP), cationic (cetyltrimethylammonium bromide, CTAB), and anionic

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surfactants (sodium dodecylbenzene sulfonate, SDBS) on the stability of

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zirconium oxide nanoparticles, ZrO2. The results outlined an improvement in the

stability, and reduced agglomeration of the synthesized ZrO2 with the surfactant
[95]. Both SDBS and CTAB surfactants conferred higher stability to the ZrO2
suspension, with zeta potentials of −50.38 ± 2.13 and 42.22 ± 3.27 mV compared
to that induced by PVP with a zeta potential of −19.99 ± 2.9 mV. A similar trend
was observed by Grządka et al. who reported that some cationic surfactants such
as CTAB, silicone surfactants, and fluorocarbon (S-106-A) surfactants improved
the stability of alginic acid/ZrO2 nanofluid [111].
The colloidal stability of the as-prepared AgNPs was found to be dependent
on the length of the hydrocarbon tail of a series cationic surfactants, as reported

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by Shaban et al. [112]. The surfactant with a longer tail (C16Dim) produced more
stable AgNPs with a zeta potential of 52 ± 10.7 mV, whereas the shorter-tail
surfactant C10Dim produced less stable AgNPs with a relatively lower zeta
potential of 34.1 ± 10.4 mV. Another study on the effect of modifying the
surfactant chain length on the synthesized AgNPs was also conducted by Abd-
Elaal et al., where they found that the aggregation and particle size mainly
depended on the length of the hydrophobic tail of three different nonionic

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surfactants, namely, HTOPD, HTOPT, and HTOPH, with 12, 14, and 16 carbon

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atoms, respectively [113]. In addition, the surfactant HTOPH with a longer chain
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length yielded more stable AgNPs, whereas the zeta potentials of the AgNP
colloids obtained with HTOPD, HTOPT, and HTOPH were ‒23.7, ‒32.7, and ‒
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35.4 mV, respectively. Similar behaviors have also been reported elsewhere [114-
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116]. Aiad et al. reported the dependence of the stability of AgNPs on the
amphipathic alkyl chain of two series of antipyrine cationic surfactants [117]. By
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utilizing a series of surfactants (APC8, APC12, and APC16, where 8, 12, and 16
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refer to the number of carbon atoms in the alkyl chain), the zeta potential
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increased to +31, +34, and +40 mV for the series APB8, APB12, and APB16,
respectively, indicating an increase in the nanoparticle stability with the
surfactants [117].

The effects of the spacer length of a synthesized Gemini cationic surfactant

with structures 18-s-18 (s equal to 3, 4, 6, 8, 10, and 12) on the stability of AuNPs
were reported by Qian Liu et al. [118]. As the spacer length increased, the
stability of the synthesized AuNPs increased, as confirmed by the increased zeta
potential of the AuNPs. The maximum zeta potential was obtained when s = 8
carbon atoms. Similar results have been reported by Pisárčik Martin et al. [119],

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 Mini-Review

who investigated the correlation between the surfactant structure and stability of
as-synthesized AgNPs. Increasing the length of the hydrophobic carbon
substituents associated with the ammonium head led to the formation of AgNPs
with a higher zeta potential, as an indication of their higher stability [119]. Morsi
et al. reported that using CTAB and SDS as respective cationic and anionic
surfactants improved the stability of yttrium oxide nanoparticles, where the
measured zeta potentials were 37.3 mV and ‒61.7 mV for the Y2O3/CTAB and

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Y2O3/SDS systems, respectively, indicating stable nanofluid systems. In

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accordance with previous reports, Peng et al. reported that the stability of C60
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nanoparticles was improved by SDBS, where the zeta potential of the C60-SDBS
complex was ‒49.5 mV [96].
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Based on previous reports, it is concluded that the surfactant strongly affects the
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stability of the synthesized nanoparticles. The stability is also influenced by the

hydrophobic tail of the surfactant and the spacer, as in the case of the Gemini
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surfactant, where these factors improved the stability of the produced nanofluid
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system.
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In general, modification of the chain length of surfactants and the hydrophobic

spacers between the hydrophilic heads are found to control the size distribution of
the as-synthesized nanoparticles, which can provide a route for enhancing the
sensitivity of nanoscale sensors. Adsorption of surfactant molecules onto the
surface of the nanomaterials not only controls their stability, but also significantly
controls the particle size. The surfactant is characterized by excellent adsorption
on the surface of the nanoparticles and can readily form micelles. The presence of
the surfactant during nucleation of the nanoparticles can control the growth of the
nanoparticles. As the hydrophobicity of the surfactant increases, the rate of
migration onto the surfaces of nanoparticles in nanomaterials increases, forming a

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more protective layer, thereby maintaining the dispersion of the nanoparticles in

solution with less agglomeration. Consequently, a larger particle size is attained.
In another study on the effect of modifying the surfactant chain length on
the particle size of the synthesized AgNPs, Abd-Elaal et al. found that the particle
size mainly depended on the length of the hydrophobic tail of three different
nonionic surfactants, HTOPD, HTOPT, and HTOPH, having 12, 14, and 16
carbon atoms, respectively. It has been reported that the size of AgNPs is reduced

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as the tail length increases from 12 to 16 (Figure 1b) [113].

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Figure 1. (a) Characterization of Au nanoparticles formed with Gemini surfactant

(18-s-18) having different spacer lengths. Reproduced from Ref. [118]. (b)
Surfactant tail length-dependence of aggregation tendency and size of AgNPs:
(A) HTOPD, (B) HTOPT, and (C) HTOPH nonionic surfactants. Reproduced
from Ref. [113].

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 Mini-Review

Shaban et al. revealed the effect of the length of the hydrophobic tail of the
surfactant by exploring the effect of cationic, Gemini cationic, and polymeric
anionic surfactants on the geometric modifications and size of silver nanoparticles
(AgNPs) prepared in situ via the photochemical reduction method [104, 110,
120](Figure 2a-c). Increasing the hydrocarbon chain length of the surfactant tail
led to the formation of smaller AgNPs.

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Figure 2. TEM images and DLS size distribution data for AgNPs synthesized
using different surfactants with various hydrophobic chain lengths; the
hydrophobic chain length increases from left to right. (a) Gemini cationic

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surfactant-AgNP colloidal system, (b) anionic polymeric surfactant-AgNP

colloidal system, and (c) cationic surfactant-AgNP colloidal system. Reproduced
from Refs. [104, 110, 120].

Similar results have been reported by Pisárčik Martin et al. [119], who
investigated the correlation between the surfactant structure and particle size of
as-synthesized AgNPs. Increasing the length of the hydrophobic carbon

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substituents associated with the ammonium head led to smaller AgNPs. The size

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of the AgNPs was controlled by changing the length of the surfactant tail, as
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reported by Feng Xu, et al. A new series of Gemini surfactants Cn-C4-Cn.2Br,
where n = 12, 14, 16, and 18 carbon atoms, was prepared, and it was shown that
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the size of the AgNPs decreased as the number of carbon atoms attached to the
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hydrophilic head increased; the size was 5.6 ± 1.9, 5 ± 1.8, 3.9 ± 1.4, and 4 ± 1.4
nm, respectively [121]. Similar behaviors have also been reported elsewhere
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[114-116]. Aiad et al. reported size control of AgNPs based on the amphipathic
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alkyl chain of two series of antipyrine cationic surfactants [117]. By utilizing the
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APC8, APC12, and APC16 series, where 8, 12, and 16 refer to the number of
carbon atoms in the alkyl chain, the size of the AgNPs decreased from 25 to 15
nm as the length of the hydrophobic tail increased [117]. Surfactant-dependent
size modification has also been demonstrated for ZnS nanoparticles, where
particle diameters of 55.5 ± 0.5, 13.4 ± 0.5, and 11.6 ± 0.5 nm were obtained
using different surfactants, namely DTAB, TTAB, and CTAB, respectively,
where the formation of smaller nanoparticles was triggered by the hydrophobicity
of the surfactant tail [122]. The effect of the nonionic chain length (polyethylene
glycol chains) on the preparation of a silver nanohybrid was reported by Negm et
al. [123]. The particle diameter was influenced by the polyethylene glycol chains

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joined to the polyurethane nonionic surfactant. The size of the AgNPs decreased
from 152 to 14 nm as the molecular weight of polyethylene oxide in the nonionic
chains increased from 400 to 100000 g/mol. El-Dib et al. reported that the use of
a surfactant during the synthesis of magnetite nanoparticles (Fe2O4) produced
smaller particles than those achieved without surfactants [124].
The head groups of surfactants can be replaced that affects to size,
hydrophobicity/hydrophilicity, and degree of aggregation of nanoparticles. Mehta

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et al. have reported that the size of ZnS nanoparticles and their dispersion stability

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can be controlled by variation of the hydrophilic head group [125]. Two cationic
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surfactants with different hydrophilic cetyltrimethylammonium chloride (CTAC)
and cetyltrimethylpyridinium chloride (CPyC) were explored, where the large
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head surfactant CPyC shows higher affinity and yields smaller ZnS nanoparticles
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with higher colloidal stability compared to CTAC [125]. Based on the approach,
it was proved that the smaller size of ZnS can be synthesized using CPyC due to
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more hydrophobic pyridine ring in CPyC compared to the trimethyl groups in

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CTAC, and thus the hydrophobicity of the CPyC is much higher than CTAB,
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which can be the controlling factor of ZnS nanoparticles size.

In addition to the size control, shapes of nanoparticles can be controlled
based on a molecular structure of incorporated surfactant via a controlling the
facet growth method. In this case, surfactants play a role as a shape directing
agent [126-129]. A hydrophobic tail length of a surfactant significantly affects a
shape of gold nanorods as reported by Gao et al., as the length of the alkyl chain
increases from 10 to 16 carbons atoms, an aspect ratio of synthesized gold
nanorods increases [127]. A longer hydrocarbon chain produces a compacted
bilayer because of the stronger hydrophobic tail interactions that allows less
possibility of freshly generated gold atoms penetration to nucleate laterally,

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therefore both ends of the nanorod are preferred for further growth resulting in
the formation of higher aspect ratio gold nanorods [129, 130]. Furthermore,
surfactants control the nucleation and growth of nanoparticles during a seed-
mediated growth, and yield various shapes of gold and silver nanoparticles (e.g.,
rods, spheres, cubes, and octahedra) [131-134]. The Kou et al. used the seed
mediated growth method for gold nanorods and bipyramids synthesis. They
revealed that cetyltriethylammonium bromide (CTEAB) can control the shape of

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the gold nanorods while absence of the CTAEB and using citrate as stabilizing

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agent can produce both gold nanorods and gold bipyramids [135].
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2.2 Surfactant structure dependent nanoparticle properties
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Modification of the geometry of as-synthesized nanoparticles based on the

molecular structures of the surfactants, where the size distribution and the
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colloidal stability are strongly correlated to the alkyl chain length, can open a new
avenue for optimizing the desired properties of nanoparticles. In this section, we
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discuss the effects of varying the surfactant structure (i.e., alkyl chain length) on
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the nanoparticle properties.

Dadwal and Joy et al. reported the colloidal stability of Fe3O4 nanoparticles in
toluene solvent using myristic, palmitic, and stearic acid as surfactants with long
alkyl chains. It was demonstrated that different chain lengths influenced the
thermal conductivity of the magnetite nanofluid under an applied magnetic field.
The thermal conductivity decreased as the length of the surfactant chain increased
[136]. Modification of the alkyl chain length also affects the antimicrobial
activity of nanoparticles, as reported by Shaban et al. It was demonstrated that
increasing the tail length of the surfactant changed the antibacterial activity of the

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AgNP nanohybrid system [112, 114-116]. In another study by Aiad et al., a

similar result was demonstrated wherein the surfactant tail length modified not
only the size of the AgNPs, but also their antimicrobial activity [117]. In a
different material obtained by Negm et al. [137], it was shown that cationic
polymeric surfactants with different alkyl chain lengths (8 and 12 carbon atoms)
did not affect the size of copper nanoparticles, but influenced the antimicrobial
activity. In addition, increasing the number of ethylene oxide units in a

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synthesized cationic quaternary polymer produced smaller silver nanoparticles

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with high microbial activity against sulfate-reducing bacteria [138]. Zhou et al.
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investigated the synergetic effect between SDS and TiO2 nanoparticles on the
viscosity of water-based nanofluids at different temperatures. Zhou reported that
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the resulting viscosity of the suspension when both SDS and TiO2 were added
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together in water was lower than when they were added separately [139]. Kumari
et al. investigated the effect of some surfactants, CTAB, SDS, and TX-100, on the
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toxicity of AgNPs toward the crop Fagopyrum esculentum L [140]. The

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phytotoxic effect of the AgNPs formed without any surfactant induced 77.4% cell
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death compared to the control without AgNPs. Treatment of the plant crop
Fagopyrum esculentum with AgNPs with incorporated surfactants (TX-100,
CTAB, and SDS) led to a significant reduction in the cell death (by 37%). As
illustrated in Figure 3, that study provides promising data on the significant role
of surfactants in enhancing plant tolerance to AgNP stress and ensuring food
safety [140].

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Figure 3. Schematics showing the change in the phytotoxic effect of AgNPs
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on the crop Fagopyrum esculentum with the use of different surfactants.
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Reproduced from Ref. [140].
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Ghahfarokhi et al. investigated the effects of different molecular weights of

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ethylene oxide surfactants on the magnetic properties of spinel-strontium ferrite

(SrFe2O4) nanoparticles [141]. The addition of ethylene glycol surfactants
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decreased the particle size of SrFe2O4, thereby increasing the magnetism of

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SrFe2O4, as evaluated using a vibrating sample magnetometer, owing to the

reversible relationship between the magnetic coercivity and particle size of
SrFe2O4, which greatly depends on the ethylene glycol surfactant.

3. Ionic surfactants with magnetic properties

In the past decade, an enthralling new class of ionic liquid surfactants with
magnetic responsivity, termed magnetic ionic liquids or magneto surfactants, has
been reported [142-144]. These new categories of surfactants exhibit a unique
magnetic response in addition to the common properties of the surfactants (i.e.,

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adsorption and micellization). Magneto surfactants were first discovered by

Brown et al. in 2012 [145, 146], and have been rapidly developed in the fields of
biomedicine and magneto nanomaterial immobilization [147, 148]. In this
section, we discuss the synthesis, properties, and applications of magneto
surfactants.

3.1. Synthesis of magneto surfactants

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Magneto surfactants were synthesized by stirring a metal trihalide with a

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surfactant in an alcoholic solution for 12 h, as shown in Scheme 1a [149]. Kevin
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et al. reported the successful synthesis of a new series of paramagnetic ionic
liquid surfactants based on N,N'-bis(alkyl)imidazolium bromotrichloroferrate.
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Scheme 1b illustrates the protocol for the synthesis of [(Cn)2Im][FeCl3Br] and
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[CnC1Im][FeCl3Br], where C1 refers to a methyl group; Cn refers to ethyl, butyl,

hexyl, octyl, decyl, and dodecyl groups in succession; and Im refers to imidazole
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[150].
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Scheme 1. (a) Synthesis of magneto surfactant alkyltrimethylammonium

bromotrichloroferrate, reproduced from Ref. [149]. (b) Preparation of
[(Cn)2Im][FeCl3Br] and [CnC1Im][FeCl3Br] magnetic surfactants. Reproduced
from Ref. [150].

Subsequently, Brown et al. reported a new set of magnetic surfactants based on

a lanthanide metal as a counter ion (Table 1), where one mole of metal trichloride
was added to the methanolic solution of nonmagnetic surfactant DTAB or
C10mimCl, the mixture was stirred overnight (12 h) at room temperature, and then

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dehydrated under vacuum at 80 °C overnight to obtain the desired magnetic

nanoparticles [145].

Table 1. Chemical structure of some prepared lanthanide magnetic surfactants.

Reproduced from Ref. [145]

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Under an applied magnetic field, the surface tension changes reversibly, and this
property of magneto surfactants allows a switching “on” and “off” behavior by
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controlling the external magnetic field [151]. A change in the surface parameters
was also proved by Brown et al., where the surface tension could be reduced by
12.1% compared to that achieved with the corresponding nonmagnetic surfactant
under identical conditions, as illustrated in Figure 4. Here, H refers to holmium
metal [145].

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Figure 4. Pendant drop profiles of magnetic surfactants (0.1 mol) with and
without an external magnet. Reproduced from Ref. [145].
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Another new series of cationic and anionic magneto surfactants based on a
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gadolinium counter ion [152] with CTAG (cationic

hexadecyltrimethlyammonium bromotrichlorogadolinate) and DTAG
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(decyltrimethylammonium bromotrichlorogadolinate) was demonstrated. These

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magnetic surfactants were synthesized by stirring overnight using an equivalent

quantity of GdCl3.6H2O and either DTAB or CTAB in methanol, following which
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the solvent was evaporated under vacuum at 80 °C. The anionic magneto
surfactant based on gadolinium Gd(AOT)3 (tris-(1,4-bis(2-ethylhexoxy)-1,4-
dioxobutane-2-sulfonate) was synthesized via a liquid−liquid ion exchange
method. The GdCl3.6H2O was dissolved in an ethanol and water mixture (75:25
v/v, ethanol:water); 3 M aqueous NaAOT was added to the aforementioned
solution and stirred for 5 h. The solvent was then removed under low-pressure
and the sample was dried for 2 d at 80 °C. The anionic magneto surfactant was
then resolubilized in dry dichloromethane to remove the insoluble salts, and
finally, the pure product was obtained by centrifugation [152]. The synthesized

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magneto surfactants were functionalized with proteins; consequently, protein

separation and extraction was enabled by simply using an external magnetic field.
It is noted that the toxicity of magneto surfactants, in some cases, is lower than
that of conventional halide-based surfactant analogs [152] which may make
magneto surfactants suitable for use in contaminated or infected sites to enable
selective microbial reduction without influencing normal tissues and cells [153].

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3.2. Applications of magneto surfactants

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For cancer therapy, the emerging technology of smart nano-vehicles has
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received significant attention for improving chemotherapy efficiency and
preventing side effects. This has been increased by directing drugs to the targeted
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area and controlling drug release. Nucleic acids are crucial biological building
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blocks as they are characterized by molecular self-recognition [154-156].

Although DNA acts as a better intercalating platform to carry anticancer drugs, it
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is not considered a good nano-vehicle for delivering cancer drugs to infected

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tissues for specific targeting [157] because DNA with high molecular weight
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does not readily pass across the cell membranes independently, resulting in poor
intracellular uptake due to repulsive interaction between the negatively charged
DNA and cytomembrane.
When the surfactant concentration is increased beyond the critical micelle
concentration limit, the surfactant tends to aggregate as cationic micelles in the
vicinity of DNA [158-160]. These multivalent cationic micelles interact with
DNA through hydrophobic and electrostatic interactions to decrease the repulsion
between the DNA segments. This induces interaction between the multivalent
cationic micelles and at least three positive centers and DNA, and consequently
further induces compaction from the extended linear structure to the compacted

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form [161]. Although this approach can provide a solution for DNA delivery, it
still presents obstacles with respect to sensitivity and controllability, which are
required for more specific tissue targeting. By replacing the conventional
surfactants with magneto surfactants, a solution can be provided, where magnetic
switching allows the surfactants to reach an effective concentration under an
external magnetic field, resulting in a more condensed DNA structure at lower
concentration [148, 162]. The magneto surfactant with a magnetic counter ion has

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more functionalities that interact with the DNA [163]. Hao et al. reported that 10

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mM (high concentration) of the conventional surfactants CTAB or CTAC could
-p
promote the de-compaction of 0.15 mM of DNA, whereas the same concentration
of a magneto surfactant in which the counter ions (Cl¯ or Br¯ ) were replaced by
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[FeCl3Br]¯ afforded completely compacted DNA [163].
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Ling Wang et al. synthesized multiple responsive nano-vehicles that

effectively combine with DNA by utilizing a magneto surfactant and glutathione
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GSH-reductive triggers to control the delivery of the anticancer drug doxorubicin

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(DOX) with precise targeting, as illustrated in Figure 5a. The magneto surfactant
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CTAF, where the counter ion is [FeCl3Br]¯ , was synthesized with fullerenes
(C60) to increase the solubility and dispersity and increase the overall positive
charge around the cationic micelles to produce magnetic fullerenes
(C60@CTAF). DNA loaded with the anticancer drug DOX and treated with the
modified polysaccharide hyaluronic acid was then fabricated with as-synthesized
C60@CTAF to form C60@CTAF/DNA/HA-SS-COOH. The composite was then
used as an electrostatic platform to load the anticancer drug DOX, and the DNA-
DOX backbones were assembled with C60@CTAF to construct
C60@CTAF/DNA complexes. Under an applied magnetic field,

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C60@CTAF/DNA/HA-SS-COOH afforded controlled transport of the anticancer

drug DOX to the target tissue [147].

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Figure 5. (a) Schematic representation of magnetic fullerene-DNA vehicles.

Reproduced from Ref. [147]. (b) Schematic of ordered magneto surfactant/DNA
nanosphere hybrid: synthesis and structure. Reproduced from Ref. [164].

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Xu et al. synthesized well-ordered surfactant-DNA hybrid nanospheres using

a magnetic cationic surfactant (C16H33(CH3)3N+[FeCl3Br]−, CTAFe) and a
cationic ionic liquid C2H5O-azobenzene-OC2H4(CH3)3N+[FeCl3Br]−, azoTAFe.
The synthesized hybrid nanospheres could be targeted using a magnetic field, as
shown in Figure 5b. The procedure for synthesizing the final nanosphere
products was via DNA compaction, aggregation, and coagulation, and the
synthesized nanospheres could be used as promising drug vehicles in the field of

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nanomedicine [164]. Subsequently, Xu et al. reported the synthesis of AuNPs

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using the magnetic surfactant CH3(CH2)14CH2N(CH3)3+ [FeCl3Br]‒ (Figure 6a)
-p
[148]. These magnetic AuNPs enabled DNA delivery under the influence of a
low-strength magnetic field.
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Figure 6. (a) Schematic representation of synthesis of AuNPs using magneto

surfactant (A) and DNA and protein migration under low-strength external
magnetic field (B). Reproduced from Ref. [148]. (b) Synthesis of magnetic network
clusters and subsequent in situ AgNP formation on network templates (A);
synthesis of magnetic network for capturing specific sequence of DNA (B),
Reproduced from Ref. [165]. (c) Schematic illustrating control of biomolecule
migration by magneto-surfactant-coated carbon nanotubes. Reproduced from Ref.
[166].

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Wang et al. utilized fluorescent carbon quantum dots (CQDs) conjugated with
cysteine to produce a ligand (cys-CQDs), which then self-assembled with the
synthesized magnetic surfactants (CTAHo and CTAGd) via a facile non-covalent
method [165]. This magnetic network can separate DNA molecules with the
assistance of an external magnet. The cysteine protein on the CQD-magneto
surfactant network was used for in situ synthesis of AgNPs, as shown in Figure
6b (A), through three interaction centers in the cysteine molecules (carboxylate,

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ammonium, and sulfide groups). The AgNPs produced on the CQD-magneto

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surfactant network were functionalized with DNA modified-thiol through the
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bond between Ag and sulfide. The thus-constructed magnetic vehicle was used to
select specific sequences of DNA by DNA base pairing, as illustrated in Figure
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6b (B), thereby furnishing magnetic assemblies with high capture efficiency and
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recovery [165].
Xu et al. prepared cetyltrimethyl ammonium trichloromonobromocerate
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(CTACe). The cationic surfactant CTAB was stirred with CeCl3 in a molar ratio
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of 1:1 in methanol for 12 h under environmental conditions, and the solvent was
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evaporated to obtain the magneto surfactant (CTACe), which was then mixed
with carbon nanotubes under ultrasonication to obtain carbon nanotubes
functionalized with the magneto surfactant (CNTs@CTACe) [166].
CNTs@CTACe was used as an efficient nano-vehicle for drug delivery, as
illustrated in Figure 6c. The synthesized CNTs@CTACe can electrostatically
interact with proteins and DNA and also make compact structures of proteins and
DNA. Under an external magnetic force, the migration of DNA and proteins
could be controlled [166].
Zhao et al. synthesized magnetic-aggregated surfactants comprised of a
layered structure by co-assembling a double-tailed magneto surfactant with a

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chemical structure comprising (C18)2C2N+[FeCl4]‒ and polyoxometalate (POM)

[167]. The POM-magneto surfactant (Figure 7a) exhibits high transportation
efficiency for delivering myoglobin (protein) under an applied magnetic field.

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Figure 7. (a) Fabrication of magnetic POM-magneto surfactant (A) and

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schematic of magnet-facilitated protein delivery B), reproduced from Ref. [167].

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(b) Magnetic response of magnetic surfactant−graphene oxide systems; all

samples contain graphene oxide in water, but only the right-hand vials contain
additional magneto surfactant (DTA and min), reproduced from Ref. [168].

Graphene oxide (GO) has been intensively studied in a wide range of

applications, including water treatment [169], optics [170], and interface
stabilization [171], owing to its high dispersability, stability, and massive surface
area. Furthermore, GO has been modified and functionalized with magnetic
nanocomposites in many studies for targeted purposes. For example, modified

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GO can remover water pollutants such as arsenic [172], selenium [173],

chromium, and mercury [174, 175]. All of the aforementioned methods require
multi-step preparation, which undoubtedly affects the GO structure. To overcome
the issue, Thomas et al. developed a new method for implanting GO with an as-
synthesized magneto surfactant, where the magnetic ionic liquid surfactants, 1-
methyl-3-butylimidazolium tetrachloroferrate [mim] and
dodecyltrimethylammonium trichloromonobromoferrate [DTA], were

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synthesized with the GO nanosheets, providing a simple and economic method

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for GO recycling by using an external magnetic field [168], as shown in Figure
7b. -p
In drug delivery, cytotoxicity of surfactants should also be considered and
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discussed in elsewhere [176]. In addition to the properties of magnetic surfactants
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in the field of drug delivery as discussed above, magnetic surfactants have

advantages for their applications in many research fields of nanotechnology
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compared to the non-magnetic conventional surfactants. For example, their

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unique magnetic response can be easily controlled under the external magnetic
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field which can be particularly applicable for protein and DNA extraction and
self-aggregation-free molecular magnets. Beyond nanotechnology, the magnetic
surfactants have a great potential to use in environmental clean-up, water-
treatment. etc [177].

Conclusion and Future outlook

In this short review, we discussed the recent advances in surfactants and
their tunable, structure-dependent properties for optimized applications in
nanotechnology. During the synthesis of nanoparticles in solution, surfactants
play an important role in improving the dispersion stability and controlling the

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size distributions of the as-synthesized nanoparticles. In more detail, as the tail

length of the surfactant used for nanoparticle synthesis increases, smaller, less
aggregated, and more stable nanoparticles are produced. This development can
significantly promote colorimetric sensor applications based on size-tunable
nanoparticles. However, the correlation between the surfactant structure and
nanoparticle geometry should still be defined through intensive studies to provide
direct evidence of this correlation and molecular fingerprints. Furthermore, a new

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category of surfactants, namely, magneto surfactants, has been introduced. By

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forming a mixture of conventional surfactants and magnetic elements, a new
-p
series of surfactants having unique magnetic properties can be successfully
synthesized. Magneto surfactants have been further utilized in the field of drug
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delivery because of their high selectivity and sensitivity to target a certain
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position. Although the emerging category of surfactants has been intensively

studied, it is still necessary to elucidate the fundamental mechanisms, provide
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technical solutions, achieve deeper understanding of their toxicity, and enable the
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possibility of large-scale production for commercial uses, considering the short

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history of surfactants since their initial discovery.

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Acknowledgement

This study was supported by the National Research Foundation of Korea (NRF) grant, funded

by the Korean Government (MSIT) (2020R1A5A1018052, 2020R1C1C1009381, and

2020R1A4A3079710).

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 Mini-Review

Recent advances in surfactants-assisted nanotechnology

Samy M. Shaban1,2,3, Joohoon Kang4,*, and Dong-Hwan Kim1,2,*
1. School of Chemical Engineering, Sungkyunkwan University (SKKU), Suwon 16419,
Republic of Korea
2. Biomedical Institute for Convergence at SKKU (BICS), Sungkyunkwan University
(SKKU), Suwon 16419, Republic of Korea
3. Petrochemicals Department, Egyptian Petroleum Research Institute, Egypt
4. School of Advanced Materials Science and Engineering, Sungkyunkwan University

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(SKKU), Suwon 16419, Republic of Korea

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E-mail: dhkim1@skku.edu (D.-H. K.) and joohoon@skku.edu (J.K.)
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Highlights
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- Surfactant-assisted technological advances in nanotechnology
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- Surfactant structure-oriented nanoparticle synthesis and dispersion stability

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- Emerging category of surfactant with magnetic properties; magneto-

surfactants
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- Magneto-surfactants based applications; drug delivery and biomolecules

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separation

1
Declaration of interests

☒ 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.

☐The authors declare the following financial interests/personal relationships which may be considered
as potential competing interests:

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